EP1140375B1 - Method and device for continuously coating at least a metal strip with a crosslinkable polymer fluid film - Google Patents

Method and device for continuously coating at least a metal strip with a crosslinkable polymer fluid film Download PDF

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Publication number
EP1140375B1
EP1140375B1 EP99957371A EP99957371A EP1140375B1 EP 1140375 B1 EP1140375 B1 EP 1140375B1 EP 99957371 A EP99957371 A EP 99957371A EP 99957371 A EP99957371 A EP 99957371A EP 1140375 B1 EP1140375 B1 EP 1140375B1
Authority
EP
European Patent Office
Prior art keywords
metal strip
roller
cross
temperature
film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP99957371A
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German (de)
French (fr)
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EP1140375A1 (en
Inventor
Claude Bonnebat
Frédéric JENNY
Thierry Soas
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sollac SA
Original Assignee
Sollac SA
Lorraine de Laminage Continu SA SOLLAC
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Filing date
Publication date
Priority claimed from FR9815900A external-priority patent/FR2787353B1/en
Priority claimed from FR9815901A external-priority patent/FR2787354B1/en
Application filed by Sollac SA, Lorraine de Laminage Continu SA SOLLAC filed Critical Sollac SA
Publication of EP1140375A1 publication Critical patent/EP1140375A1/en
Application granted granted Critical
Publication of EP1140375B1 publication Critical patent/EP1140375B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/14—Removing excess of molten coatings; Controlling or regulating the coating thickness
    • C23C2/22—Removing excess of molten coatings; Controlling or regulating the coating thickness by rubbing, e.g. using knives, e.g. rubbing solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C1/00—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating
    • B05C1/04—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length
    • B05C1/08—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line
    • B05C1/0826—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line the work being a web or sheets
    • B05C1/083—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line the work being a web or sheets being passed between the coating roller and one or more backing rollers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C1/00—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating
    • B05C1/04—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length
    • B05C1/08—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line
    • B05C1/0826—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line the work being a web or sheets
    • B05C1/0834—Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line the work being a web or sheets the coating roller co-operating with other rollers, e.g. dosing, transfer rollers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/28—Processes for applying liquids or other fluent materials performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers

Definitions

  • the present invention relates to a method and a device for continuously coating at least one metal strip with a fluid film of small thickness of crosslinkable polymer free of solvent or non-reactive diluent.
  • thermosetting polymers for example thermosetting polymers, or physically, such as, for example, photopolymerizable polymers, are known.
  • thermosetting organic coatings that are continuously applied to metal substrates.
  • these are complex formulations that associate in a solvent or aqueous medium a system of functional organic prepolymer binders, a crosslinking system and additives such as pigments or fillers, various formulation adjuvants.
  • thermoplastic or thermosetting organic coating to a bare or coated metal strip.
  • organic coatings such as for example liquid paints or varnishes is most often carried out by roller coating of these liquid coatings as a solution or dispersion in a solvent or aqueous medium.
  • the liquid coating is deposited on a metal strip by pre-dosing the solution or dispersion by means of a two or three-roll system and transferring part or all of the liquid coating thus pre-stressed to a applicator roll in contact with the surface of the metal strip to be coated.
  • the transfer is carried out either by friction of the applicator roll and the metal strip, the scrolling of the two contacting surfaces being effected in the opposite direction or by contact in the same direction.
  • extrusion coating of a thin organic coating is routinely practiced especially with thermoplastic polymers on flexible surfaces, such as paper, plastic films, textiles or even thin metal substrates such as packaging materials.
  • the application of the molten coating is carried out by means of a rigid flat die or a nozzle positioned in direct contact with the substrate.
  • the pressure exerted by the die on the substrate results from the viscosity of the melt.
  • the possibilities of correcting unevenness of the substrate by plating it on the support roll are very limited.
  • This coating extrusion technique requires perfect parallelism between the edges of the die and the substrate and this substrate must be either perfectly flat or deformable to allow the formation of a thin deposit of uniform thickness.
  • the deposited material thickness is controlled by the play and pressure between the die and the substrate, which imposes a perfect parallelism of these two elements when one wants to achieve very thin applications.
  • the technique of extrusion lamination of a uniform layer of fluid coating on a substrate uses die drawing of a fluid web at the exit of a flat die, which web is then pressed onto the substrate using for example a cold roller, a rotating bar or by an air knife or an electrostatic field.
  • the thickness of the fluid web is controlled by the flow rate of the material in the die section and the substrate speed.
  • the plating pressure must, however, be small enough to avoid the formation of a calender bead and, therefore, this transfer mode does not make it possible to compensate for possible variations in thickness and unevenness in the case of a rigid substrate.
  • This technique for applying the coating with formation of a free strand at the extrusion die exit avoids the problems of coupling between the die and the rigid substrate, but it induces instabilities of application if the length free strand fluctuates and is difficult to implement with thermosetting systems with a viscosity of less than 2000 Pa.s because of the difficulties in achieving regular stretching and good plating.
  • the continuous application of a thin organic coating on metal substrates is carried out under low contact pressures, insufficient to allow a thin coating, uniformly and homogeneously applied on rigid substrates which may have flatness and thickness heterogeneity defects.
  • microbubbles of air can be interposed between the coating and the substrate which affects the homogeneous application and the surface appearance of this coating.
  • the polymer coating after crosslinking, the polymer coating must be sufficiently hard while being deformable to allow the shaping of the sheets thus coated without causing degradation or detachment of the coating.
  • the increase in the molecular weight of the precursors has a very unfavorable effect on the viscosity of a solvent-free polymer or a non-reactive diluent, which is detrimental to the ease of transfer and application of the web to the state. melted uncrosslinked on the metal strip.
  • EPC discloses a process for continuously coating at least one metal strip with a crosslinkable polymer-free solvent-free or diluent-thick film and a thickness less than that of the metal strip, in which the metal strip is continuously scrolled, said metal strip is preheated to a temperature substantially equal to or greater than the temperature of the crosslinkable polymer fluid film and the softening temperature of this crosslinkable polymer a homogeneous sheet of uniform thickness of said crosslinkable polymer is formed by forced flow on a hard surface gripping cylinder, said gripping cylinder being heated to a temperature substantially equal to or greater than the temperature of said sheet and at the temperature of softening of this crosslinkable polymer and rotated in the same direction as the support roll of the metal band allique and form the crosslinkable polymer film to a uniform thickness substantially equal to the desired thickness, and is compressed between the gripper cylinder and the metal strip, a deformable surface applicator element, heated to a
  • the aim of the invention is to avoid these drawbacks by proposing a method and a device for continuously coating at least one metal strip with a fluid film of small thickness made of crosslinkable polymer that is free of solvent or non-reactive diluent and whose the softening temperature is greater than 50 ° C, to obtain a coating of uniform thickness of a few microns to a few tens of microns applied in a homogeneous manner on this strip, while avoiding that microbubbles of air are inserted between the film and the metal strip and overcoming flatness and roughness defects of this band and by allowing an application on part or all of the coating and this despite variations in width and transverse positioning of this band.
  • FIGs. 1 and 3 schematically shows two installations for continuously coating a metal strip 1 with a fluid crosslinkable polymer film, free of solvent or non-reactive diluent and having a thickness for example between 5 and 50 .mu.m.
  • This metal strip 1 has a thickness for example between 0.10 and 4 mm and is for example steel or aluminum or aluminum alloy and can be coated or prepainted on one or both sides.
  • the polymer used to coat the metal strip 1 is a solvent-free polymer or non-reactive and thermally crosslinkable diluent such as a thermosetting polymer or physically such as a photopolymerizable polymer.
  • This polymer has in the uncrosslinked state a softening temperature greater than 50 ° C.
  • These polymers have different softening, start-flow, start-cross-cure and crosslinking temperatures.
  • the crosslinking start temperature is the temperature from which an increase in viscosity of greater than 10% is observed in less than 15 minutes.
  • the metal strip 1 is driven in scrolling along the arrow F and the metal strip 1 is supported on at least one support cylinder 3.
  • the installations comprise means 2 for preheating the metal strip 1 at a temperature substantially equal to or greater than the temperature of the crosslinkable polymer fluid film to deposit said metal strip 1 and the softening temperature of this crosslinkable polymer.
  • the means 2 for preheating the metal strip 1 are constituted for example by at least one induction furnace.
  • the cooking means comprise for example at least one induction furnace and cooling means and in the case where the polymer is physically crosslinkable, the cooking means may be constituted by ultraviolet lamps or by electron beams.
  • the crosslinkable polymer film to be deposited on the metal strip 1 must be of uniform thickness, although this metal strip 1 has thickness heterogeneities or flatness defects as well as roughness and / or significant surface ripples. amplitudes equal to or greater than the thickness of the film to be deposited on the metal strip 1.
  • the forced flow forming means of the crosslinkable polymer ply 30 comprise, for example, an extrusion machine, not shown, of conventional type, provided with a spinneret 11 comprising an extrusion slot 12 and a flow control member, not shown, constituted for example by a metering pump and disposed between the extrusion machine and the die 11.
  • the formation and total transfer means in thickness of the film 31 of crosslinkable polymer are formed by the cylinder 20 and by means for compressing the metal strip 1 between the cylinder 20 and the support cylinder 3 for obtain a coating of uniform thickness.
  • a transfer is considered to be total or almost total thickness when more than 90% of the material has been transferred.
  • the cylinder 20 is heated to a temperature substantially equal or greater, on the one hand, to the formation temperature of the web 30 and, on the other hand, to the softening temperature of the crosslinkable polymer and is rotated, by means of appropriate means not shown, in a reverse direction in the direction of travel of the metal strip 1, as represented by the arrows f1 in Figs. 1 and 2.
  • the cylinder 20 comprises a metal core coated with an envelope of deformable material, such as an elastomer, and the support cylinder 3 has a hard surface.
  • the cylinder 20 has a hard surface and the support cylinder 3 comprises a metal core coated with an envelope of deformable material such as an elastomer.
  • the formation of the web 30 of said crosslinkable polymer is carried out for example by extrusion coating or by extrusion lamination.
  • the means for forming by forced flow of the sheet 30 are formed by the die 11 bearing against the surface of the cylinder 20 and provided with means of adjustment, of the conventional type, the position of the edges of the extrusion slot 12 of said die 11 relative to the surface of the cylinder 20.
  • the die 11 of the extrusion machine gives the uniform distribution of the ply 30 which is obtained by adjusting the flow rate of the die 11 and the speed of rotation of the cylinder 20.
  • the die 11 is supported on the cylinder 20 for example by means of cylinders, not shown, the pressure of which makes it possible to standardize the leakage rate of the fluid crosslinkable polymer.
  • the means for forming by forced flow of the ply 30 are formed by the die 11, means for drawing the ply 30 by adjusting the flow rate of this spinneret 11 and / or the speed of rotation of the applicator roll 20, adjustment means of the conventional type, the position of the edges of the extrusion slot 12 of said die 11 relative to the surface of the cylinder 20 and by means of means, not shown, for plating the ply 30 on said surface of the applicator roll 20.
  • the plating means of the ply 30 on the surface of the cylinder 20 are formed for example by an air knife directed towards this cylinder 20 at the generatrix of contact of said ply 30 on said applicator cylinder 20.
  • the cylinder 20 and the support cylinder 3 each comprise a hard surface and the transfer element is formed by a transfer cylinder 21 or applicator cylinder comprising a metal core coated with a casing of deformable material, such as an elastomer.
  • the cylinder 20 and the support cylinder 3 each comprise a metal core coated with an envelope of deformable material, such as for example an elastomer, and the transfer element is formed by an applicator roll 21 of hard surface.
  • the transfer element is formed by an endless band.
  • the cylinder 20 heated to a temperature substantially equal to the formation temperature of the web 30 and the softening temperature of the crosslinkable polymer, is rotated in the opposite direction to the running direction of the metal strip.
  • the applicator cylinder 21 heated to a temperature substantially equal to or greater than the temperature of the cylinder 20 is rotated also in the opposite direction to the direction of travel of the support cylinder 3 of the metal strip 1, as represented by FIG. arrow f2 in FIG. 3 and 4.
  • the thermal conditioning of the crosslinkable polymer during the contact of the sheet 30 on the cylinder 20 in the case of the first embodiment shown in Figs. 1 and 2 or during the contact of the intermediate web 30b on the cylinder 20 and / or the contact of the film 31 on the transfer element 21 in the case of the embodiment shown in Figs. 3 and 4, to lower the viscosity of this crosslinkable polymer, can be achieved in different ways.
  • the heat-conditioning means of the crosslinkable polymer are formed by an internal heating system of the cylinder 20 and / or the applicator cylinder 21 and / or by at least one source 15 for applying a heat flux. complementary to the ply 30 or to the intermediate ply 30b and / or to the film 31.
  • the thermal conditioning means of the crosslinkable polymer are formed by an internal heating system of the cylinder 20 and / or by an external heating system of the applicator roll 21 and / or by at least one source 15 of applying a complementary thermal flux to the ply 30 or to the intermediate ply 30b and / or to the film 31.
  • the internal heating system of the cylinder 20 and / or the applicator cylinder 21 is constituted by electrical resistances embedded in the mass of each of said cylinders or by channels formed in said cylinders for the circulation of a coolant, such as for example oil.
  • the temperature of these cylinders must be adjusted, for example by means of a not shown thermocouple, in order not to exceed a limit value to avoid damaging the outer envelope of deformable material by too high a temperature and to deteriorate the bonding layer between the deformable material and the metal core of said cylinders.
  • this heating system is arranged facing the corresponding cylinder in the zone not covered by the film 31 and is consisting for example of hot air generators or infrared lamps.
  • the source or sources of application of the complementary heat flux on the film 31 or on the intermediate layer 30b and / or on the film 31 consist for example of infrared lamps of medium absorption wavelength between 1 , 5 and 4 ⁇ m or by hot air generators or by microwave systems.
  • the heat-conditioning means of the cross-linkable polymer in suitable modalities therefore make it possible to lower the viscosity of this polymer, ie the fluidity of the polymer, in order to facilitate its transfer and its application on the metal strip 1.
  • the modalities are adapted to lower the viscosity of the crosslinkable polymer by at least a factor of 2, and for the temperature of said crosslinkable polymer to exceed the crosslinking start temperature of this polymer.
  • this viscosity retains at least transiently a very low level facilitating the transfer and the application of the film 31 crosslinkable polymer on the metal strip 1.
  • the coating device 10 comprises means, not shown, of conventional type, for adjusting the tangential speeds of the cylinder 20 or the cylinder 20 and the applicator roll 21 in a ratio between 0.5 and 2 times the running speed of the metal strip 1.
  • the speeds of the cylinder 20 or the cylinder 20 and the applicator roll 21 can be adjusted independently of one another.
  • the coating device 10 also comprises means (not shown) for adjusting the contact pressure between the cylinder 20 and the metal strip 1 (FIGS 1 and 2) and, on the one hand, between the cylinder 20 and the cylinder applicator 21 and, on the other hand, between the applicator roll 21 and the metal strip 1 (Figs 3 and 4).
  • These means consist, for example, of hydraulic cylinders or screw / nut systems which make it possible to adjust the contact pressures as a function of the viscosity of the crosslinkable polymer so as to ensure a total transfer of the material and to minimize the friction forces. .
  • the extrusion slot 12 of the die 11 and the cylinder 20 or the cylinder 20 and the applicator roll 21 have a length greater than the width of the metal strip 1 so as to coat the entire surface of the face of this metal strip 1 in contact with the cylinder 20 or the applicator cylinder 21.
  • the extrusion slot 12 of the die 11 and the cylinder 20 or the cylinder 20 and the applicator roll 21 may have a length less than the width of the metal strip 1 to coat only part of the surface the face of said metal strip 1 in contact with the cylinder 20 or the applicator roll 21.
  • the application of the thin and thin film 31 of thermally or physically crosslinkable polymer is carried out as follows.
  • the metal strip 1 is maintained at a temperature equal to or greater than the softening temperature of the crosslinkable polymer and the cylinder 20 is rotated in the opposite direction to the running direction of this metal strip 1.
  • the metal strip 1 is preheated to a temperature of 140 ° C immediately before passing on the support cylinder 3 and scrolls at a speed of 30m / min.
  • the sheet 30 formed by forced flow at a temperature above the softening temperature of the crosslinkable polymer in the uncrosslinked state is pressed onto the cylinder 20 so as to form the film 31 of crosslinkable polymer of uniform thickness substantially corresponding to the thickness of the coating to be formed on the metal strip 1.
  • the metal strip 1 thus coated passes into the cooking means 5, then into the cooling means 6 of the film 31 of crosslinkable polymer.
  • the application of the thin and thin film 31 of thermally or physically curable polymer is carried out as follows.
  • the metal strip 1 is maintained at a temperature equal to or greater than the softening temperature of the crosslinkable polymer in the uncrosslinked state and the rolls 20 and 21 are rotated in a direction opposite to the running direction of the metal strip 1.
  • the sheet 30 formed by forced flow at a temperature above the softening temperature of the crosslinkable polymer is pressed onto the cylinder 20 so as to form the intermediate layer 30b of polymer crosslinkable of uniform thickness.
  • the intermediate web 30b is transferred from the roll 20 to the applicator roll 21 which forms the film 31 and this film 31 is transferred from the applicator roll 21 on the surface of the metal strip 1 to be coated.
  • the metal strip 1 thus coated passes into the cooking means 5, then into the cooling means 6 of the film 31 of crosslinkable polymer.
  • the crosslinkable polymer film 31 may be deposited on a bare metal strip of steel or aluminum or aluminum alloy or on a pre-coated or prepainted metal strip.
  • the coating thus produced on the metal strip 1 has for example a thickness of between 5 and 50 ⁇ m with a uniformity of thickness of a few microns and this despite the notable defects of flatness or thickness heterogeneity of the metal strip 1.
  • the means for forming by forced flow of the sheet 30 may be formed by a rigid block of crosslinkable polymer applied under controlled pressure to deposit crosslinkable polymer particles on the cylinder 20 and form said sheet 30 or by a transfer system under an electrostatic field of a polymer powder crosslinkable on the cylinder 20 to form this web 30.
  • the means for forming by forced flow of the ply 30 may be formed by a fluid crosslinkable polymer spraying system on the cylinder 20 or by an application system on this cylinder 20 of a continuous strip. crosslinkable polymer previously produced to form said web 30.
  • the means for forming by forced flow of the sheet 30 may be formed by a rotating bar disposed between the die 12 and this cylinder 20.
  • the web 30 and the cross-linkable polymer film 31 may have a width less than the width of the metal strip 1 to coat a part of this metal strip 1 or a width greater than the width of this metal strip 1 to coat the entire of said metal strip 1.
  • This excess cross-linkable polymer must be removed in order to prevent it from creating an excess thickness on the cylinder 20 or on the applicator roll 21.
  • the coating device 10 is equipped with means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20.
  • the means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20 are formed by two scraped, respectively 41a and 41b, for example metal, in contact with the cylinder 20 in each zone located outside the zone in contact with the cylinder 20 with the metal strip 1.
  • doctor blades 41a and 41b in contact with the cylinder 20 are arranged upstream of the generatrix for applying the ply 30 to this cylinder 20 with respect to the direction of rotation of said cylinder 20.
  • the transverse position of the rades 41a and 41b on the cylinder 20 may be secured, by appropriate means, not shown, to the width of the metal strip 1 and / or to the transverse position of this metal strip 1 on the support cylinder 3.
  • this metal strip 1 on the support cylinder 3 may vary.
  • doctor blades 41a and 41b are thus in contact with the cylinder 20 and remove the excess of crosslinkable polymer by friction on said cylinder 20.
  • the means 40 for removing the excess crosslinkable polymer on the cylinder 20 may be formed by two recovery cylinders arranged between the scrapers 41a and 41b and the cylinder 20.
  • the means for removing the excess crosslinkable polymer on the cylinder 20 may be formed by a recovery cylinder interposed between the cylinder 20 and a doctor blade having a length at least equal to the length of the cylinder 20 .
  • the means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20 are formed by at least one squeegee, for example metal, in contact with the cylinder 20.
  • the means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20 are formed by two doctor blades, respectively 42a and 42b, for example metal, each in contact with the lateral edge of the cylinder 20 upstream of the generator for applying the ply 30 to this cylinder 20.
  • the transverse position of the doctor blades 42a and 42b on the cylinder 20 is secured by appropriate means, not shown, to the width of the metal strip 1 and / or to the transverse position of this metal strip 1 on the support cylinder 3.
  • doctor blades 42a and 42b are thus in contact with the cylinder 20 and remove the excess of crosslinkable polymer by friction on said cylinder 20.
  • the second solution consists in equipping the applicator cylinder 21 with means 40 for removing the excess crosslinkable polymer.
  • these means 40 for removing the crosslinkable polymer excess on the applicator roll 21 are formed by a recovery cylinder 22 in contact with the applicator roll 21, and by at least one squeegee 43 in contact with said recovery roll 22 .
  • the excess crosslinkable polymer deposited on the applicator cylinder 21 is transferred to the recovery cylinder 22 because of the pressure exerted by said recovery cylinder on the applicator cylinder 21 and this excess crosslinkable polymer is removed from the recovery cylinder 22 by the squeegee 43.
  • the means for removing the excess crosslinkable polymer on the applicator roll 21 may be formed by a recovery cylinder 22 and by two scrapes each in contact with a lateral edge of said recovery cylinder 22.
  • the means for removing the excess crosslinkable polymer deposited on the cylinder 20 or the applicator roll 21 avoids having to add inserts at the slot 12 of the extrusion die 11 so as to calibrate as soon as leaving the die 12 the web 30 of crosslinkable polymer and to accommodate variations in width and transverse positioning of the metal strip 1 within the predefined tolerance limits.
  • the point of application of the film 31 of the crosslinkable polymer may be located at a different location than in front of the support cylinder 3 of the metal strip 1 and, for example, on a free arm stretched by this metal strip 1 downstream of said support cylinder 3.
  • the two faces of the metal strip 1 can be coated with a film 31 of crosslinkable polymer.
  • a device 10 for applying the film 31 is disposed on one side of the metal strip 1 and another film application device 31 is disposed on the other side of said metal strip 1.
  • the application of the film 31 on each side of the metal strip 1 may be shifted or simultaneous.
  • the support cylinder 3 is removed and replaced by an applicator cylinder of the second application device.
  • the applicator roll of each device forms a support cylinder of the metal strip.
  • the transverse position of the extrusion die 11 may be permanently centered with respect to the metal strip 1 by arranging this extrusion die 11 on a transversely movable support and by connecting this die to the extrusion machine by a flexible which makes it possible to slave the position of this extrusion die 11 with respect to the metal strip 1 as a function of the variations of the transverse position of said metal strip 1 relative to the cylinder of the support 3.
  • a lubricant may be deposited on the applicator roll 20 outside the zone in contact with the metal strip 1 so as to facilitate the operation of the squeegees 41a and 41b for the removal of the excess of crosslinkable polymer.
  • This mixture is entirely in the fluid and / or viscous state starting from a temperature equal to 120 ° C. and its rapid cross-linking temperature is between 170 ° and 250 ° C.
  • the crosslinkable polymer may also be pigmented and loaded, for example, with 40% and more by weight of titanium oxide.
  • This value causes rapid wear of the applicator roll.
  • the coating device according to the invention makes it possible to obtain a cross-linkable polymer coating with a uniform thickness of, for example, between 5 and 50 ⁇ m and homogeneously applied to a metal strip having a large roughness of amplitude comparable to that of film thickness and this thanks to the perfect contact between the applicator roll and the surface of the metal strip to be coated, despite the defects of flatness and thickness heterogeneity of the metal strip.
  • the speed of the applicator roll can be adjusted to a level substantially greater or less than the running speed of the metal strip so as to obtain a perfect continuity of the coating and an excellent surface state of this crosslinkable polymer coating transferred onto this metal strip.
  • the surface energy of the applicator roll is adapted to the crosslinkable polymer to allow good spreading of the web on the applicator roll.
  • the coating device according to the invention can also be used for a downward or horizontal metal strip.
  • thermosetting polymers Since the forced flow through an extrusion slot involves significant stagnation of the polymer which are necessary for a good distribution of this polymer over the entire width of this extrusion slot and it should not risk at this level a crosslinking of said polymer.
  • the coating device according to the invention makes it possible to continuously coat metal strips of different widths or to coat simultaneously several metal strips arranged parallel to each other and to overcome by simple and effective means fluctuations in width and transverse positioning of the metal strip or strips.
  • the coating device according to the invention makes it possible to facilitate the regular and uniform supply of the crosslinkable polymer coating by selecting the most appropriate mode of supply according to the product to be used.
  • the temperature of the material delivered by the supply system located upstream of the applicator cylinder is limited to a value lower than that of the beginning of crosslinking to avoid any risk of evolution of the product in the feed system and any risk of blockage of this system.
  • this device also makes it possible, in the case of a chemical transfer process, to raise the temperature of the crosslinkable polymer so as to reduce its viscosity and to facilitate its transfer and spreading on the metal strip. .
  • the material can withstand a very large heating, but for a very short time that avoids any risk of crosslinking the product at this level.
  • the device according to the invention makes it possible to compensate for variations in the width or transverse position of the metal strip during application and to overcome the defects of uniformity of the metal strip and thus to make a coating of Uniform surface thickness on a non-uniform metal substrate.

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Abstract

The invention concerns a method for continuously coating at least a metal strip with a crosslikable polymer fluid film free of non-active solvent or diluent and whereof the softening temperature is higher than 50° C. The method consists in continuously unwinding the metal strip (1) on at least a back-up roll (3); forming, on a roll (20) by forced flow, a layer of said crosslinkable polymer in melted state; forming, from said layer (30), said crosslinkable polymer film (31); and transferring entirely in thickness said film onto the metal strip (1) and, between the zone forming the layer (30) on the roll (20) and the zone applying the film (31) on the metal strip, in thermally conditioning the crosslinkable polymer to reduce its viscosity. The invention also concerns a coating device for implementing said method.

Description

La présente invention a pour objet un procédé et un dispositif de revêtement en continu d'au moins une bande métallique par un film fluide et de faible épaisseur en polymère réticulable exempt de solvant ou de diluant non réactif.The present invention relates to a method and a device for continuously coating at least one metal strip with a fluid film of small thickness of crosslinkable polymer free of solvent or non-reactive diluent.

On connaît des polymères qui sont réticulables par voie thermique, comme par exemple les polymères thermodurcissables, ou par voie physique, comme par exemple les polymères photopolymérisables.Polymers which are thermally crosslinkable, for example thermosetting polymers, or physically, such as, for example, photopolymerizable polymers, are known.

Il existe une grande variété de revêtements organiques thermodurcissables qui sont appliqués en continu sur des substrats métalliques.There is a wide variety of thermosetting organic coatings that are continuously applied to metal substrates.

Dans la plupart des cas, il s'agit de formulations complexes q'ui associent dans un milieu solvant ou aqueux un système de liants organiques fonctionnels prépolymères, un système réticulant et des additifs tels que les pigments ou charges, adjuvants divers de formulation.In most cases, these are complex formulations that associate in a solvent or aqueous medium a system of functional organic prepolymer binders, a crosslinking system and additives such as pigments or fillers, various formulation adjuvants.

On connaît également divers procédés d'application d'un revêtement organique thermoplastique ou thermodurcissable sur une bande métallique nue ou revêtue.Various methods of applying a thermoplastic or thermosetting organic coating to a bare or coated metal strip are also known.

L'application des revêtements organiques comme par exemple des peintures ou des vernis liquides s'effectue le plus souvent par enduction au rouleau de ces revêtements liquides à l'état de solution ou de dispersion en milieu solvant ou aqueux.The application of organic coatings such as for example liquid paints or varnishes is most often carried out by roller coating of these liquid coatings as a solution or dispersion in a solvent or aqueous medium.

Pour cela, on réalise le dépôt du revêtement liquide sur une bande métallique en effectuant un prédosage de la solution ou de la dispersion grâce à un système à deux ou trois rouleaux et en transférant une partie ou la totalité de ce revêtement liquide ainsi prédosé sur un rouleau applicateur en contact avec la surface de la bande métallique à revêtir.For this purpose, the liquid coating is deposited on a metal strip by pre-dosing the solution or dispersion by means of a two or three-roll system and transferring part or all of the liquid coating thus pre-stressed to a applicator roll in contact with the surface of the metal strip to be coated.

Le transfert est réalisé soit par friction du rouleau applicateur et de la bande métallique, le défilement des deux surfaces en contact s'effectuant en sens contraire ou soit par contact dans le même sens.The transfer is carried out either by friction of the applicator roll and the metal strip, the scrolling of the two contacting surfaces being effected in the opposite direction or by contact in the same direction.

Une évolution intéressante de la technologie d'application en continu des revêtements en polymère réticulable, comme par exemple des peintures ou des vernis thermodurcissables, sur une bande métallique consiste à effectuer le dépôt de ce revêtement sans faire intervenir de solvant ou de diluant.An interesting evolution of the technology for continuous application of crosslinkable polymer coatings, such as paints or thermosetting varnishes, on a metal strip is to perform the deposition of this coating without involving solvent or thinner.

Plusieurs alternatives ont été proposées pour l'élaboration et l'application de revêtements organiques sans emploi de solvant ou de diluant non réactif.Several alternatives have been proposed for the development and application of organic coatings without the use of solvent or non-reactive diluent.

Ainsi, pour réaliser des dépôts minces de produits organiques visqueux, une autre technique consiste à utiliser l'extrusion du revêtement organique à l'état fluide et à appliquer ce revêtement sur un substrat par couchage ou par lamination.Thus, for producing thin deposits of viscous organic products, another technique is to use the extrusion of the organic coating in the fluid state and to apply this coating to a substrate by coating or lamination.

L'extrusion couchage d'un revêtement organique mince est pratiquée de façon courante en particulier avec des polymères thermoplastiques sur des surfaces souples, comme le papier, les films plastiques, les textiles, voire des supports métalliques minces comme des matériaux d'emballage.The extrusion coating of a thin organic coating is routinely practiced especially with thermoplastic polymers on flexible surfaces, such as paper, plastic films, textiles or even thin metal substrates such as packaging materials.

L'application du revêtement fondu est réalisé au moyen d'une filière plate rigide ou d'une buse positionnée au contact direct du substrat.The application of the molten coating is carried out by means of a rigid flat die or a nozzle positioned in direct contact with the substrate.

La pression exercée par la filière sur le substrat provient de la viscosité de la matière fondue. Ainsi, les possibilités de correction des défauts de planéité du substrat par plaquage de celui-ci sur le cylindre d'appui sont très limitées.The pressure exerted by the die on the substrate results from the viscosity of the melt. Thus, the possibilities of correcting unevenness of the substrate by plating it on the support roll are very limited.

Cette technique d'extrusion couchage exige un parallélisme parfait entre les bords de la filière et le substrat et ce substrat doit être soit parfaitement plan, soit déformable pour permettre la formation d'un dépôt mince d'épaisseur uniforme.This coating extrusion technique requires perfect parallelism between the edges of the die and the substrate and this substrate must be either perfectly flat or deformable to allow the formation of a thin deposit of uniform thickness.

En effet, l'épaisseur de matière déposée est contrôlée par le jeu et la pression entre la filière et le substrat, ce qui impose un parallélisme parfait de ces deux éléments lorsque l'on veut réaliser des applications en très fine épaisseur.Indeed, the deposited material thickness is controlled by the play and pressure between the die and the substrate, which imposes a perfect parallelism of these two elements when one wants to achieve very thin applications.

Cette condition n'est pas réalisable dans le cas de bandes d'acier d'épaisseur comprise entre 0,3 et 2mm, qui présentent une rigidité trop importante et une planéité ou une régularité d'épaisseur insuffisante pour permettre un ajustement aussi précis du jeu entre la filière et le substrat, en particulier dans le cas de bandes de grande largeur.This condition is not feasible in the case of steel strips of thickness between 0.3 and 2 mm, which have too much rigidity and flatness or thickness regularity insufficient to allow such a precise adjustment of the game between the die and the substrate, especially in the case of wide strips.

La technique de l'extrusion lamination d'une couche uniforme de revêtement fluide sur un substrat utilise l'étirage sous filière d'une nappe fluide à la sortie d'une filière plate, cette nappe étant ensuite plaquée sur le substrat à l'aide par exemple d'un rouleau froid, d'une barre rotative ou encore par une lame d'air ou un champ électrostatique.The technique of extrusion lamination of a uniform layer of fluid coating on a substrate uses die drawing of a fluid web at the exit of a flat die, which web is then pressed onto the substrate using for example a cold roller, a rotating bar or by an air knife or an electrostatic field.

Dans ce cas, l'épaisseur de la nappe fluide est contrôlée par le débit de la matière dans la section de la filière et par la vitesse de substrat.In this case, the thickness of the fluid web is controlled by the flow rate of the material in the die section and the substrate speed.

En cas de collage de la nappe fluide sur le rouleau de plaquage, la nappe se séparerait alors en deux parties dans son épaisseur, une partie étant appliquée sur le substrat et l'autre partie restant appliquée sur le rouleau. Cette séparation de la nappe implique donc que le transfert n'est pas total et le revêtement obtenu sur le substrat ne présente pas un aspect de surface satisfaisant, ni une épaisseur uniforme.In case of bonding of the fluid layer on the plating roll, the ply would then separate in two parts in its thickness, a portion being applied to the substrate and the other part remaining applied to the roll. This separation of the web therefore implies that the transfer is not complete and the coating obtained on the substrate does not have a satisfactory surface appearance or a uniform thickness.

Pour éviter le collage de la nappe fluide sur le rouleau de plaquage, celui-ci doit présenter une surface parfaitement lisse et refroidie.To avoid sticking of the fluid web on the plating roll, it must have a perfectly smooth and cooled surface.

La pression de plaquage doit cependant être suffisant faible pour éviter la formation d'un bourrelet de calandrage et, de ce fait, ce mode de transfert ne permet pas de compenser les variations éventuelles d'épaisseur et des défauts de planéité dans le cas d'un substrat rigide.The plating pressure must, however, be small enough to avoid the formation of a calender bead and, therefore, this transfer mode does not make it possible to compensate for possible variations in thickness and unevenness in the case of a rigid substrate.

Cette technique d'application du revêtement avec formation d'un brin libre à la sortie de la filière d'extrusion permet d'éviter les problèmes de couplage entre la filière et le substrat rigide, mais elle induit des instabilités d'application si la longueur du brin libre fluctue et elle est difficile à mettre en oeuvre avec des systèmes thermodurcissables de viscosité inférieure à 2000 Pa.s en raison des difficultés à réaliser un étirage régulier et un bon plaquage.This technique for applying the coating with formation of a free strand at the extrusion die exit avoids the problems of coupling between the die and the rigid substrate, but it induces instabilities of application if the length free strand fluctuates and is difficult to implement with thermosetting systems with a viscosity of less than 2000 Pa.s because of the difficulties in achieving regular stretching and good plating.

D'une manière générale, dans les différentes techniques connues énumérées ci-dessus, l'application en continu d'un revêtement organique mince sur des substrats métalliques s'effectue sous des pressions de contact faibles, insuffisantes pour permettre de réaliser un revêtement mince, uniforme et appliqué de manière homogène sur des substrats rigides qui peuvent présenter des défauts de planéité et d'hétérogénéité d'épaisseur.In general, in the various known techniques listed above, the continuous application of a thin organic coating on metal substrates is carried out under low contact pressures, insufficient to allow a thin coating, uniformly and homogeneously applied on rigid substrates which may have flatness and thickness heterogeneity defects.

Ces différentes techniques d'application ne permettent pas de compenser les variations d'épaisseur du substrat métallique, qui induisent de ce fait des fluctuations inacceptables d'épaisseur du revêtement notamment dans le cas où le substrat est formé par une bande métallique qui présente une rugosité et/ou des ondulations de surface importantes d'amplitude égale ou supérieure à l'épaisseur du revêtement à réaliser sur ladite bande métallique.These different application techniques do not make it possible to compensate for variations in the thickness of the metal substrate, which consequently induce unacceptable variations in the thickness of the coating, particularly in the case where the substrate is formed by a metal strip which has a roughness and / or large surface corrugations with an amplitude equal to or greater than the thickness of the coating to be produced on said metal strip.

D'autre part, ces différentes techniques d'application ne permettent pas de s'accommoder des variations de largeur du substrat, ni des variations de positionnement transversal de ce substrat, de sorte que le revêtement ne peut pas être déposé de manière uniforme sur toute la largeur du substrat.On the other hand, these different application techniques do not allow to accommodate variations in the width of the substrate, nor variations in transverse positioning of this substrate, so that the coating can not be uniformly deposited on any the width of the substrate.

Enfin, lors de l'application du revêtement, des micro-bulles d'air peuvent s'intercaler entre le revêtement et le substrat ce qui nuit à l'application homogène et à l'aspect de surface de ce revêtement.Finally, during the application of the coating, microbubbles of air can be interposed between the coating and the substrate which affects the homogeneous application and the surface appearance of this coating.

Ainsi, l'application en continu d'un revêtement en polymère réticulable de faible épaisseur et uniforme sur une bande métallique pose des problèmes du fait que cette bande métallique présente des défauts de planéité et d'épaisseur ainsi qu'une rugosité et/ou des ondulations importantes d'amplitude égale ou supérieure à l'épaisseur du film de revêtement à déposer sur ladite bande même lorsque cette bande est plaquée sous une tension élevée sur un cylindre uniforme.Thus, the continuous application of a thin and uniform crosslinkable polymer coating on a metal strip poses problems because this metal strip has flatness and thickness defects as well as roughness and / or large corrugations of amplitude equal to or greater than the thickness of the coating film to be deposited on said strip even when this strip is plated under high tension on a uniform cylinder.

De plus, les différentes techniques utilisées jusqu'à présent ne permettent pas d'appliquer sur une bande métallique un revêtement de faible épaisseur en polymère réticulable exempt de solvant ou de diluant non réactif répondant à deux exigences contradictoires et qui sont la dureté et la déformabilité.In addition, the various techniques used up to now do not make it possible to apply to a metal strip a thin coating of crosslinkable polymer without solvent or non-reactive diluent meeting two contradictory requirements and which are the hardness and deformability .

En effet, après réticulation, le revêtement en polymère doit être suffisamment dur tout en étant déformable pour permettre la mise en forme des tôles ainsi revêtues sans provoquer une dégradation ou un décollement du revêtement.Indeed, after crosslinking, the polymer coating must be sufficiently hard while being deformable to allow the shaping of the sheets thus coated without causing degradation or detachment of the coating.

Or, on sait que l'élévation de la masse moléculaire des précurseurs réticulables du polymère est très favorable à l'obtention d'un revêtement final à la fois dur et déformable.However, it is known that the increase in the molecular weight of the crosslinkable precursors of the polymer is very favorable to obtaining a final coating that is both hard and deformable.

Mais, l'élévation de la masse moléculaire des précurseurs a un effet très défavorable sur la viscosité d'un polymère exempt de solvant ou de diluant non réactif ce qui nuit à la facilité de transfert et d'application de la nappe à l'état fondu non réticulé sur la bande métallique.However, the increase in the molecular weight of the precursors has a very unfavorable effect on the viscosity of a solvent-free polymer or a non-reactive diluent, which is detrimental to the ease of transfer and application of the web to the state. melted uncrosslinked on the metal strip.

Le document EP-A-1 001 848 cité selon l'article 54(3) CBE décrit un procédé de revêtement en continu d'au moins une bande métallique par un film fluide en polymère réticulable exempt de solvant ou de diluant et d'épaisseur inférieure à celle de la bande métallique, dans lequel on fait défiler en continu la bande métallique, on préchauffe ladite bande métallique à une température sensiblement égale ou supérieure à la température du film fluide en polymère réticulable et à la température de ramollissement de ce polymère réticulable, on forme par écoulement forcé, sur un cylindre preneur de surface dure, une nappe homogène et d'épaisseur uniforme dudit polymère réticulable, ledit cylindre preneur étant chauffé à une température sensiblement égale ou supérieure à la température de ladite nappe et à la température de ramollissement de ce polymère réticulable et entraîné en rotation dans le même sens que le cylindre de support de la bande métallique et on forme le film en polymère réticulable à une épaisseur uniforme sensiblement égale à l'épaisseur désirée, et on comprime, entre le cylindre preneur et la bande métallique, un élément applicateur de surface déformable, chauffé à une température sensiblement égale ou supérieure à la température du cylindre preneur et entraîné en rotation dans le même sens que le cylindre de support de la bande métallique.EP-A-1 001 848 cited in accordance with Article 54 (3) EPC discloses a process for continuously coating at least one metal strip with a crosslinkable polymer-free solvent-free or diluent-thick film and a thickness less than that of the metal strip, in which the metal strip is continuously scrolled, said metal strip is preheated to a temperature substantially equal to or greater than the temperature of the crosslinkable polymer fluid film and the softening temperature of this crosslinkable polymer a homogeneous sheet of uniform thickness of said crosslinkable polymer is formed by forced flow on a hard surface gripping cylinder, said gripping cylinder being heated to a temperature substantially equal to or greater than the temperature of said sheet and at the temperature of softening of this crosslinkable polymer and rotated in the same direction as the support roll of the metal band allique and form the crosslinkable polymer film to a uniform thickness substantially equal to the desired thickness, and is compressed between the gripper cylinder and the metal strip, a deformable surface applicator element, heated to a temperature substantially equal to or greater than the temperature of the gripper cylinder and rotated in the same direction as the support cylinder of the metal strip.

On connaît également dans le document US-A-5 407 702 un procédé et un dispositif de revêtement en continu d'une bande métallique par un film fluide en polyester de haute viscosité par défilement en continu de la bande métallique sur un cylindre de support, formation d'une nappe dudit polymère par écoulement forcé et sur un cylindre, puis dudit film à partir de ladite nappe, et transfert total en épaisseur dudit film sur la bande métallique.Also known in US-A-5 407 702 a method and a device for continuously coating a metal strip with a high viscosity polyester fluid film by continuously moving the metal strip on a support cylinder, forming a web of said polymer by forced flow and on a cylinder, then said film from said web, and total transfer in thickness of said film on the metal strip.

L'invention a pour but d'éviter ces inconvénients en proposant un procédé et un dispositif de revêtement en continu d'au moins une bande métallique par un film fluide et de faible épaisseur en polymère réticulable exempt de solvant ou de diluant non réactif et dont la température de ramollissement est supérieure à 50°C, permettant d'obtenir un revêtement d'épaisseur uniforme de quelques microns à quelques dizaines de microns appliqués d'une manière homogène sur cette bande, tout en évitant que des micro-bulles d'air s'intercalent entre le film et la bande métallique et en s'affranchissant des défauts de planéité et de rugosité de cette bande ainsi qu'en permettant une application sur une partie ou la totalité du revêtement et cela malgré les fluctuations de largeur et de positionnement transversal de cette bande.The aim of the invention is to avoid these drawbacks by proposing a method and a device for continuously coating at least one metal strip with a fluid film of small thickness made of crosslinkable polymer that is free of solvent or non-reactive diluent and whose the softening temperature is greater than 50 ° C, to obtain a coating of uniform thickness of a few microns to a few tens of microns applied in a homogeneous manner on this strip, while avoiding that microbubbles of air are inserted between the film and the metal strip and overcoming flatness and roughness defects of this band and by allowing an application on part or all of the coating and this despite variations in width and transverse positioning of this band.

L'invention a donc pour objet un procédé de revêtement en continu d'au moins une bande métallique par un film fluide en polymère réticulable exempt de solvant ou de diluant non réactif et dont la température de ramollissement est supérieure à 50°C, ledit film ayant une épaisseur inférieure à celle de la bande métallique, procédé dans lequel :

  • on fait défiler en continu la bande métallique sur au moins un cylindre de support,
  • on forme, sur un cylindre et par écoulement forcé à une température supérieure à la température de ramollissement du polymère réticulable, une nappe dudit polymère réticulable à l'état fondu possédant une viscosité supérieure à 10 Pa.s dans les conditions de formation de ladite nappe, la température de formation de cette nappe étant inférieure à la température de début de réticulation du polymère réticulable et ledit cylindre étant entraîné en rotation en sens inverse au sens de défilement de la bande métallique,
  • on forme, à partir de ladite nappe, ledit film en polymère réticulable,
  • on effectue un transfert total en épaisseur du film sur la bande métallique,
  • et, entre la zone de formation de la nappe sur le cylindre et la zone d'application du film sur la bande métallique, on conditionne thermiquement le polymère réticulable selon des modalités adaptées pour abaisser la viscosité de ce polymère réticulable d'au moins un facteur 2 par rapport à ladite viscosité mesurée dans les conditions dudit écoulement forcé.
The subject of the invention is therefore a process for continuously coating at least one metal strip with a fluid film made of a crosslinkable polymer that is free of solvent or non-reactive diluent and whose softening temperature is greater than 50.degree. having a thickness less than that of the metal strip, in which process:
  • the metal strip is continuously scrolled on at least one support cylinder,
  • forming on a cylinder and by forced flow at a temperature above the softening temperature of the crosslinkable polymer, a web of said polymer crosslinkable in the molten state having a viscosity greater than 10 Pa.s under the conditions of formation of said web , the formation temperature of this web being lower than the crosslinking polymer start temperature and said cylinder being rotated in the opposite direction to the running direction of the metal strip,
  • from said web, said crosslinkable polymer film is formed,
  • a total transfer in thickness of the film is carried out on the metal strip,
  • and, between the web-forming zone on the cylinder and the film application zone on the metal strip, the cross-linkable polymer is thermally conditioned in suitable ways to lower the viscosity of this cross-linkable polymer by at least one factor. 2 with respect to said viscosity measured under the conditions of said forced flow.

L'invention a également pour objet un dispositif de revêtement en continu d'au moins une bande métallique par un film fluide en polymère réticulable exempt de solvant ou de diluant non réactif et dont la température de ramollissement est supérieure à 50°C, ledit film ayant une épaisseur inférieure à celle de la bande métallique, dispositif comprenant:

  • des moyens d'entraînement en continu de la bande métallique,
  • au moins un cylindre de support de la bande métallique,
  • des moyens de formation, sur un cylindre et par écoulement forcé à une température supérieure à la température de ramollissement du polymère réticulable, d'une nappe dudit polymère réticulable à l'état fondu possédant une viscosité supérieure à 10Pa.s dans les conditions de formation de ladite nappe, la température de formation de cette nappe étant inférieure à la température de début de réticutation du polymère réticulable et ledit cylindre étant entraîné en rotation en sens inverse au sens de défilement de la bande métallique,
  • des moyens de formation, à partir de ladite nappe, dudit film en polymère réticulable et de transfert total en épaisseur de ce film sur la bande métallique,
  • et, entre la zone de formation de la nappe sur le cylindre et la zone d'application du film sur la bande métallique, des moyens de conditionnement thermique du polymère réticulable selon des modalités adaptées pour abaisser la viscosité de ce polymère réticulable d'au moins un facteur 2 par rapport à ladite viscosité mesurée dans les conditions dudit écoulement forcé.
The invention also relates to a device for continuously coating at least one metal strip with a crosslinkable polymer fluid film. solvent-free or non-reactive diluent and having a softening temperature above 50 ° C, said film having a thickness less than that of the metal strip, comprising:
  • means for continuously driving the metal strip,
  • at least one support cylinder of the metal strip,
  • means for forming, on a cylinder and by forced flow at a temperature above the softening temperature of the crosslinkable polymer, a web of said melt crosslinkable polymer having a viscosity of greater than 10 Pa.s under the formation conditions of said web, the formation temperature of this web being lower than the start of crosslinking of the crosslinkable polymer and said cylinder being rotated in the opposite direction to the running direction of the metal strip,
  • means for forming, from said sheet, said crosslinkable polymer film and for transferring the film thickness to the metal strip,
  • and, between the region of formation of the web on the cylinder and the zone of application of the film on the metal strip, thermal conditioning means of the crosslinkable polymer in suitable ways to lower the viscosity of this crosslinkable polymer of at least a factor 2 with respect to said viscosity measured under the conditions of said forced flow.

Les caractéristiques et avantages de l'invention apparaîtront au cours de la description qui va suivre, donnée uniquement à titre d'exemple et faite en référence aux dessins annexés, sur lesquels :

  • la Fig. 1 est une vue schématique en élévation d'une installation de revêtement d'une bande métallique par un film en polymère réticulable comportant un premier mode de réalisation d'un dispositif d'application de ce revêtement, conforme à l'invention,
  • la Fig. 2 est une vue schématique en perspective du dispositif d'application de la Fig. 1,
  • la Fig. 3 est une vue schématique en élévation d'une installation de revêtement d'une bande métallique par un film en polymère réticulable comportant un second mode de réalisation d'un dispositif d'application de ce revêtement, conforme à l'invention,
  • la Fig. 4 est une vue schématique en perspective du dispositif d'application de la Fig. 3,
  • les Figs. 5 et 6 sont deux vues schématiques en élévation des moyens d'enlèvement de l'excès de polymère réticulable.
The features and advantages of the invention will become apparent from the following description, given solely by way of example and with reference to the appended drawings, in which:
  • FIG. 1 is a schematic elevational view of an installation for coating a metal strip with a crosslinkable polymer film comprising a first embodiment of a device for applying this coating, according to the invention,
  • FIG. 2 is a schematic perspective view of the application device of FIG. 1
  • FIG. 3 is a diagrammatic elevational view of an installation for coating a metal strip with a crosslinkable polymer film comprising a second embodiment of a device for applying this coating, according to the invention,
  • FIG. 4 is a schematic perspective view of the application device of FIG. 3
  • Figs. 5 and 6 are two schematic views in elevation of the means for removing the excess crosslinkable polymer.

Sur les Figs. 1 et 3, on a représenté schématiquement deux installations de revêtement en continu d'une bande métallique 1 par un film en polymère réticulable fluide, exempt de solvant ou de diluant non réactif et d'épaisseur comprise par exemple entre 5 et 50µm.In Figs. 1 and 3, schematically shows two installations for continuously coating a metal strip 1 with a fluid crosslinkable polymer film, free of solvent or non-reactive diluent and having a thickness for example between 5 and 50 .mu.m.

Cette bande métallique 1 a une épaisseur comprise par exemple entre 0,10 et 4mm et est par exemple en acier ou en aluminium ou encore en alliage d'aluminium et peut être revêtue ou prépeinte sur l'une ou sur ses deux faces.This metal strip 1 has a thickness for example between 0.10 and 4 mm and is for example steel or aluminum or aluminum alloy and can be coated or prepainted on one or both sides.

Le polymère utilisé pour revêtir la bande métallique 1 est un polymère exempt de solvant ou de diluant non réactif et réticulable par voie thermique comme par exemple un polymère thermodurcissable ou par voie physique comme par exemple un polymère photopolymérisable.The polymer used to coat the metal strip 1 is a solvent-free polymer or non-reactive and thermally crosslinkable diluent such as a thermosetting polymer or physically such as a photopolymerizable polymer.

Ce polymère possède à l'état non réticulé une température de ramollissement supérieure à 50°C.This polymer has in the uncrosslinked state a softening temperature greater than 50 ° C.

Ces polymères ont des températures de ramollissement, de début d'écoulement, de début de réticulation et de réticulation rapide qui sont différentes.These polymers have different softening, start-flow, start-cross-cure and crosslinking temperatures.

D'une manière générale, la température de début de réticulation est la température à partir de laquelle on observe un accroissement de la viscosité supérieure à 10% en moins de 15 minutes.In general, the crosslinking start temperature is the temperature from which an increase in viscosity of greater than 10% is observed in less than 15 minutes.

Dans les exemples de réalisation représentés sur les Figs. 1 et 3, la bande métallique 1 est entraînée en défilement selon la flèche F et cette bande métallique 1 est en appui sur au moins un cylindre de support 3.In the exemplary embodiments shown in FIGS. 1 and 3, the metal strip 1 is driven in scrolling along the arrow F and the metal strip 1 is supported on at least one support cylinder 3.

Les installations comportent des moyens 2 de préchauffage de la bande métallique 1 à une température sensiblement égale ou supérieure à la température du film fluide en polymère réticulable à déposer ladite bande métallique 1 et à la température de ramollissement de ce polymère réticulable.The installations comprise means 2 for preheating the metal strip 1 at a temperature substantially equal to or greater than the temperature of the crosslinkable polymer fluid film to deposit said metal strip 1 and the softening temperature of this crosslinkable polymer.

Les moyens 2 de préchauffage de la bande métallique 1 sont constitués par exemple par au moins un four à induction.The means 2 for preheating the metal strip 1 are constituted for example by at least one induction furnace.

Ces installations comportent également, de l'amont à l'aval :

  • un dispositif désigné dans son ensemble par la référence 10 de revêtement de la bande métallique 1 par un film en polymère réticulable fluide, exempt de solvant ou de diluant non réactif et dont la température de ramollissement est supérieure à 50°C,
  • des moyens 5 de cuisson ou de réticulation du film en polymère réticulable,
  • et un bloc 7 de traction de la bande métallique 1.
These installations also include, from upstream to downstream:
  • a device generally designated by the reference numeral 10 for coating the metal strip 1 with a fluid crosslinkable polymer film, free of solvent or non-reactive diluent and having a softening temperature greater than 50 ° C,
  • means 5 for baking or crosslinking the crosslinkable polymer film,
  • and a block 7 of traction of the metal strip 1.

Dans le cas où le polymère est réticulable par voie thermique, les moyens 5 de cuisson comprennent par exemple au moins un four à induction et des moyens 6 de refroidissement et dans le cas où le polymère est réticulable par voie physique, les moyens 5 de cuisson peuvent être constitués par des lampes à rayons ultraviolets ou par des faisceaux d'électrons.In the case where the polymer is thermally crosslinkable, the cooking means comprise for example at least one induction furnace and cooling means and in the case where the polymer is physically crosslinkable, the cooking means may be constituted by ultraviolet lamps or by electron beams.

Le film en polymère réticulable à déposer sur la bande métallique 1 doit être d'épaisseur uniforme, bien que cette bande métallique 1 présente des hétérogénéités d'épaisseur ou des défauts de planéité ainsi qu'une rugosité et/ou des ondulations de surface importantes d'amplitudes égales ou supérieures à l'épaisseur du film à déposer sur la bande métallique 1.The crosslinkable polymer film to be deposited on the metal strip 1 must be of uniform thickness, although this metal strip 1 has thickness heterogeneities or flatness defects as well as roughness and / or significant surface ripples. amplitudes equal to or greater than the thickness of the film to be deposited on the metal strip 1.

D'une manière générale, le dispositif 10 de revêtement comporte:

  • des moyens 11 et 12 de formation, sur un cylindre 20 et par écoulement forcé à une température supérieure à la température de ramollissement du polymère réticulable, d'une nappe 30 dudit polymère réticulable à l'état fondu, possédant une viscosité supérieure à 10Pa.s et de préférence comprise entre 20Pa.s et 2000Pa.s dans les conditions de formation de ladite nappe 30, la température de formation de cette nappe 30 étant inférieure à la température de début de réticulation du polymère réticulable,
  • des moyens de formation, à partir de ladite nappe 30, du film 31 en polymère réticulable et de transfert total en épaisseur de ce film 31 sur la bande métallique 1,
  • et, entre la zone de formation de la nappe 30 sur le cylindre 20 et la zone d'application du film 31 sur la bande métallique 1, des moyens 15 de conditionnement thermique du polymère réticulable selon des modalités adaptées pour abaisser la viscosité de ce polymère réticulable à une valeur inférieure à ladite viscosité mesurée dans les conditions dudit écoulement forcé.
In general, the coating device 10 comprises:
  • means 11 and 12 for forming, on a cylinder 20 and by forced flow at a temperature above the softening temperature of the crosslinkable polymer, a web 30 of said melt-crosslinkable polymer having a viscosity of greater than 10 Pa. s and preferably between 20Pa.s and 2000Pa.s under the conditions of formation of said sheet 30, the formation temperature of this sheet 30 being lower than the crosslinking polymer start temperature,
  • forming means, from said web 30, of the film 31 of crosslinkable polymer and of total transfer in thickness of this film 31 on the metal strip 1,
  • and, between the zone of formation of the ply 30 on the cylinder 20 and the zone of application of the film 31 on the metal strip 1, means 15 for thermally conditioning the crosslinkable polymer in suitable ways to lower the viscosity of this polymer crosslinkable at a value less than said viscosity measured under the conditions of said forced flow.

Les moyens de formation par écoulement forcé de la nappe 30 en polymère réticulable comprennent par exemple une machine d'extrusion non représentée, de type classique, munie d'une filière 11 comportant une fente d'extrusion 12 et un organe de régulation de débit, non représenté, constitué par exemple par une pompe doseuse et disposé entre la machine d'extrusion et la filière 11.The forced flow forming means of the crosslinkable polymer ply 30 comprise, for example, an extrusion machine, not shown, of conventional type, provided with a spinneret 11 comprising an extrusion slot 12 and a flow control member, not shown, constituted for example by a metering pump and disposed between the extrusion machine and the die 11.

Selon un premier mode de réalisation de l'installation représenté sur les Figs. 1 et 2, les moyens de formation et de transfert total en épaisseur du film 31 en polymère réticulable sont formés par le cylindre 20 et par des moyens de mise en compression de la bande métallique 1 entre le cylindre 20 et le cylindre de support 3 pour obtenir un revêtement d'épaisseur homogène.According to a first embodiment of the installation shown in Figs. 1 and 2, the formation and total transfer means in thickness of the film 31 of crosslinkable polymer are formed by the cylinder 20 and by means for compressing the metal strip 1 between the cylinder 20 and the support cylinder 3 for obtain a coating of uniform thickness.

Un transfert est considéré comme total ou quasi-total en épaisseur lorsque plus de 90% de la matière ont été transférés.A transfer is considered to be total or almost total thickness when more than 90% of the material has been transferred.

Le cylindre 20 est chauffé à une température sensiblement égale ou supérieure, d'une part, à la température de formation de la nappe 30 et, d'autre part, à la température de ramollissement du polymère réticulable et est entraîné en rotation, par des moyens appropriés non représentés, dans un sens inverse au sens de défilement de la bande métallique 1, comme représenté par les flèches f1 sur les Figs. 1 et 2.The cylinder 20 is heated to a temperature substantially equal or greater, on the one hand, to the formation temperature of the web 30 and, on the other hand, to the softening temperature of the crosslinkable polymer and is rotated, by means of appropriate means not shown, in a reverse direction in the direction of travel of the metal strip 1, as represented by the arrows f1 in Figs. 1 and 2.

Par rapport au cylindre 3 de support de ladite bande métallique 1, le cylindre 20 est entraîné en rotation dans le même sens que ce cylindre 3.With respect to the support cylinder 3 of said metal strip 1, the cylinder 20 is rotated in the same direction as this cylinder 3.

Le cylindre 20 comporte une âme métallique revêtue d'une enveloppe en matériau déformable, comme par exemple un élastomère, et le cylindre de support 3 comporte une surface dure.The cylinder 20 comprises a metal core coated with an envelope of deformable material, such as an elastomer, and the support cylinder 3 has a hard surface.

Selon une variante, le cylindre 20 comporte une surface dure et le cylindre de support 3 comporte une âme métallique revêtue d'une enveloppe en matériau déformable comme par exemple un élastomère.According to a variant, the cylinder 20 has a hard surface and the support cylinder 3 comprises a metal core coated with an envelope of deformable material such as an elastomer.

La formation de la nappe 30 dudit polymère réticulable est réalisée par exemple par extrusion couchage ou par extrusion lamination.The formation of the web 30 of said crosslinkable polymer is carried out for example by extrusion coating or by extrusion lamination.

Dans le cas de l'extrusion couchage comme représenté à la Fig. 2, les moyens de formation par écoulement forcé de la nappe 30 sont formés par la filière 11 en appui contre la surface du cylindre 20 et munie de moyens de réglage, du type classique, de la position des bords de la fente d'extrusion 12 de ladite filière 11 par rapport à la surface du cylindre 20.In the case of the extrusion coating as shown in FIG. 2, the means for forming by forced flow of the sheet 30 are formed by the die 11 bearing against the surface of the cylinder 20 and provided with means of adjustment, of the conventional type, the position of the edges of the extrusion slot 12 of said die 11 relative to the surface of the cylinder 20.

La filière 11 de la machine d'extrusion donne la répartition uniforme de la nappe 30 qui est obtenue en jouant sur le débit de la filière 11 et sur la vitesse de rotation du cylindre 20.The die 11 of the extrusion machine gives the uniform distribution of the ply 30 which is obtained by adjusting the flow rate of the die 11 and the speed of rotation of the cylinder 20.

La filière 11 est appuyée sur le cylindre 20 par exemple au moyen de vérins, non représentés, dont la pression permet d'uniformiser le débit de fuite du polymère réticulable fluide.The die 11 is supported on the cylinder 20 for example by means of cylinders, not shown, the pressure of which makes it possible to standardize the leakage rate of the fluid crosslinkable polymer.

Du fait du parfait parallélisme de la filière 11 et du cylindre 20, il se forme sur ce dernier une nappe 30 d'épaisseur uniforme.Due to the perfect parallelism of the die 11 and the cylinder 20, a sheet 30 of uniform thickness is formed on the latter.

Dans le cas de l'extrusion lamination, comme représenté à la Fig. 3, les moyens de formation par écoulement forcé de la nappe 30 sont formés par la filière 11, des moyens d'étirage de la nappe 30 par ajustement du débit de cette filière 11 et/ou de la vitesse de rotation du cylindre applicateur 20, des moyens de réglage du type classique, de la position des bords de la fente d'extrusion 12 de ladite filière 11 par rapport à la surface du cylindre 20 et par des moyens, non représentés, de plaquage de la nappe 30 sur ladite surface du cylindre applicateur 20.In the case of lamination extrusion, as shown in FIG. 3, the means for forming by forced flow of the ply 30 are formed by the die 11, means for drawing the ply 30 by adjusting the flow rate of this spinneret 11 and / or the speed of rotation of the applicator roll 20, adjustment means of the conventional type, the position of the edges of the extrusion slot 12 of said die 11 relative to the surface of the cylinder 20 and by means of means, not shown, for plating the ply 30 on said surface of the applicator roll 20.

Les moyens de plaquage de la nappe 30 sur la surface du cylindre 20 sont formés par exemple par une lame d'air dirigée vers ce cylindre 20 au niveau de la génératrice de contact de ladite nappe 30 sur ledit cylindre applicateur 20.The plating means of the ply 30 on the surface of the cylinder 20 are formed for example by an air knife directed towards this cylinder 20 at the generatrix of contact of said ply 30 on said applicator cylinder 20.

Dans le mode de réalisation représenté sur les Figs. 3 et 4, les moyens de formation et de transfert total en épaisseur du film 31 en polymère réticulable sur la bande métallique 1 comprennent :

  • le cylindre 20 pour former, à partir de la nappe 30, une nappe intermédiaire 30b en polymère réticulable,
  • un élément 21 de transfert intermédiaire intercalé entre le cylindre 20 et la bande métallique 1 et entraîné en rotation en sens inverse au sens de défilement de la bande métallique 1 pour former, à partir de la nappe intermédiaire 30b le film 31 en polymère réticulable,
  • des moyens de mise en compression de l'élément de transfert 21 entre le cylindre 20 et le cylindre de support 3 pour transférer la nappe intermédiaire 30b sur ledit élément de transfert 21,
  • et des moyens de mise en compression de la bande métallique 1 entre le cylindre de transfert 21 et le cylindre de support 3 pour transférer le film 31 sur ladite bande métallique 1.
In the embodiment shown in Figs. 3 and 4, the forming means and total transfer in thickness of the film 31 of crosslinkable polymer on the metal strip 1 comprise:
  • the cylinder 20 for forming, from the sheet 30, an intermediate layer 30b made of crosslinkable polymer,
  • an intermediate transfer element 21 interposed between the cylinder 20 and the metal strip 1 and rotated in the opposite direction to the direction of travel of the metal strip 1 to form, from the intermediate layer 30b, the film 31 made of crosslinkable polymer,
  • means for compressing the transfer element 21 between the cylinder 20 and the support cylinder 3 to transfer the intermediate web 30b to said transfer element 21,
  • and means for compressing the metal strip 1 between the transfer cylinder 21 and the support cylinder 3 to transfer the film 31 to said metal strip 1.

Le cylindre 20 et le cylindre de support 3 comportent chacun une surface dure et l'élément de transfert est formé par un cylindre de transfert 21 ou cylindre applicateur comportant une âme métallique revêtue d'une enveloppe en matériau déformable, comme par exemple un élastomère.The cylinder 20 and the support cylinder 3 each comprise a hard surface and the transfer element is formed by a transfer cylinder 21 or applicator cylinder comprising a metal core coated with a casing of deformable material, such as an elastomer.

Selon une variante, le cylindre 20 et le cylindre de support 3 comportent chacun une âme métallique revêtue d'une enveloppe en matériau déformable, comme par exemple un élastomère, et l'élément de transfert est formé par un cylindre applicateur 21 de surface dure.According to a variant, the cylinder 20 and the support cylinder 3 each comprise a metal core coated with an envelope of deformable material, such as for example an elastomer, and the transfer element is formed by an applicator roll 21 of hard surface.

Selon encore une autre variante, l'élément de transfert est formé par une bande sans fin.According to yet another variant, the transfer element is formed by an endless band.

Dans chaque mode de réalisation, le cylindre 20, chauffé à une température sensiblement égale à la température de formation de la nappe 30 et à la température de ramollissement du polymère réticulable, est entraîné en rotation en sens inverse au sens de défilement de la bande métallique 1.In each embodiment, the cylinder 20, heated to a temperature substantially equal to the formation temperature of the web 30 and the softening temperature of the crosslinkable polymer, is rotated in the opposite direction to the running direction of the metal strip. 1.

Dans le cas du mode de réalisation représenté sur les Figs. 3 et 4, le cylindre applicateur 21 chauffé à une température sensiblement égale ou supérieure à la température du cylindre 20, est entraîné en rotation également en sens inverse au sens de défilement du cylindre de support 3 de la bande métallique 1, comme représenté par la flèche f2 sur la Fig. 3 et 4.In the case of the embodiment shown in Figs. 3 and 4, the applicator cylinder 21 heated to a temperature substantially equal to or greater than the temperature of the cylinder 20, is rotated also in the opposite direction to the direction of travel of the support cylinder 3 of the metal strip 1, as represented by FIG. arrow f2 in FIG. 3 and 4.

Le conditionnement thermique du polymère réticulable pendant le contact de la nappe 30 sur le cylindre 20 dans le cas du premier mode de réalisation représenté sur les Figs. 1 et 2 ou pendant le contact de la nappe intermédiaire 30b sur le cylindre 20 et/ou le contact du film 31 sur l'élément de transfert 21 dans le cas du mode de réalisation représenté sur les Figs. 3 et 4, pour abaisser la viscosité de ce polymère réticulable, peut être réalisé de différentes manières.The thermal conditioning of the crosslinkable polymer during the contact of the sheet 30 on the cylinder 20 in the case of the first embodiment shown in Figs. 1 and 2 or during the contact of the intermediate web 30b on the cylinder 20 and / or the contact of the film 31 on the transfer element 21 in the case of the embodiment shown in Figs. 3 and 4, to lower the viscosity of this crosslinkable polymer, can be achieved in different ways.

Selon un premier mode de réalisation, les moyens de conditionnement thermiques du polymère réticulable sont formés par un système de chauffage interne du cylindre 20 et/ou du cylindre applicateur 21 et/ou par au moins une source 15 d'application d'un flux thermique complémentaire sur la nappe 30 ou sur la nappe intermédiaire 30b et/ou sur le film 31.According to a first embodiment, the heat-conditioning means of the crosslinkable polymer are formed by an internal heating system of the cylinder 20 and / or the applicator cylinder 21 and / or by at least one source 15 for applying a heat flux. complementary to the ply 30 or to the intermediate ply 30b and / or to the film 31.

Selon un second mode de réalisation, les moyens de conditionnement thermique du polymère réticulable sont formés par un système de chauffage interne du cylindre 20 et/ou par un système de chauffage externe du cylindre applicateur 21 et/ou par au moins une source 15 d'application d'un flux thermique complémentaire sur la nappe 30 ou sur la nappe intermédiaire 30b et/ou sur le film 31.According to a second embodiment, the thermal conditioning means of the crosslinkable polymer are formed by an internal heating system of the cylinder 20 and / or by an external heating system of the applicator roll 21 and / or by at least one source 15 of applying a complementary thermal flux to the ply 30 or to the intermediate ply 30b and / or to the film 31.

Le système de chauffage interne du cylindre 20 et/ou du cylindre applicateur 21 est constitué par des résistances électriques noyées dans la masse de chacun desdits cylindres ou par des canaux ménagés dans lesdits cylindres pour la circulation d'un fluide caloporteur, comme par exemple de l'huile.The internal heating system of the cylinder 20 and / or the applicator cylinder 21 is constituted by electrical resistances embedded in the mass of each of said cylinders or by channels formed in said cylinders for the circulation of a coolant, such as for example oil.

Dans le cas où les cylindres 20 et 21 comportent une enveloppe externe en matériau déformable, la température de ces cylindres doit être réglée, par exemple au moyen d'un thermocouple non représenté, afin de ne pas dépasser une valeur limite pour éviter d'endommager l'enveloppe externe en matériau déformable par une température trop élevée et de détériorer la couche de liaison entre le matériau déformable et l'âme métallique desdits cylindres.In the case where the cylinders 20 and 21 comprise an outer envelope of deformable material, the temperature of these cylinders must be adjusted, for example by means of a not shown thermocouple, in order not to exceed a limit value to avoid damaging the outer envelope of deformable material by too high a temperature and to deteriorate the bonding layer between the deformable material and the metal core of said cylinders.

Dans le cas d'un système de chauffage externe de la surface du cylindre 20 et/ou du cylindre applicateur 21, ce système de chauffage, non représenté, est disposé en regard du cylindre correspondant dans la zone non recouverte par le film 31 et est constitué par exemple par des générateurs d'air chaud ou des lampes à infrarouge.In the case of an external heating system of the surface of the cylinder 20 and / or the applicator cylinder 21, this heating system, not shown, is arranged facing the corresponding cylinder in the zone not covered by the film 31 and is consisting for example of hot air generators or infrared lamps.

La ou les sources 15 d'application du flux thermique complémentaire sur le film 31 ou sur la nappe intermédiaire 30b et/ou sur le film 31 sont constitués par exemple par des lampes à infrarouge de moyenne longueur d'ondes d'absorption comprises entre 1,5 et 4µm ou par des générateurs d'air chaud ou encore par des systèmes à micro-ondes.The source or sources of application of the complementary heat flux on the film 31 or on the intermediate layer 30b and / or on the film 31 consist for example of infrared lamps of medium absorption wavelength between 1 , 5 and 4μm or by hot air generators or by microwave systems.

Les moyens de conditionnement thermique du polymère réticulable selon des modalités adaptées permettent donc d'abaisser la viscosité de ce polymère c'est à dire la fluidité du polymère afin de faciliter son transfert et son application sur la bande métallique 1.The heat-conditioning means of the cross-linkable polymer in suitable modalities therefore make it possible to lower the viscosity of this polymer, ie the fluidity of the polymer, in order to facilitate its transfer and its application on the metal strip 1.

Les modalités sont adaptées pour abaisser la viscosité du polymère réticulable d'au moins un facteur 2, et pour que la température dudit polymère réticulable dépasse la température de début de réticulation de ce polymère.The modalities are adapted to lower the viscosity of the crosslinkable polymer by at least a factor of 2, and for the temperature of said crosslinkable polymer to exceed the crosslinking start temperature of this polymer.

Ainsi, malgré l'augmentation de la température du polymère réticulable à un niveau habituellement considéré comme susceptible de provoquer un début de réticulation et donc une augmentation de la viscosité, cette viscosité conserve au moins de manière transitoire un niveau très faible facilitant le transfert et l'application du film 31 en polymère réticulable sur la bande métallique 1.Thus, despite the increase in the temperature of the crosslinkable polymer to a level usually considered likely to cause a beginning of crosslinking and therefore an increase in viscosity, this viscosity retains at least transiently a very low level facilitating the transfer and the application of the film 31 crosslinkable polymer on the metal strip 1.

De plus, le dispositif de revêtement 10 comprend des moyens, non représentés, de type classique, de réglage des vitesses tangentielles du cylindre 20 ou du cylindre 20 et du cylindre applicateur 21 dans un rapport compris entre 0,5 et 2 fois la vitesse de défilement de la bande métallique 1.In addition, the coating device 10 comprises means, not shown, of conventional type, for adjusting the tangential speeds of the cylinder 20 or the cylinder 20 and the applicator roll 21 in a ratio between 0.5 and 2 times the running speed of the metal strip 1.

Les vitesses du cylindre 20 ou du cylindre 20 et du cylindre applicateur 21 peuvent être réglées indépendamment l'une de l'autre.The speeds of the cylinder 20 or the cylinder 20 and the applicator roll 21 can be adjusted independently of one another.

Le dispositif de revêtement 10 comprend aussi des moyens, non représentés, de réglage de la pression de contact entre le cylindre 20 et la bande métallique 1 (Figs. 1 et 2) et, d'une part, entre le cylindre 20 et le cylindre applicateur 21 et, d'autre part, entre le cylindre applicateur 21 et la bande métallique 1 (Figs. 3 et 4).The coating device 10 also comprises means (not shown) for adjusting the contact pressure between the cylinder 20 and the metal strip 1 (FIGS 1 and 2) and, on the one hand, between the cylinder 20 and the cylinder applicator 21 and, on the other hand, between the applicator roll 21 and the metal strip 1 (Figs 3 and 4).

Ces moyens sont constitués par exemple par des vérins hydrauliques ou des systèmes vis/écrou qui permettent d'ajuster les pressions de contact en fonction de la viscosité du polymère réticulable de manière à assurer un transfert total de la matière et à minimiser les efforts de friction.These means consist, for example, of hydraulic cylinders or screw / nut systems which make it possible to adjust the contact pressures as a function of the viscosity of the crosslinkable polymer so as to ensure a total transfer of the material and to minimize the friction forces. .

Ainsi que représenté sur les Figs. 2 et 4, la fente d'extrusion 12 de la filière 11 ainsi que le cylindre 20 ou que le cylindre 20 et le cylindre applicateur 21 ont une longueur supérieure à la largeur de la bande métallique 1 de façon à revêtir toute la surface de la face de cette bande métallique 1 en contact avec le cylindre 20 ou le cylindre applicateur 21.As shown in Figs. 2 and 4, the extrusion slot 12 of the die 11 and the cylinder 20 or the cylinder 20 and the applicator roll 21 have a length greater than the width of the metal strip 1 so as to coat the entire surface of the face of this metal strip 1 in contact with the cylinder 20 or the applicator cylinder 21.

Selon une variante, la fente d'extrusion 12 de la filière 11 et le cylindre 20 ou le cylindre 20 et le cylindre applicateur 21 peuvent avoir une longueur inférieure à la largeur de la bande métallique 1 pour ne revêtir qu'une partie de la surface de la face de ladite bande métallique 1 en contact avec le cylindre 20 ou le cylindre applicateur 21.According to one variant, the extrusion slot 12 of the die 11 and the cylinder 20 or the cylinder 20 and the applicator roll 21 may have a length less than the width of the metal strip 1 to coat only part of the surface the face of said metal strip 1 in contact with the cylinder 20 or the applicator roll 21.

Selon le premier mode de réalisation représenté sur les Figs. 1 et 2, l'application du film 31 fluide et de faible épaisseur en polymère réticulable par voie thermique ou par voie physique est réalisée de la façon suivante.According to the first embodiment shown in Figs. 1 and 2, the application of the thin and thin film 31 of thermally or physically crosslinkable polymer is carried out as follows.

La bande métallique 1 est maintenue à une température égale ou supérieure à la température de ramollissement du polymère réticulable et le cylindre 20 est entraîné en rotation en sens inverse au sens de défilement de cette bande métallique 1.The metal strip 1 is maintained at a temperature equal to or greater than the softening temperature of the crosslinkable polymer and the cylinder 20 is rotated in the opposite direction to the running direction of this metal strip 1.

A titre d'exemple, la bande métallique 1 est préchauffée à une température de 140°C immédiatement avant son passage sur le cylindre de support 3 et elle défile à une vitesse de 30m/min.For example, the metal strip 1 is preheated to a temperature of 140 ° C immediately before passing on the support cylinder 3 and scrolls at a speed of 30m / min.

A la sortie de la filière 11 de la machine d'extrusion, la nappe 30 formée par écoulement forcé à une température supérieure à la température de ramollissement du polymère réticulable à l'état non réticulé, est plaquée sur le cylindre 20 de façon à former le film 31 en polymère réticulable d'épaisseur uniforme correspondant sensiblement à l'épaisseur du revêtement à former sur la bande métallique 1.At the outlet of the die 11 of the extrusion machine, the sheet 30 formed by forced flow at a temperature above the softening temperature of the crosslinkable polymer in the uncrosslinked state, is pressed onto the cylinder 20 so as to form the film 31 of crosslinkable polymer of uniform thickness substantially corresponding to the thickness of the coating to be formed on the metal strip 1.

Du fait de la pression exercée sur la bande métallique 1 par le cylindre 20 et le cylindre de support 3, l'ensemble ou une partie du film 31 en largeur est transféré du cylindre 20 sur la surface de la bande métallique 1 à revêtir.Due to the pressure exerted on the metal strip 1 by the cylinder 20 and the support cylinder 3, all or a portion of the film 31 in width is transferred from the cylinder 20 to the surface of the metal strip 1 to be coated.

Ensuite, la bande métallique 1 ainsi revêtue passe dans les moyens 5 de cuisson, puis dans les moyens 6 de refroidissement du film 31 en polymère réticulable.Then, the metal strip 1 thus coated passes into the cooking means 5, then into the cooling means 6 of the film 31 of crosslinkable polymer.

Dans le cas du second mode de réalisation représenté sur les Figs. 3 et 4, l'application du film 31 fluide et de faible épaisseur en polymère réticulable par voie thermique ou par physique est réalisée de la façon suivante.In the case of the second embodiment shown in Figs. 3 and 4, the application of the thin and thin film 31 of thermally or physically curable polymer is carried out as follows.

La bande métallique 1 est maintenue à une température égale ou supérieure à la température de ramollissement du polymère réticulable à l'état non réticulé et les cylindres 20 et 21 sont entraînés en rotation dans un sens inverse au sens de défilement de la bande métallique 1.The metal strip 1 is maintained at a temperature equal to or greater than the softening temperature of the crosslinkable polymer in the uncrosslinked state and the rolls 20 and 21 are rotated in a direction opposite to the running direction of the metal strip 1.

A la sortie de la filière 12 de la machine d'extrusion, la nappe 30 formée par écoulement forcé à une température supérieure à la température de ramollissement du polymère réticulable, est plaquée sur le cylindre 20 de façon à former la nappe intermédiaire 30b en polymère réticulable d'épaisseur uniforme.At the outlet of the die 12 of the extrusion machine, the sheet 30 formed by forced flow at a temperature above the softening temperature of the crosslinkable polymer, is pressed onto the cylinder 20 so as to form the intermediate layer 30b of polymer crosslinkable of uniform thickness.

Du fait de la pression exercée par le cylindre 20 et la bande métallique 1 sur le cylindre applicateur 21, la nappe intermédiaire 30b est transférée du cylindre 20 sur le cylindre applicateur 21 qui forme le film 31 et ce film 31 est transféré du cylindre applicateur 21 sur la surface de la bande métallique 1 à revêtir.Due to the pressure exerted by the cylinder 20 and the metal strip 1 on the applicator roll 21, the intermediate web 30b is transferred from the roll 20 to the applicator roll 21 which forms the film 31 and this film 31 is transferred from the applicator roll 21 on the surface of the metal strip 1 to be coated.

Ensuite, la bande métallique 1 ainsi revêtue passe dans les moyens 5 de cuisson, puis dans les moyens 6 de refroidissement du film 31 en polymère réticulable.Then, the metal strip 1 thus coated passes into the cooking means 5, then into the cooling means 6 of the film 31 of crosslinkable polymer.

Le film 31 en polymère réticulable peut être déposé sur une bande métallique nue en acier ou en aluminium ou en alliage d'aluminium ou sur une bande métallique pré-revêtue ou prépeinte.The crosslinkable polymer film 31 may be deposited on a bare metal strip of steel or aluminum or aluminum alloy or on a pre-coated or prepainted metal strip.

Le revêtement ainsi réalisé sur la bande métallique 1 a par exemple une épaisseur comprise entre 5 et 50µm avec une uniformité d'épaisseur de quelques microns et cela malgré les défauts notables de planéité ou d'hétérogénéité d'épaisseur de la bande métallique 1.The coating thus produced on the metal strip 1 has for example a thickness of between 5 and 50 μm with a uniformity of thickness of a few microns and this despite the notable defects of flatness or thickness heterogeneity of the metal strip 1.

D'autres moyens de formation par écoulement forcé de la nappe 30 peuvent également être utilisés.Other forced flow forming means of the web 30 may also be used.

Ainsi, les moyens de formation par écoulement forcé de la nappe 30 peuvent être formés par un bloc rigide en polymère réticulable appliqué sous pression contrôlée pour déposer des particules de polymère réticulable sur le cylindre 20 et former ladite nappe 30 ou encore par un système de transfert sous un champ électrostatique d'une poudre en polymère réticulabte sur ce cylindre 20 pour former cette nappe 30.Thus, the means for forming by forced flow of the sheet 30 may be formed by a rigid block of crosslinkable polymer applied under controlled pressure to deposit crosslinkable polymer particles on the cylinder 20 and form said sheet 30 or by a transfer system under an electrostatic field of a polymer powder crosslinkable on the cylinder 20 to form this web 30.

Selon d'autres variantes, les moyens de formation par écoulement forcé de la nappe 30 peuvent être formés par un système de projection de polymère réticulable fluide sur le cylindre 20 ou par un système d'application sur ce cylindre 20 d'une bande continue en polymère réticulable préalablement réalisée pour former ladite nappe 30.According to other variants, the means for forming by forced flow of the ply 30 may be formed by a fluid crosslinkable polymer spraying system on the cylinder 20 or by an application system on this cylinder 20 of a continuous strip. crosslinkable polymer previously produced to form said web 30.

Selon une autre variante, les moyens de formation par écoulement forcé de la nappe 30 peuvent être formés par une barre rotative disposée entre la filière 12 et ce cylindre 20.According to another variant, the means for forming by forced flow of the sheet 30 may be formed by a rotating bar disposed between the die 12 and this cylinder 20.

La nappe 30 et le film 31 en polymère réticulable peuvent avoir une largeur inférieure à la largeur de la bande métallique 1 pour revêtir qu'une partie de cette bande métallique 1 ou une largeur supérieure à la largeur de cette bande métallique 1 pour revêtir la totalité de ladite bande métallique 1.The web 30 and the cross-linkable polymer film 31 may have a width less than the width of the metal strip 1 to coat a part of this metal strip 1 or a width greater than the width of this metal strip 1 to coat the entire of said metal strip 1.

Dans le cas où la nappe 30 et le film 31 ont une largeur supérieure à la bande métallique 1, comme représentée sur les figures, il subsiste de part et d'autre de la zone utile d'application sur ladite bande métallique 1, une portion de polymère réticulable qui n'est pas appliquée sur cette bande métallique 1.In the case where the ply 30 and the film 31 have a width greater than the metal strip 1, as shown in the figures, there remains either side of the useful area of application on said metal strip 1, a crosslinkable polymer portion which is not applied to this metal strip 1.

Cet excès de polymère réticulable doit être enlevé afin d'éviter qu'il crée une surépaisseur sur le cylindre 20 ou sur le cylindre applicateur 21.This excess cross-linkable polymer must be removed in order to prevent it from creating an excess thickness on the cylinder 20 or on the applicator roll 21.

En effet, étant donné l'espace qu'il subsiste entre le cylindre 20 et le cylindre de support 3 ou le cylindre applicateur 21 et le cylindre de support 3, de part et d'autre de la bande métallique 1 et du fait de l'épaisseur de cette bande métallique 1, l'excès de polymère réticulable reste sur le cylindre 20 ou sur le cylindre applicateur 21.Indeed, given the space that remains between the cylinder 20 and the support cylinder 3 or the applicator cylinder 21 and the support cylinder 3, on either side of the metal strip 1 and because of the the thickness of this metal strip 1, the excess crosslinkable polymer remains on the cylinder 20 or on the applicator cylinder 21.

Pour enlever cet excès de matière, plusieurs solutions sont envisageables.To remove this excess material, several solutions are possible.

Pour cela, le dispositif de revêtement 10 est équipé de moyens 40 d'enlèvement de l'excès de polymère réticulable déposé sur le cylindre 20.For this, the coating device 10 is equipped with means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20.

Selon un premier mode de réalisation représenté sur les figures 1 et 2, les moyens 40 d'enlèvement de l'excès de polymère réticulable déposé sur le cylindre 20 sont formés par deux raclés, respectivement 41a et 41b, par exemple métalliques, en contact avec le cylindre 20 dans chaque zone située à l'extérieur de la zone en contact dudit cylindre 20 avec la bande métallique 1.According to a first embodiment shown in Figures 1 and 2, the means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20 are formed by two scraped, respectively 41a and 41b, for example metal, in contact with the cylinder 20 in each zone located outside the zone in contact with the cylinder 20 with the metal strip 1.

Les racles 41a et 41b en contact avec le cylindre 20 sont disposées en amont de la génératrice d'application de la nappe 30 sur ce cylindre 20 par rapport au sens de rotation dudit cylindre 20.The doctor blades 41a and 41b in contact with the cylinder 20 are arranged upstream of the generatrix for applying the ply 30 to this cylinder 20 with respect to the direction of rotation of said cylinder 20.

La position transversale des rades 41a et 41b sur le cylindre 20 peut être assujettie, par des moyens appropriés non représentés, à la largeur de la bande métallique 1 et/ou à la position transversale de cette bande métallique 1 sur le cylindre de support 3.The transverse position of the rades 41a and 41b on the cylinder 20 may be secured, by appropriate means, not shown, to the width of the metal strip 1 and / or to the transverse position of this metal strip 1 on the support cylinder 3.

En effet, la position de cette bande métallique 1 sur le cylindre de support 3 peut varier.Indeed, the position of this metal strip 1 on the support cylinder 3 may vary.

Les racles 41a et 41b sont donc en contact avec le cylindre 20 et enlèvent l'excès de polymère réticulable par frottement sur ledit cylindre 20.The doctor blades 41a and 41b are thus in contact with the cylinder 20 and remove the excess of crosslinkable polymer by friction on said cylinder 20.

Selon une variante, les moyens 40 d'enlèvement de l'excès de polymère réticulable sur le cylindre 20 peuvent êtres formés par deux cylindres de récupération disposés entre les racles 41a et 41b et le cylindre 20.According to one variant, the means 40 for removing the excess crosslinkable polymer on the cylinder 20 may be formed by two recovery cylinders arranged between the scrapers 41a and 41b and the cylinder 20.

Selon encore une autre variante, les moyens d'enlèvement de l'excès de polymère réticulable sur le cylindre 20 peuvent être formés par un cylindre de récupération intercalé entre le cylindre 20 et une racle ayant une longueur au moins égale à la longueur du cylindre 20.According to yet another variant, the means for removing the excess crosslinkable polymer on the cylinder 20 may be formed by a recovery cylinder interposed between the cylinder 20 and a doctor blade having a length at least equal to the length of the cylinder 20 .

Dans le cas du mode de réalisation représenté sur les Figs. 3 et 4, l'excès de matière qui n'a pas été déposé sur la bande métallique 1 reste sur le cylindre applicateur 21 et est transféré sur le cylindre 20 du fait de la pression exercée sur ledit cylindre applicateur 21.In the case of the embodiment shown in Figs. 3 and 4, the excess material that has not been deposited on the metal strip 1 remains on the applicator roll 21 and is transferred onto the roll 20 because of the pressure exerted on said applicator roll 21.

Dans ce cas, les moyens 40 d'enlèvement de l'excès de polymère réticulable déposé sur le cylindre 20 sont formés par au moins une racle, par exemple, métallique en contact avec le cylindre 20.In this case, the means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20 are formed by at least one squeegee, for example metal, in contact with the cylinder 20.

Selon un exemple de réalisation représenté sur les Figs. 4 et 5, les moyens 40 d'enlèvement de l'excès de polymère réticulable déposé sur le cylindre 20 sont formés par deux racles, respectivement 42a et 42b, par exemple métalliques en contact chacune avec le bord latéral du cylindre 20 en amont de la génératrice d'application de la nappe 30 sur ce cylindre 20.According to an exemplary embodiment shown in FIGS. 4 and 5, the means 40 for removing the excess crosslinkable polymer deposited on the cylinder 20 are formed by two doctor blades, respectively 42a and 42b, for example metal, each in contact with the lateral edge of the cylinder 20 upstream of the generator for applying the ply 30 to this cylinder 20.

De préférence, la positon transversale des racles 42a et 42b sur le cylindre 20 est assujettie par des moyens appropriés, non représentés, à la largeur de la bande métallique 1 et/ou à la position transversale de cette bande métallique 1 sur le cylindre de support 3.Preferably, the transverse position of the doctor blades 42a and 42b on the cylinder 20 is secured by appropriate means, not shown, to the width of the metal strip 1 and / or to the transverse position of this metal strip 1 on the support cylinder 3.

Les racles 42a et 42b sont donc en contact avec le cylindre 20 et enlèvent l'excès de polymère réticulable par frottement sur ledit cylindre 20.The doctor blades 42a and 42b are thus in contact with the cylinder 20 and remove the excess of crosslinkable polymer by friction on said cylinder 20.

La seconde solution consiste à équiper le cylindre applicateur 21 de moyens 40 d'enlèvement de l'excès de polymère réticulable.The second solution consists in equipping the applicator cylinder 21 with means 40 for removing the excess crosslinkable polymer.

Ainsi que représenté à la Fig. 6, ces moyens 40 d'enlèvement de l'excès polymère réticulable sur le cylindre applicateur 21 sont formés par un cylindre de récupération 22 en contact avec le cylindre applicateur 21, et par au moins une racle 43 en contact avec ledit cylindre de récupération 22.As shown in FIG. 6, these means 40 for removing the crosslinkable polymer excess on the applicator roll 21 are formed by a recovery cylinder 22 in contact with the applicator roll 21, and by at least one squeegee 43 in contact with said recovery roll 22 .

Ainsi, l'excès de polymère réticulable déposé sur le cylindre applicateur 21 est transféré sur le cylindre de récupération 22 du fait de la pression exercée par ledit cylindre de récupération sur le cylindre applicateur 21 et cet excès de polymère réticulable est enlevé du cylindre de récupération 22 par la racle 43.Thus, the excess crosslinkable polymer deposited on the applicator cylinder 21 is transferred to the recovery cylinder 22 because of the pressure exerted by said recovery cylinder on the applicator cylinder 21 and this excess crosslinkable polymer is removed from the recovery cylinder 22 by the squeegee 43.

Selon un autre mode de réalisation, les moyens d'enlèvement de l'excès de polymère réticulable sur le cylindre applicateur 21 peuvent être formés par un cylindre de récupération 22 et par deux racles en contact chacune avec un bord latéral dudit cylindre de récupération 22.According to another embodiment, the means for removing the excess crosslinkable polymer on the applicator roll 21 may be formed by a recovery cylinder 22 and by two scrapes each in contact with a lateral edge of said recovery cylinder 22.

Ces deux derniers modes de réalisation peuvent également s'appliquer pour l'installation représentée sur les Figs. 1 et 2.These last two embodiments can also be applied for the installation shown in Figs. 1 and 2.

Les moyens d'enlèvement de l'excès de polymère réticulable déposé sur le cylindre 20 ou sur le cylindre applicateur 21 évitent d'avoir à ajouter des inserts au niveau de la fente 12 de la filière d'extrusion 11 de façon à calibrer dès sa sortie la filière 12 la nappe 30 en polymère réticulable et de s'accommoder des variations de largeur et de positionnement transversal de la bande métallique 1 dans les limites de tolérance prédéfinies.The means for removing the excess crosslinkable polymer deposited on the cylinder 20 or the applicator roll 21 avoids having to add inserts at the slot 12 of the extrusion die 11 so as to calibrate as soon as leaving the die 12 the web 30 of crosslinkable polymer and to accommodate variations in width and transverse positioning of the metal strip 1 within the predefined tolerance limits.

Selon une variante, le point d'application du film 31 du polymère réticulable peut être située à un autre emplacement qu'en face du cylindre de support 3 de la bande métallique 1 et, par exemple sur un bras libre tendu de cette bande métallique 1 en aval dudit cylindre de support 3.According to one variant, the point of application of the film 31 of the crosslinkable polymer may be located at a different location than in front of the support cylinder 3 of the metal strip 1 and, for example, on a free arm stretched by this metal strip 1 downstream of said support cylinder 3.

Selon une variante, les deux faces de la bande métallique 1 peuvent être revêtues par un film 31 en polymère réticulable.According to one variant, the two faces of the metal strip 1 can be coated with a film 31 of crosslinkable polymer.

Dans ce cas, un dispositif 10 d'application du film 31 est disposé d'un côté de la bande métallique 1 et un autre dispositif d'application du film 31 est disposé de l'autre côté de ladite bande métallique 1.In this case, a device 10 for applying the film 31 is disposed on one side of the metal strip 1 and another film application device 31 is disposed on the other side of said metal strip 1.

L'application du film 31 sur chaque face de la bande métallique 1 peut être décalée ou simultanée. Pour une application simultanée, le cylindre de support 3 est supprimé et remplacé par un cylindre applicateur du second dispositif d'application. Le cylindre applicateur de chaque dispositif forme un cylindre de support de la bande métallique.The application of the film 31 on each side of the metal strip 1 may be shifted or simultaneous. For simultaneous application, the support cylinder 3 is removed and replaced by an applicator cylinder of the second application device. The applicator roll of each device forms a support cylinder of the metal strip.

Par ailleurs, la position transversale de la filière d'extrusion 11 peut être centrée en permanence par rapport à la bande métallique 1 en disposant cette filière d'extrusion 11 sur un support mobile transversalement et en reliant cette filière à la machine d'extrusion par un flexible ce qui permet d'asservir la position de cette filière d'extrusion 11 par rapport à la bande métallique 1 en fonction des variations de la position transversale de ladite bande métallique 1 par rapport au cylindre du support 3.Furthermore, the transverse position of the extrusion die 11 may be permanently centered with respect to the metal strip 1 by arranging this extrusion die 11 on a transversely movable support and by connecting this die to the extrusion machine by a flexible which makes it possible to slave the position of this extrusion die 11 with respect to the metal strip 1 as a function of the variations of the transverse position of said metal strip 1 relative to the cylinder of the support 3.

Selon encore une autre variante, un lubrifiant peut être déposé sur le cylindre applicateur 20 à l'extérieur de la zone en contact avec la bande métallique 1 de façon à faciliter le fonctionnement des racles 41a et 41b pour l'enlèvement de l'excès de polymère réticulable.According to yet another variant, a lubricant may be deposited on the applicator roll 20 outside the zone in contact with the metal strip 1 so as to facilitate the operation of the squeegees 41a and 41b for the removal of the excess of crosslinkable polymer.

A titre d'exemple, la formulation du mélange de polymère réticulable est réalisée comme suit :

  • 85% en poids d'un polyester polyol dénommé URALAC P1460 de la société DSM Resins (pays Bas) présentant les caractéristiques suivantes :
  • Nombre moyen de -OH par molécules ; F OH.moy = 3
  • Indice d'hydroxyle du polyol IOH   = 37 à 47
  • Masse molaire moyenne (en masse) Mw   = 20000g/mole
  • Masse molaire moyenne (en nombre de molécule) Mn = 4090
  • Indice de polydispersité Mw/Mn : Ip   = 4,9
(L'indice d'hydroxyle du polyol IOH étant défini comme la quantité nécessaire de potasse - en mg - pour neutraliser toutes les fonctions hydroxyle ; on a donc : F OH.moy = I OH x M n /56100)
  • comme durcisseur, 15% en masse d'isocyanate bloqué dénommé VESTAGON BF 1540 de la société HÜLS, constitué essentiellement d'urétidione d'IPDI.
  • Nombre moyen de - NCO par molécule : Fiso.moy = 2
  • Température de fusion comprise entre 105°C et 115°C
  • Température de déblocage de réticulation   = 160°C
  • Quantité totale de radicaux NCO   = 14,7 à 16% massique
  • Proportion radicaux NCO libres (non bloqués) < 1% massique,
  • viscosité pour une vitesse de cisaillement de 10s-1 :
    • . à 120°C :   900 Pa.s
    • . à 130°C :   400 Pa.s
    • . à 140°C :   180 Pa.s
    • . à 150°C :   80 Pa.s
By way of example, the formulation of the crosslinkable polymer mixture is carried out as follows:
  • 85% by weight of a polyester polyol called URALAC P1460 from DSM Resins (Netherlands) having the following characteristics:
  • Average number of -OH per molecule; F OH.moy = 3
  • Hydroxyl number of polyol I OH = 37 to 47
  • Molar mass average (mass) M w = 20000g / mole
  • Molar mass average (in number of molecules) M n = 4090
  • Polydispersity index M w / M n : I p = 4.9
(The hydroxyl number of the polyol I OH being defined as the necessary quantity of potash - in mg - to neutralize all the hydroxyl functions, we have: F OH.moy = I OH x M not / 56100)
  • as curing agent, 15% by weight of blocked isocyanate called VESTAGON BF 1540 from HÜLS, consisting essentially of uretidione of IPDI.
  • Average number of - NCO per molecule: F iso.moy = 2
  • Melting temperature between 105 ° C and 115 ° C
  • Crosslinking deblocking temperature = 160 ° C
  • Total amount of NCO radicals = 14.7 to 16% by mass
  • Free (non-blocked) NCO radical proportion <1% by mass,
  • viscosity for a shear rate of 10s -1 :
    • . at 120 ° C: 900 Pa.s
    • . at 130 ° C: 400 Pa.s
    • . at 140 ° C: 180 Pa.s
    • . at 150 ° C: 80 Pa.s

Ce mélange est entièrement à l'état fluide et/ou visqueux à partir d'une température égale à 120°C et sa température de réticulation rapide est comprise entre 170° et 250°C.This mixture is entirely in the fluid and / or viscous state starting from a temperature equal to 120 ° C. and its rapid cross-linking temperature is between 170 ° and 250 ° C.

Le polymère réticulable peut être également pigmenté et chargé par exemple à 40% et plus en poids d'oxyde de titane.The crosslinkable polymer may also be pigmented and loaded, for example, with 40% and more by weight of titanium oxide.

Le tableau ci-dessous permet de mettre en évidence l'effet du conditionnement thermique du polymère réticulable entre la zone de formation de la nappe 30 et la zone d'application du film 31 sur la viscosité de ce polymère réticulable afin de faciliter le transfert et l'application du film 31 sur la bande métallique 1. Température polymère(°C) Viscosité polymère (Pa.s) Couple (daN/m) Epaisseur film (mm) Transfert Aspect 120 120 34 40 partiel non lisse 130 60 30 40 partiel non lisse 140 30 20 40 total lisse 150 15 17 40 total lisse The table below makes it possible to highlight the effect of the thermal conditioning of the crosslinkable polymer between the zone of formation of the ply 30 and the zone of application of the film 31 on the viscosity of this crosslinkable polymer in order to facilitate the transfer and applying the film 31 to the metal strip 1. Polymer temperature (° C) Polymer viscosity (Pa.s) Couple (daN / m) Thickness film (mm) Transfer Aspect 120 120 34 40 partial not smooth 130 60 30 40 partial not smooth 140 30 20 40 total smooth 150 15 17 40 total smooth

Comme indiqué dans ce tableau, plus la température du polymère réticulable augmente, plus sa viscosité diminue ce qui permet de réduire pratiquement de la moitié le couple entre le cylindre de formation et d'application du film et la bande métallique et d'obtenir un aspect de surface lisse du revêtement sur ladite bande métallique.As indicated in this table, the more the temperature of the crosslinkable polymer increases, the lower its viscosity decreases which makes it possible to reduce by practically half the torque between the formation and application roll of the film and the metal strip and to obtain an appearance smooth surface of the coating on said metal strip.

Du fait de la diminution du couple, la pression au niveau du cylindre applicateur est diminuée ce qui permet de réduire de manière important l'usure du cylindre applicateur du film en polymère réticulable sur la bande métallique ce qui est d'autant plus important lorsque la surface de ce cylindre applicateur est en matériau déformable.Due to the decrease in torque, the pressure on the applicator roll is reduced, which makes it possible to significantly reduce the wear of the applicator roll of the crosslinkable polymer film on the metal strip. this is all the more important when the surface of this applicator roll is deformable material.

En effet, avec des températures du polymère réticulable de l'ordre de 120 ou 130°, pour obtenir un aspect lisse du revêtement sur la bande métallique, il faut atteindre un couple d'une valeur supérieure à 60 daN/m.Indeed, with temperatures of the crosslinkable polymer of the order of 120 or 130 °, to obtain a smooth appearance of the coating on the metal strip, it is necessary to achieve a torque of a value greater than 60 daN / m.

Cette valeur entraîne une usure rapide du cylindre applicateur.This value causes rapid wear of the applicator roll.

Le dispositif de revêtement selon l'invention permet d'obtenir un revêtement en polymère réticulable d'épaisseur uniforme comprise par exemple entre 5 et 50µm et appliqué d'une manière homogène sur une bande métallique présentant une rugosité importante d'amplitude comparable à l'épaisseur de film et cela grâce au contact parfait entre le cylindre applicateur et la surface de la bande métallique à revêtir, malgré les défauts de planéité et d'hétérogénéité d'épaisseur de la bande métallique.The coating device according to the invention makes it possible to obtain a cross-linkable polymer coating with a uniform thickness of, for example, between 5 and 50 μm and homogeneously applied to a metal strip having a large roughness of amplitude comparable to that of film thickness and this thanks to the perfect contact between the applicator roll and the surface of the metal strip to be coated, despite the defects of flatness and thickness heterogeneity of the metal strip.

La vitesse du cylindre applicateur peut être ajustée à un niveau sensiblement supérieur ou inférieur à la vitesse de défilement de la bande métallique de manière à obtenir une parfaite continuité du revêtement et un excellent état de surface de ce revêtement polymère réticulable transféré sur cette bande métallique.The speed of the applicator roll can be adjusted to a level substantially greater or less than the running speed of the metal strip so as to obtain a perfect continuity of the coating and an excellent surface state of this crosslinkable polymer coating transferred onto this metal strip.

Par ailleurs, l'énergie de surface du cylindre applicateur est adaptée au polymère réticulable pour permettre un bon étalement de la nappe sur ce cylindre applicateur.Furthermore, the surface energy of the applicator roll is adapted to the crosslinkable polymer to allow good spreading of the web on the applicator roll.

Le dispositif de revêtement selon l'invention peut également être utilisé pour une bande métallique descendante ou horizontale.The coating device according to the invention can also be used for a downward or horizontal metal strip.

Le fait que la température de formation de la nappe soit inférieure à la température de réticulation du polymère est une caractéristique importante dans le cas des polymères thermodurcissables puisque l'écoulement forcé au travers d'une fente d'extrusion implique des stagnations importantes du polymère qui sont nécessaires pour une bonne répartition de ce polymère sur toute la largeur de cette fente d'extrusion et il ne faut pas risquer à ce niveau une réticulation dudit polymère.The fact that the formation temperature of the web is lower than the crosslinking temperature of the polymer is an important characteristic in the case of thermosetting polymers since the forced flow through an extrusion slot involves significant stagnation of the polymer which are necessary for a good distribution of this polymer over the entire width of this extrusion slot and it should not risk at this level a crosslinking of said polymer.

Par ailleurs, le dispositif de revêtement selon l'invention permet de revêtir en continu des bandes métalliques de différentes largeurs ou de revêtir simultanément plusieurs bandes métalliques disposées parallèlement les unes aux autres et de s'affranchir par des moyens simples et efficaces des fluctuations de largeur et de positionnement transversal de la ou des bandes métalliques.Furthermore, the coating device according to the invention makes it possible to continuously coat metal strips of different widths or to coat simultaneously several metal strips arranged parallel to each other and to overcome by simple and effective means fluctuations in width and transverse positioning of the metal strip or strips.

Le dispositif de revêtement selon l'invention permet de faciliter l'alimentation régulière et uniforme du revêtement en polymère réticulable en sélectionnant le mode d'alimentation le mieux adapté en fonction du produit à mettre en oeuvre.The coating device according to the invention makes it possible to facilitate the regular and uniform supply of the crosslinkable polymer coating by selecting the most appropriate mode of supply according to the product to be used.

L'intérêt de ce large choix est particulièrement important dans le cas de revêtements thermodurcissables hautement réactifs dont l'alimentation ne peut pas s'effectuer à une température élevée proche du domaine de réactivité.The interest of this wide choice is particularly important in the case of highly reactive thermosetting coatings which can not be fed at an elevated temperature close to the reactivity range.

La température de la matière délivrée par le système d'alimentation situé en amont du cylindre applicateur est limitée à une valeur inférieure à celle du début de réticulation pour éviter tout risque d'évolution du produit dans le système d'alimentation et tout risque de blocage de ce système.The temperature of the material delivered by the supply system located upstream of the applicator cylinder is limited to a value lower than that of the beginning of crosslinking to avoid any risk of evolution of the product in the feed system and any risk of blockage of this system.

Du fait de cette limitation de température, il était difficile d'obtenir un bon transfert et un bon étalement sur la bande métallique.Because of this temperature limitation, it was difficult to obtain a good transfer and a good spread on the metal strip.

Grâce à l'invention, ce dispositif permet également, dans le cas d'un processus de réticutation par voie chimique, d'élever la température du polymère réticulable de manière à réduire sa viscosité et à faciliter son transfert et son étalement sur la bande métallique.Thanks to the invention, this device also makes it possible, in the case of a chemical transfer process, to raise the temperature of the crosslinkable polymer so as to reduce its viscosity and to facilitate its transfer and spreading on the metal strip. .

Lors du contact avec le cylindre applicateur, la matière peut supporter un échauffement très important, mais pendant une durée très faible qui permet d'éviter tout risque de réticulation du produit à ce niveau.During contact with the applicator roll, the material can withstand a very large heating, but for a very short time that avoids any risk of crosslinking the product at this level.

Enfin, le dispositif selon l'invention permet de compenser des fluctuations de largeur ou de position transversale de la bande métallique lors de l'application et de s'affranchir des défauts d'uniformité de la bande métallique et de réaliser ainsi un revêtement d'épaisseur uniforme en surface sur un substrat métallique non uniforme.Finally, the device according to the invention makes it possible to compensate for variations in the width or transverse position of the metal strip during application and to overcome the defects of uniformity of the metal strip and thus to make a coating of Uniform surface thickness on a non-uniform metal substrate.

Claims (24)

  1. Method for continuously coating at least one metal strip (1) with a fluid cross-linkable polymer film (31) which is froe from non-reactive solvent and diluent and whose softening temperature is greater than 50°C, the film (31) having a thickness less than that of the metal strip (1), in which mothod:
    - the metal strip (1) is continuously moved on at least one support roller (3),
    - there is formed, on a roller (20) and by means of forced flow at a temperature qreater than the softening temperature of the cross-linkable polymer, a sheet (30) of the cross-linkable polymer in the molten state having a viscosity greater than 10Pa.s under the conditions under which the sheet is formed, the formation temperature of this sheet (30) being less than the temperature at which the cross-linkable polymer begins to cross-link, and the roller (20) being caused to rotate in the opposite direction to that in which the metal strip (1) moves,
    - the cross-linkable polymer film (31) is formed from the sheet (30),
    - a total transfer in terms of the thickness of the film (31) is carried out to the metal strip (1),
    - and, between the zone in which the sheet (30) is formed cn the roller (20) and the zone in which the film (31) is applied to the metal strip (1), the cross-linkable polymer is processed thermally according to suitable means in order to reduce the viscosity of the cross-linkable polymer by at least a factor of 2 relative to the viscosity measured under the conditions of the forced flow.
  2. Method according to claim 1, characterised in that the means are adapted so that the temperature of the cross-linkable polymer exceeds the temperature at which the cross-linkable polymer begins to cross-link.
  3. Method according to claim 1, characterised in that the cross-linkable polymer film (31) is formed on the roller (20) and the total transfer in terms of the thickness of the film is carried out from this roller (20) to the metal strip (1) by this metal strip being compressed between the support roller (3) and the roller (20) in order to obtain a coating of uniform thickness.
  4. Method according to claim 1 or 3, characterised in that the roller (20) has a deformable surface and the support roller (3) has a hard surface.
  5. Method according to claim 1 or 3, characterised in that the roller (20) has a hard surface and the support roller (3) has a deformable surface.
  6. Method according to claim 1, characterised in that:
    - an intermediate sheet (30b) of cross-linkable polymer is formed on the roller (20) from the sheet (30) in the molten state,
    - this intermediate sheet (30b) is transferred to an intermediate transfer element (21) by the element (21) being compressed against the roller (20), the transfer element (21) being interposed between the roller (20) and the metal strip (1) and being caused to rotate in the opposite direction to that in which the metal strip (1) moves,
    - the cross-linkable polymer film (31) is formed on the transfer element (21),
    - and a total transfer in terms of the thickness of the film (31) is carried out from the transfer element (21) to the matal strip (1) by the metal strip (1) being compressed between the transfer roller (21) and the support roller (3) in order to obtain a coating of uniform thickness.
  7. Method according to claim 1 or 6, characterised in that the transfer element (21) has a deformable surface and the roller (20) and the support roller (3) each have a hard surfiace.
  8. Mothod according to claim 1 or 6, characterised in that the transfer element (21) has a hard surface and the roller (20) and the support roller (3) each have a deformable surface.
  9. Coating method according to any one of the preceding claims, characterised in that the metal strip (1) is preheated to a temperature which is substantially equal to or greater than the temperature of the fluid cross-linkable polymer film and the softoning temperature of the cross-linkable polymer.
  10. Coating method according to any one of the preceding claims, characterised in that the roller (20) is heated to a temperature which is substantially equal to or greater than the temperature of the sheet (30) and the softening temperature of the cross-linkable polymer.
  11. Coating method according to any one of claims 6 to 10, characterised in that the transfer element (21) is heated to a temperature which is equal to or groater than the temperature of the roller (20).
  12. Coating method according to any one of the preceding claims, characterised in that the cross-linkable polymer is processed thermally by heating the roller (20) and/or the transfer element (21) and/or by applying an additional thermal flux to the intermediate sheet (30b) and/or the film (31).
  13. Device for continuously coating at least one metal strip (1) with a fluid cross-linkable polymer film (31) which is free from non-reactive solvent and diluent and whose softening temperature is greater than 50°C, the film (31) having a thickness less than that of the metal strip (1), which dovice comprises:
    - means for continuously driving the metal strip (1),
    - at least one support roller (3) for the metal strip,
    - means for forming, on a roller (20) and by means of forced flow at a temperature greater than the softening temperature of the cross-linkable polymer, a sheet (30) of the cross-linkable polymer in the molten state haring a viscosity greater than 10Pa.s under the conditions under which the sheet is formed, the formation temperature of this sheet (30) being less than the temperature at which the cross-linkable polymer begins to cross-link and the roller (20) being caused to rotate in the opposite direction to that in which the metal strip (1) moves,
    - means for forming the cross-linkable polymer film (31) from the sheet (30) and for a total transfer in terms of the thickness of the film to the metal strip (1),
    - and, between the zone in which the sheet (30) is formed on the roller (20) and the zone in which the film (31) is applied to the metal strip (1), means for thermally processing the cross-linkable polymer according to suitable means in order to reduce the viscosity of the cross-linkable polymex by at least a factor of 2 relative to the viscosity measured under the conditions of the forced flow.
  14. Device according to claim 13, characterised in that the means for forming the cross-linkable polymer film (31) and for a total transfer in terms of the thickness thereof are formed by the roller (20) and by means for compressing the metal strip (1) between the roller (20) and the support roller (3) in order to obtain a coating of uniform thickness.
  15. Device according to claim 14, characterised in that the roller (20) comprises a metal core which is covered by a casing of deformable material, such as, for example, an elastomer, and the support roller (3) comprises a hard surface.
  16. Davice according to claim 14, characterised in that the roller (20) comprises a hard surface and the support roller (3) comprises a metal core which is covered by a casing of deformable matorial, such as, for example, an elastomer.
  17. Device according to claim 13, characterised in that the means for forming the cross-linkable polymer film (31) and for a total transfer in terms of the thickness thereof comprise:
    - the roller (20) which forms an intermediate sheet (30b) of cross-linkable polymer from the sheet (30),
    - an intermediate transfer element (21) which is interposed between the roller (20) and the metal strip (1) and which is caused to rotate in the opposite direction to that in which the metal strip (1) moves in order to form the cross-linkable polymer film (31) from the intermediate sheet (30b),
    - means for compressing the transfer element (21) between the roller (20) and the support roller (3) in order to transfer the intermediate sheet (30b) to the transfer element (21),
    - and means for compressing the metal strip (1) between the transfer element (21) and the support roller (3) in order to transfer the film (31) to the metal strip.
  18. Device according to claim 17, characterised in that the roller (20) and the support roller (3) each comprise a hard surface and the transfer element is formed by an applicator roller (21) which comprises a motel core which is covered by a casing of deformable material, such as, for example, an elastomer.
  19. Device according to claim 17, characterised in that the roller (20) and the support roller (3) each comprise a metal core which is covered by a casing of doformable material, such as, for example, an elastomer, and the transfer element is formed by an applicator roller (21) which has a hard surface.
  20. Coating device according to any one of claims 13 to 19,
    characterised in that it comprises means for preheating the metal strip (1) to a temperature which is equal to or greater than the temperature of the fluid cross-linkable polymer film (31) and the softening temperature of the cross-linkable polymer.
  21. Coating dovice according to any one of claims 13 to 20, characterised in that it comprises means for heating the roller (20) to a temperature which is substantially equal to or greater than the temperature of the sheet (30) and the softening temperature of the cross-linkable polymer.
  22. Coating device according to any one of claims 17 to 19, characterised in that it comprises means for heating the transfer element (21) to a temperature which is substantially equal to or greater than the temperature of the roller (20).
  23. Coating device according to any one of claims 13 to 23, characterised in that the means for thermally processing the cross-linkable polymer are formed by a system for heating the roller (20) and/or the transfer element (21) and/or by at least one source (15) for applying an additional thermal flux to the intermediate sheet (30b) and/or the film (31).
  24. Coating device according to any one of claims 13 to 23, characterised in that the source (15) for applying the additional thermal flux is constituted by hot air generators or infrared lamps or microwave systems.
EP99957371A 1998-12-16 1999-12-07 Method and device for continuously coating at least a metal strip with a crosslinkable polymer fluid film Expired - Lifetime EP1140375B1 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
FR9815901 1998-12-16
FR9815900A FR2787353B1 (en) 1998-12-16 1998-12-16 METHOD AND DEVICE FOR THE CONTINUOUS COATING OF AT LEAST ONE METAL STRIP WITH A FLUID FILM OF CROSSLINKABLE POLYMER
FR9815901A FR2787354B1 (en) 1998-12-16 1998-12-16 METHOD AND DEVICE FOR THE CONTINUOUS COATING OF AT LEAST ONE METAL STRIP WITH A FLUID FILM OF CROSSLINKABLE POLYMER
FR9815900 1998-12-16
PCT/FR1999/003040 WO2000035593A1 (en) 1998-12-16 1999-12-07 Method and device for continuously coating at least a metal strip with a crosslinkable polymer fluid film

Publications (2)

Publication Number Publication Date
EP1140375A1 EP1140375A1 (en) 2001-10-10
EP1140375B1 true EP1140375B1 (en) 2003-09-10

Family

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Application Number Title Priority Date Filing Date
EP99957371A Expired - Lifetime EP1140375B1 (en) 1998-12-16 1999-12-07 Method and device for continuously coating at least a metal strip with a crosslinkable polymer fluid film

Country Status (13)

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US (1) US6562407B1 (en)
EP (1) EP1140375B1 (en)
JP (1) JP2002532231A (en)
KR (1) KR100598709B1 (en)
AT (1) ATE249287T1 (en)
AU (1) AU765280B2 (en)
BR (1) BR9916098A (en)
CA (1) CA2355383C (en)
DE (1) DE69911245T2 (en)
DK (1) DK1140375T3 (en)
ES (1) ES2207309T3 (en)
PT (1) PT1140375E (en)
WO (1) WO2000035593A1 (en)

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FR2814688B1 (en) * 2000-09-29 2003-06-27 Usinor METHOD AND DEVICE FOR CONTINUOUSLY COATING AT LEAST ONE SIDE OF A METAL STRIP WITH A SINGLE-LAYER OR MULTILAYER FILM OF CROSS-LINKABLE POLYMERS
FR2831470A1 (en) * 2001-10-29 2003-05-02 Usinor PROCESS FOR CONTINUOUSLY COATING A STRIP WITH A FLUID CROSSLINKABLE POLYMER FILM
FR2845299B1 (en) * 2002-10-04 2004-12-03 Usinor METHOD AND DEVICE FOR CONTINUOUSLY COATING AT LEAST ONE SUBSTRATE WITH A FILM
US7722922B2 (en) * 2003-10-20 2010-05-25 Furukawa-Sky Aluminum Corp. Coating apparatus for an aluminum alloy heat exchanger member, method of producing a heat exchanger member, and aluminum alloy heat exchanger member
WO2005037479A1 (en) * 2003-10-20 2005-04-28 Furukawa-Sky Aluminum Corp. Coating apparatus for member for heat exchanger made of aluminum alloy and method for manufacturing member for heat exchanger, and member for heat exchanger made of aluminum alloy
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US6562407B1 (en) 2003-05-13
DE69911245D1 (en) 2003-10-16
PT1140375E (en) 2004-01-30
AU1509800A (en) 2000-07-03
AU765280B2 (en) 2003-09-11
ATE249287T1 (en) 2003-09-15
CA2355383A1 (en) 2000-06-22
EP1140375A1 (en) 2001-10-10
CA2355383C (en) 2008-10-07
DK1140375T3 (en) 2004-01-19
JP2002532231A (en) 2002-10-02
KR100598709B1 (en) 2006-07-10
WO2000035593A1 (en) 2000-06-22
DE69911245T2 (en) 2004-09-09
KR20010086114A (en) 2001-09-07
ES2207309T3 (en) 2004-05-16
BR9916098A (en) 2001-09-04

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