WO2019115261A1 - Procédé de production de matières lignocellulosiques monocouches ou multicouches dans des conditions spéciales sous presse chaude - Google Patents

Procédé de production de matières lignocellulosiques monocouches ou multicouches dans des conditions spéciales sous presse chaude Download PDF

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Publication number
WO2019115261A1
WO2019115261A1 PCT/EP2018/083277 EP2018083277W WO2019115261A1 WO 2019115261 A1 WO2019115261 A1 WO 2019115261A1 EP 2018083277 W EP2018083277 W EP 2018083277W WO 2019115261 A1 WO2019115261 A1 WO 2019115261A1
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Prior art keywords
component
weight
mixture
acid
lignocellulosic materials
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PCT/EP2018/083277
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German (de)
English (en)
Inventor
Stephan Weinkoetz
Jean-Pierre Berkan LINDNER
Ralph Lunkwitz
Claus Fueger
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Basf Se
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Publication of WO2019115261A1 publication Critical patent/WO2019115261A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
    • B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
    • B27N3/002—Manufacture of substantially flat articles, e.g. boards, from particles or fibres characterised by the type of binder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
    • B27N1/00—Pretreatment of moulding material
    • B27N1/02—Mixing the material with binding agent
    • B27N1/0209—Methods, e.g. characterised by the composition of the agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6492—Lignin containing materials; Wood resins; Wood tars; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse

Definitions

  • the present invention relates to a process for the production of single or multilayered lignocellulosic materials consisting of a core layer (KS) and optionally further layer (s) (WS), wherein the mixture of the components A, B, C and optionally D, E and F, used for the preparation of the mixture for the core layer, a gelling time at 60 ° C (GZ60) of 10 to 450 seconds and wherein in process step (IV) special conditions are met.
  • the present invention relates to the lignocellulosic materials thus obtainable and their use in furniture construction, house construction, interior construction and exhibition construction.
  • EP-B-1 852 231 discloses a process for producing wood-based materials from comminution products of lignocellulose-containing materials and an adhesive, wherein the comminuted products before hot-pressing are admixed with at least one additive selected from the group of maleic anhydride, fumaric acid, acrylic acid, Polyacrylates, homologues of acrylic acid or mixtures thereof is added.
  • the additive after the refiner may be added to the fibers e.g. be mixed with the blowing of the adhesive.
  • adhesives u.a.
  • Aminoplast resins such as urea-formaldehyde resins (UF resins), adhesives based on isocyanates (PMDI) or a mixture thereof.
  • a process for the production of lignocellulosic materials in which the wood chips are glued with a binder and a hardener, wherein the hardener is preferably added shortly before the use of the binder.
  • a binder i.a. Aminoplastharze, organic isocyanates having at least two isocyanate groups (such as PMDI) or mixtures thereof, as a hardener all known in the art hardener or mixtures thereof, in particular carboxylic acids, sulfonic acids, phosphoric acid, polyphosphoric or their salts such as halides.
  • WO-A-2016/156226 is a discontinuous or continuous process for the preparation of single or multilayered lignocellulosic materials comprising the process steps (I) mixing the components of the individual layers, (II) scattering the in process step ( I) to a mat, (III) optionally pre-compaction of the scattered mat and (IV) hot pressing the optionally pre-compressed mat, by in the process step (I) for the core of multilayer or lignocellulosic for a single-layer materials
  • the object of the present invention was to remedy the aforementioned disadvantages.
  • KS core layer
  • WS further layer
  • Binders selected from the group of aminoplast resins or mixtures thereof
  • binder based on isocyanate (component D)
  • ammonium salt (component E)
  • the mixture of components A, B, C and optionally D, E and F used for the preparation of the mixture for the core layer has a gelling time at 60 ° C (GZeo) of 10 to 450 seconds and b ) the temperature T m in the middle of the pressed material at the end of the process step (IV) is between 65 and 99 ° C.
  • Pre-compaction is the reduction of the thickness of the scattered mat by mechanical influence to understand.
  • the pre-compaction takes place here in addition to the pressing in the context of process step (IV).
  • the spread mat is subjected to pre-compression to achieve a certain strength of the spread mats.
  • the temperature of the prepress is generally from 5 to 60.degree. C., preferably from 5 to 40.degree. C., in particular from 10 to 30.degree. C., more preferably from 15 to 25.degree.
  • the precompression can be done after spreading each individual layer or after spreading all the layers on top of each other. Pre-compression is preferably carried out one after the other after scattering of all layers.
  • the pre-compression can be carried out by methods known to the person skilled in the art, as described, for example, in M. Dunky, P. Niemz, Holzwerkstoffe und Leime, Springer Verlag Heidelberg, 2002, page 819 or in H.-J. Deppe, K. Ernst, MDF - medium density fiberboard, DRW-Verlag, 1996, pages 44, 45 and 93 or in A. Wagendies, F. Scholz, Taschenbuch der Holztechnik, subuchverlag für, 2012, page 219, are described.
  • Pre-compaction can be done in one, two or more steps.
  • the pre-compression is usually carried out at a pressure of 1 to 30 bar, preferably 2 to 25 bar, more preferably 3 to 20 bar.
  • a period of from 1 to 120 seconds, preferably from 2 to 60 seconds, particularly preferably from 3 to 20 seconds can be used.
  • energy can be introduced into the mat with one or more arbitrary energy sources in a preheating step.
  • Suitable energy sources are hot air, water vapor, steam / air mixtures or electrical energy (high-frequency high-voltage field or microwaves).
  • the mat is heated in the core at 30 to 55 ° C, preferably at 30 to 50 ° C, more preferably at 30 to 45 ° C.
  • the preheating can also be carried out so that, for example, by introducing water vapor, only the outer layers are heated, but not the core.
  • the mat can be prevented from springing up during heating by carrying out the heating in a space bounded above and below.
  • the boundary surfaces are designed so that the energy input is possible.
  • perforated plastic belts or steel nets can be used, which allow the passage of hot air, water vapor or water vapor-air mixtures.
  • the boundary surfaces are designed to exert a pressure on the mat which is so great as to prevent springing during heating.
  • a device for a continuous process to realize the heating by applying a high-frequency electromagnetic field after the compression within the same machine is described, for example, in WO-A-97/28936.
  • no preheating takes place during or after the precompression, that is to say that after the process step (III) the scattered mat has a lower temperature than or the same temperature as before the process step (III).
  • Process step (IV) heating and pressing the pre-compacted mat
  • the heating and pressing of the pre-compressed mat takes place.
  • the heating is required to cure the binder (component A).
  • the thickness of the mat is reduced (further) by applying a pressing pressure, or at least held constant, preferably reduced.
  • the temperature of the mat is increased by inputs of energy. This can be done either by hot pressing and / or by applying an electromagnetic high-frequency field. In the simplest case, a constant pressure is applied and at the same time by an energy heated source of constant power.
  • the energy input in process step (IV) is preferably carried out by hot pressing, ie by heat transfer from heated surfaces, for example hot pressed sheets or steel strips (in continuous double belt presses), to the mat during the pressing process.
  • the applied high-frequency electromagnetic field can be microwave radiation or a high-frequency electric field that arises after application of a high-frequency AC voltage field to a plate capacitor between the two capacitor plates.
  • the energy is usually introduced by contact with heated pressing surfaces, the temperatures of 110 to 300 ° C, preferably 150 to 280 ° C, more preferably 200 to 250 ° C, wherein during the energy input at a pressure of 1 to 50 bar, preferably 3 to 40 bar, particularly preferably 5 to 30 bar is pressed.
  • the pressing surfaces preferably have a constant temperature.
  • the temperatures of the pressing surfaces ie the steel belts
  • the temperatures can also vary slightly over the press length, with the differences generally not exceeding 30 ° C.
  • the temperatures may be lower than in the inlet area of the press.
  • the pressing can be carried out by all methods known to those skilled in the art (see examples in “Taschenbuch der Spanplattentechnik”). H.-J. Deppe, K. Ernst, 4th ed., 2000, DRW - Verlag Weinbrenner, Leinfelden-Echterdingen , Page 232 to 254, and "MDF medium-density fiberboard” H.-J. Deppe, K. Ernst, 1996, DRW- Verlag Weinbrenner, Leinfelden-Echterdingen, pages 93 to 104). Preference is given to continuous pressing processes, for example with double belt presses.
  • step (IV) If the input of energy in method step (IV) is effected by a) applying a high-frequency electromagnetic field and by b) hot pressing, then preferably the high-frequency electric field and then the hot pressing are carried out.
  • the mixture of the components A, B, C and optionally D, E and F used for the preparation of the mixture for the core layer has a gel time of 60 ° C (GZeo) of 10 to 450 seconds, preferably 30 to 400 seconds more preferably 45 to 350 seconds.
  • the temperature T m in the center of the pressed material at the end of process step (IV) is between 65 and 99.degree. C., preferably between 70 and 90.degree. C., very particularly preferably between 75 and 85.degree.
  • the temperature T m is at any time or at any point of the process step below the temperature T m at the end of the process step (IV).
  • deviations of up to 5 ° C upwards are also possible.
  • the time t from reaching a temperature T m of 60 ° C until the end of process step (IV) is greater than 3 seconds, preferably greater than 5 seconds and less than 10 seconds, a "GZ 6 o, wherein GZeo the gelation time is 60 ° C. in seconds and a is a factor which occupies a value of 0.02 to 0.25, preferably 0.03 to 0.15, particularly preferably 0.04 to 0.1.
  • pressing time factors of less than 5 seconds / mm, preferably less than 4 seconds / mm can be achieved.
  • the pressing time factor is the quotient of pressing time and plate thickness.
  • the thickness of the plate here means the average thickness of the plate immediately after process step (IV).
  • the center of the material to be pressed is a position in the material to be compacted (ie the compacted mat in process step (IV)), which has the same distance to both pressing surfaces (in the vertical direction).
  • the point at which the temperature T m is measured should have a sufficient distance from the edge of the material to be pressed. In a continuous process this means that this measuring point in the horizontal direction is at least 0.1 » BdP, preferably 0.2 * BdP, particularly preferably 0.4 * BdP, very particularly preferably exactly 0.5 * BdP away from the edge of the pressed material , where BdP is the "width of the material to be pressed" in the press (that is perpendicular to the running direction of the material to be pressed).
  • the distance from the narrow side in this case is min- least 0.1 »Ls, preferably 0.2 * s li_ particularly preferably 0.4 * li_ s, very preferably precisely 0.5 * LI_S.
  • the distance from the long side in this case is 0, 1 "Eat, preferably 0.2 * ls s, particularly preferably 0.4 * ls s, very preferably precisely 0.5 * ls s.
  • L s is the length of the longitudinal side and Is s the length of the narrow side of the material to be pressed.
  • the measurement of the temperature in the middle of the material to be pressed can be carried out by methods known per se, in particular according to Meyer / Thömen, Holz Roh Werkst (2007) 65, pages 49 to 55 [Meyer / Thömen] and Thömen, 2010, vom Wood to the Material - Basic Investigations for the Production and Structure of Wood-based Materials ", ISBN 978-3-9523198-9-5.
  • sensors such as the CONTI LOG or EASYLOG sensors from Fagus-GreCon Greten GmbH & Co. KG, which are inserted into the mat when the mat is spread.
  • the die may be laid on the mat after scattering the lower cover layer and half the middle layer, followed by scattering the second half of the middle layer and the upper cover layer.
  • the end of process step (IV) is understood to mean the point in time or the point in the process at which the pressed material no longer has any contact with the pressing surfaces at the end of the pressing process. For example, in a batch process, this is the time when the press is opened. In a continuous process with a double belt press, this is, for example, the point at which the revolving double strip separates from the pressed material.
  • the binder is usually cured.
  • the process according to the invention is characterized in that that the aminoplast resin (component A) in the produced lignocellulose material is completely or almost completely cured.
  • the lignocellulosic materials according to the invention have strengths which are sufficient for the use of the lignocellulose material in end applications which require high strength and stability of the lignocellulose material, for example in furniture construction, house construction, interior work and trade fair construction, in particular in furniture construction.
  • the final strengths may be obtained by ripening the lignocellulosic materials during storage, e.g. when stored in the stack, where the materials cool only slowly, be slightly higher than the immediate strengths, which are measured shortly after the end of the process step (IV).
  • the transverse tensile strength (measured according to EN 319: 1993) is used as a measure of the strengths of the lignocellulosic materials.
  • the final strength of the lignocellulosic materials ie the transverse tensile strength exhibited by the lignocellulosic materials one week after production (including air conditioning according to EN 319: 1993), can not exceed 30%, preferably not more than 20%, particularly preferably not more than 10% the transverse tensile strength short time after the end of the process step (IV) (instantaneous) lie.
  • the gelling time can be used as a measure of the reactivity of the binder system used.
  • the gelling time depends on the chemical composition of the binder system and the temperature. The principle of the measurement is based on measuring the time until the time at which under the chosen conditions, here at 60 ° C, the viscosity of the binder system rises sharply and the mixture pulls no strings when pulling out a glass or metal rod .
  • the gelling time QZ QO of the binder system of the invention consisting of the components A, B, C and optionally D, E and F, can be based on in Zeppenfeld, Grunwald, adhesives in the wood and furniture industry, DRW Verlag, 2. Edition, 2005, page 289, as follows:
  • total mass 50 g the components of the binder system (total mass 50 g) are weighed and stirred vigorously at room temperature for 30 seconds to obtain a homogeneous mixture as possible. Immediately weigh 1 g of this mixture into a test tube and place it one minute after preparation of the mixture in a water bath at 60 ° C so that the top of the mixture in the test tube is 2 cm below the water level in a water bath. With a glass rod warmed to 60 ° C., this mixture is stirred with time taking (stopwatch) until the mixture gels, ie the mixture no longer pulls threads when pulling out the glass rod. Gelling time is the time from immersion of the test tube in the water bath until gelation.
  • binder system BS the components A to F are used in the form as they are added in the process to the lignocellulose particles.
  • the binder system BS for gel time measurement is prepared by mixing the mixture of component A and component C with the component Mixture of component B) and D produced.
  • the lignocellulosic materials produced according to the invention are plate-shaped and can be single or multilayered.
  • the plate thickness (plate thickness) of the finished lignocellulosic materials is usually from 2 to 50 mm, preferably 10 to 25 mm.
  • the plate thickness can be greater by up to 1 mm, preferably up to 0.5 mm, particularly preferably up to 0.2 mm, than in the finished lignocellulose material, since as a rule a grinding step takes place.
  • the lignocellulosic materials are medium density fibreboard (MDF) having a density of 450 to 800 kg / m 3 or high density fiberboard (HDF) having a density of 800 to 1100 kg / m 3 .
  • MDF medium density fibreboard
  • HDF high density fiberboard
  • OSB Oriented Strand Boards
  • the lignocellulosic materials are chipboard.
  • Particularly suitable is the process for the production of plates of the type P2, P3, P4 and P5, in particular for P3 and P5 (according to EN312: 2003).
  • the process is particularly well suited for producing lignocellulosic materials, in particular chipboards with a low formaldehyde emission.
  • the formaldehyde emission is preferably less than 0.07 ppm, more preferably less than 0.05 ppm, most preferably less than 0.03 ppm.
  • the lignocellulosic materials produced according to the invention consist exclusively of a core layer (KS), i. one or more further layers (WS) are not part of the lignocellulosic materials.
  • the core layer can be scattered in one step or in several steps.
  • the lignocellulose materials produced according to the invention consist of two or more further layers (WS) in addition to the core layer (KS).
  • the core layer can be scattered in one step or in several steps.
  • WS are generally to be understood as those layers which differ from the core layer (KS), ie have a different composition than the core layer (KS).
  • Further layers (WS) are located in the lignocellulosic material above and below the core layer (KS).
  • the ratio of the mass of the further layer or of the further layers below the core layer to the mass of the further layer or of the further layers above the core layer is preferably 50:50, but may also deviate slightly therefrom and between 60:40 and 40 : 60 lie. If there are two further layers, ie one which is located above and one below the core layer, then these two layers preferably have the same composition, so that the most symmetrical plate structure is ensured. If several further layers are present, a symmetrical structure is likewise preferred.
  • the layers which are boundary layers to the environment, ie form the outer layers of the lignocellulosic material, are referred to as cover layers.
  • the further layers preferably contain at most 50%, particularly preferably at most 35%, of the total mass of the complete lignocellulose material.
  • the lignocellulosic material consists of a core layer (KS) and two outer layers.
  • cover layers In principle, all types of cover layers known to the person skilled in the art for the production of lignocellulose materials come into consideration. Suitable cover layers and their application are described, for example, in WO-2016/156226.
  • the further layers like the core layer, preferably contain binders selected from the group of amino resins, but may also contain no aminoplast resin and instead contain other binders, for example based on phenolic resins or isocyanates.
  • the mixtures of lignocellulose particles, binders and additives which are used for the preparation of the further layers preferably have a moisture content of 5 to 20%, preferably 8 to 15%, particularly preferably 10 to 13%. The moisture content of these mixtures is measured and determined in accordance with EN 322.
  • Release agents, surfactants or formaldehyde scavengers, for example urea or polyamines can be used as additives in this case.
  • the concentration of additive is between 0 and 65 wt .-%, preferably between 0 and 50 wt .-%. Particular preference is given to using water (0% by weight of additives).
  • the application to the underside of the mat takes place, for example, by applying water or aqueous solution, emulsion or suspension of an additive to the forming belt before scattering,
  • the application to the top is carried out, for example, by dripping, rolling, pouring or spraying, preferably by spraying, after scattering of all layers, before or after, preferably before process step (III).
  • the mixture for the core layer (KS) in process step (I) is preferably made of lignocellulosic particles (component L) having a residual moisture content of 0 to 10 wt.%, Preferably 0.5 to 7.5 wt. particularly preferably 1 to 5 wt .-% and
  • component A 5 to 15% by weight of component A, preferably 6 to 13% by weight, particularly preferably 6.5 to 9% by weight,
  • component B 0.005 to 0.5% by weight of component B, preferably 0.01 to 0.2% by weight, more preferably 0.02 to 0.1% by weight,
  • component C From 2 to 10% by weight of component C, preferably from 2.5 to 8.5% by weight, more preferably from 3 to 7% by weight, and
  • wt .-% 0 to 2 wt .-%, preferably 0.05 to 1 wt .-%, particularly preferably 0.1 to 0.5 wt .-% of one or more components D.
  • component L in each case based on 100 wt .-% dry weight of component L.
  • the components A to G can be added as a mixture of all components, as a mixture of individual components (partial mixture), or as individual components to the lignocellulose particles. The order of addition is arbitrary.
  • the total amount of a component can also be divided into different sub-mixtures.
  • the water (component C) can be divided into two subsets, the first subset being mixed with the component A before the application onto the lignocellulose particles or being present together with the component A (for example in the form of an aqueous aminoplast resin). and the second subset with the component B.
  • the dry weight of component L in the context of the present invention refers to the weight of component L in the dry state, sometimes also referred to as absolutely dry (atro). It is determined by the Darr method, in which the sample is dried in the oven at 103 ° C to constant weight. Details are regulated in EN 13183-1.
  • the percentage by weight of components A relates to the dry weight of component A.
  • the dry weight of an aqueous aminoplast resin is frequently also called the solid content and, according to Günter Zeppenfeld, Dirk Grunwald, adhesives in the wood and furniture industries. belindustrie, 2nd edition, DRW-Verlag, page 268.
  • To determine the dry weight of aminoplast resins 1 g of resin is accurately weighed into a weighing pan, finely distributed at the bottom and dried for 2 hours at 120 ° C. in a drying oven. After tempering to room temperature in a desiccator, the residue is weighed and calculated as a percentage of the initial weight.
  • the water contained is mathematically assigned to component C.
  • Components B, D, E, F and G may also be used as a mixture, e.g. in the form of a solution or emulsion. Again, the water obtained is mathematically assigned to the component C.
  • Component L lignocellulosic particles
  • Lignocellulose particles are generally produced by comminution of lignocellulose-containing substances.
  • Lignocellulose-containing substances are substances that contain woody plant material. Woodiness refers to the chemical and physical alteration of the cell walls of plants through the incorporation of lignin. The most important lignocellulosic substances are wood. However, it is also possible to use other plants containing lignin, or agricultural and forestry raw materials and residues containing lignin, such as straw, flax shives or cotton stalks. Also suitable are palm trees or grasses with woody stems, such as bamboo. Another source of lignocellulose-containing particles are waste paper or waste wood, for example, old furniture.
  • the lignocellulose-containing particles used may contain foreign substances which do not originate from the lignocellulose-containing plants.
  • the content of foreign substances can be varied within wide ranges and is usually 0 to 30 wt .-%, preferably 0 to 10 wt .-%, particularly preferably 0 to 5 wt .-%, in particular particular 0 to 1 wt .-%.
  • Foreign substances can be plastics, adhesives, coatings, dyes, etc., which are contained in waste wood, for example.
  • the term lignocellulose is known to the person skilled in the art.
  • One or more lignocellulosic substances can be used.
  • the lignocellulose-containing particles are used in the form of fibers, strips, chips, dust or mixtures thereof, preferably shavings, fibers, dust or mixtures thereof, particularly preferably shavings, fibers or mixtures thereof.
  • the fibers, strips or chips are usually produced by comminuting the lignocellulosic substances.
  • Wood fibers or wood layers, wood strips, sawdust, wood chips, wood shavings, wood dust or mixtures thereof, preferably wood chips, wood fibers, wood dust or mixtures thereof, particularly preferably wood chips, wood fibers or mixtures thereof are preferably used as lignocellulose particles, most preferably wood chips.
  • wood particles For the production of wood particles comes any kind of softwood and hardwood, u.a. of industrial lumber, thinning wood or plantation wood, in question, preferably eucalyptus, spruce, beech, pine, larch, linden, poplar, ash, oak, fir or their mixtures, more preferably eucalyptus, Spruce, pine and beech wood or mixtures thereof, in particular eucalyptus, pine and spruce wood or mixtures thereof.
  • lignocellulosic particles are not critical and depend on the lignocellulosic material to be produced.
  • lignocellulosic materials include MDF (with dense-dense fibreboard), HDF (high-density fiberboard), PB (chipboard), OSB (coarse chipboard) or WFI (wood fiber insulation board).
  • MDF with dense-dense fibreboard
  • HDF high-density fiberboard
  • PB chipboard
  • OSB coarse chipboard
  • WFI wood fiber insulation board
  • strands Large chips, which are used for example for the production of OSB boards, are also called strands.
  • the average size of the strands is usually 20 to 300 mm, preferably 25 to 200 mm, particularly preferably 30 to 150 mm.
  • chips For the production of chipboard usually smaller chips are used.
  • the chips required for this can be classified by sieve analysis in size.
  • the sieve analysis is described, for example, in DIN 4188 or DIN ISO 3310.
  • the average size of the chips is usually 0.01 to 30 mm, preferably 0.05 to 25 mm, particularly preferably 0.1 to 20 mm.
  • Suitable fibers are wood fibers, hemp fibers, bamboo fibers, miscanthus, bagasse (sugarcane) or mixtures thereof, preferably wood fibers, hemp fibers, bamboo fibers, miscanthus, bales or mixtures thereof, particularly preferably wood fibers, or mixtures thereof.
  • the Length of the fibers is generally 0.01 to 20 mm, preferably 0.05 to 15 mm, particularly preferably 0.1 to 10 mm.
  • the comminution of the lignocellulose-containing substances into lignocellulose-containing particles or fibers can be carried out by methods known per se (see, for example: M. Dunky, P. Niemz, Holzwerkstoffe und Leime, pages 91 to 156, Springer Verlag Heidelberg, 2002).
  • the lignocellulose-containing particles are dried by customary methods known to those skilled in the art and then contain small amounts of water.
  • the amount of water is based on the dry weight of the lignocellulose particles in the dry state and referred to as relative humidity or as residual moisture.
  • the relative humidity is measured on the basis of EN 322.
  • the relative humidity of the lignocellulose particles used in the process according to the invention is between 0 and 10% by weight. If, for example, 1100 g of lignocellulose particles with a residual moisture of 10% by weight are used, these lignocellulose particles contain 100 g of water and the dry weight is 1000 g.
  • the average density of the lignocellulose-containing starting materials according to the invention, from which the lignocellulose-containing particles or fibers are produced, is arbitrary and is generally 0.2 to 0.9 g / cm 3 , preferably 0.4 to 0.85 g / cm 3 , more preferably at 0.4 to 0.75 g / cm 3 , in particular at 0.4 to 0.6 g / cm 3 .
  • Density here means the bulk density under normal conditions (20 ° C./65% air humidity), as defined in DIN 1306, ie taking into account the cavities contained in the lignocellulose-containing starting material, eg the log.
  • Suitable binders selected from the group of aminoplast resins or their mixtures (component A) are all those skilled in the art, preferably the aminoplast resins known for the production of wood materials. Such resins and their preparation are described, for example, in Ullmanns Enzyklopadie der ischen Chemie, 4th, revised and expanded edition, Verlag Chemie, 1973, pages 403 to 424 "Aminoplasts” and Ullmann's Encyclopedia of Industrial Chemistry, Vol. A2, VCH Verlagsgesellschaft, 1985, pages 15 to 141 "Amino Resins” and in M. Dunky, P.
  • Preferred polycondensation products are urea-formaldehyde resins (UF resins), melamine-formaldehyde resins (MF resins) or melamine-urea-formaldehyde resins (MUF resins), particularly preferred urea-formaldehyde resins and melamine-urea-formaldehyde resins with little melamine ( ⁇ 10% wt .-% based on the total weight of the aqueous resin), for example Kaurit ® glue types from BASF SE.
  • urea-formaldehyde resins U resins
  • melamine-containing urea-formaldehyde resins UDF resins
  • the molar ratio of formaldehyde to NH 2 group in the range from 0.3: 1 to 1 : 1, preferably 0.3: 1 to 0.6: 1, more preferably 0.3: 1 to 0.5: 1, most preferably 0.3: 1 to 0.45: 1.
  • the aminoplast resins mentioned are usually used in liquid form, usually as a 25 to 90% strength by weight, preferably as a 50 to 70% strength by weight solution or suspension.
  • the pH values of these aqueous aminoplast resins are generally between 6.5 and 9.5, preferably between 7 and 9, particularly preferably between 7.2 and 8.8.
  • Suitable components B are organic or inorganic acid or carboxylic anhydride or carboxylic acid chloride and acidic salt and mixtures thereof, preferably organic acid or carboxylic anhydride, more preferably carboxylic anhydride.
  • Suitable inorganic acids are, for example, hydrochloric acid, boric acid, perchloric acid, phosphoric acid, polyphosphoric acid, nitric acid, nitrous acid, sulfuric acid and sulfurous acid and mixtures thereof, preferably phosphoric acid, polyphosphoric acid, salicylic acid, nitrous acid, sulfuric acid and sulfurous acid and mixtures thereof, in particular - It prefers nitric acid and sulfuric acid.
  • Suitable organic acids are monoesters of sulfuric acid, solphonic acids, phosphonic acids and organic carboxylic acids and mixtures thereof.
  • Suitable organic carboxylic acids are, in particular, those having a molecular weight of less than 2,000 g / mol, preferably less than 1,000 g / mol, particularly preferably less than 500 g / mol.
  • Suitable organic acids are C1 to C15 carboxylic acids such as formic acid, acetic acid, glycolic acid, maleic acid, fumaric acid, succinic acid, itaconic acid, benzoic acid, phthalic acid, sebacic acid, citric acid, sorbic acid, itaconic acid, tartaric acid, oxalic acid, methanesulphonic acid, p Toluenesulfonic acid and malonic acid.
  • Preferred organic carboxylic acids are maleic acid, fumaric acid, succinic acid, p-toluenesulfonic acid and acetic acid, more preferably maleic acid.
  • Suitable organic carboxylic anhydrides and carboxylic acid chlorides are those having a molecular weight of less than 2,000 g / mol, preferably less than 1,000 g / mol, particularly preferably less than 500 g / mol.
  • Suitable organic carboxylic acid chlorides are C.sub.2 to C.sub.20 carboxylic acid chlorides, such as, for example, acetic acid chloride and phthalic acid chloride, preferably C.sub.2 to C.sub.15 carboxylic acid chlorides, very particularly preferably C.sub.2 to C.sub.5 carboxylic acid chlorides.
  • Suitable organic carboxylic anhydrides are C 2 -C 5 -carboxylic anhydrides, such as acetic anhydride, succinic anhydride, phthalic anhydride, glutaric anhydride, polymaleic anhydride, perylenetetracarboxylic anhydride, itaconic anhydride, maleic anhydride, preferably C 4 - to cis-carboxylic anhydrides, such as succinic anhydride, phthalic anhydride, maleic anhydride , Particularly preferably C 4 - to Cs-carboxylic acid anhydrides such as succinic anhydride, itaconic anhydride and maleic anhydride, most preferably maleic anhydride.
  • C 2 -C 5 -carboxylic anhydrides such as acetic anhydride, succinic anhydride, phthalic anhydride, glutaric anhydride, polymaleic anhydride, perylenetetracarboxylic anhydride, it
  • Suitable acid salts are acidic metal salts, for example acidic aluminum, zinc or magnesium salts. These can be used for example in the form of nitrates, chlorides or sulfates. Particularly suitable are aluminum sulfate, aluminum nitrate and aluminum chloride.
  • Ammonium salts are not counted according to the invention to the group of acidic salts.
  • inorganic or organic acid which has a pKa value of less than 5, preferably less than 4, particularly preferably less than 3, or organic carboxylic acid anhydrides whose corresponding carboxylic acids have a pKa of less than 5, preferably less than 4, particularly preferably less than 3 more preferably, organic carboxylic anhydrides whose corresponding carboxylic acids have a pKs value of less than 5, preferably less than 4, more preferably less than 3.
  • polybasic acids for example in the case of carboxylic acids having a plurality of carboxyl groups (dicarboxylic acids, tricarboxylic acids, etc.), the pKs value of the first protolysis stage counts here.
  • the acid equivalents of the corresponding acids are understood in moles which have a pKa value of less than 7 in order to determine the acid equivalents.
  • component B may be added in liquid or solid form to the lignocellulosic particles.
  • Component B can be mixed with other components before addition, for example with component C, and then added as an aqueous solution.
  • the addition is in a form which contains no or only very little component C, ie as a liquid (for example acetic acid as the icesig), as a solid (for example maleic acid) or in the case of acid anhydrides as a solution in component D (for Example, phthalic anhydride in pMDl).
  • the addition of acids which have a melting point of> 30 ° C, as a solid and particularly preferably the addition of acid anhydrides as a solution in component D.
  • Very little component C here, less than 5 wt .-%, preferably less than 2 wt .-%, more preferably less than 1 wt .-% of component C based on the weight of component B.
  • component C can be applied to the lignocellulose particles separately or as a mixture with one or more components (A, B, D, E, F or G).
  • the quantity given for component C refers to the total amount of water applied to the lignocellulose particles in the preparation of the core layer mixture. The water, which is contained as residual moisture in the lignocellulose particles, is not counted as component C.
  • the amount of component C) is preferably selected such that a total moisture content of 2 to 12% by weight, preferably 3 to 9% by weight, particularly preferably 4 to 8% by weight, is used for the mixture of the core layer. % results.
  • the total moisture is determined based on EN 322. For this purpose, 20 g of the mixture are dried in a drying oven at a temperature of 103 ° C to constant mass. After cooling in a desiccator, the sample is weighed. The total moisture in% is calculated from the difference between the mass of the mixture before and after drying, based on the mass after drying.
  • the binders based on isocyanate (component D) contain according to the invention at least one polynuclear diphenylmethane diisocyanate.
  • Polynuclear diphenylmethane diisocyanate is understood according to the invention to mean polynuclear diphenylmethane diisocyanate having 3 or more kines, which is also referred to as oligomeric diphenylmethane diisocyanate.
  • the polynuclear diphenylmethane diisocyanate we preferably used in admixture with other polyisocyanates, in particular binuclear diphenylmethane diisocyanate.
  • the (number average) NCO functionality of the diphenylmethane diisocyanate used can vary in the range from greater than 2 to about 4, preferably from 2.1 to 3, in particular from 2.5 to 2.9.
  • the binders (component D) may additionally comprise 2,2'-diphenylmethane diisocyanate, 2,4'-diphenylmethane diisocyanate, 4,4'-diphenylmethane diisocyanate, further (other) polyisocyanates, in particular further aromatic polyisocyanates , preferably toluene diisocyanate (TDI) [such as toluene-2,4-diisocyanate (2,4-TDI) and toluene-2,6-diisocyanate (2,6-TDI)] or mixtures of two or more of the aforementioned compounds, or Roh -MDI, which is obtained in the production of MDI contained.
  • TDI toluene diisocyanate
  • Roh -MDI which is obtained in the production of MDI contained.
  • polynuclear MDI in admixture with binuclear MDI, in particular 4,4'-MDI and optionally 2,4'-MDI.
  • Component D preferably contains from 20 to 70% by weight of 4,4'-MDI, based on the total weight of component D, in particular from 25 to 50% by weight, particularly preferably from 30 to 45% by weight.
  • Component D preferably contains from 25 to 70% by weight of 4,4'-MDI, from 0 to 20% by weight of 2,4'-MDI and from 10 to 80% by weight of multinuclear MDI, in each case based on the total weight component D.
  • Component D contains particularly preferably from 20 to 70% by weight, in particular from 25 to 50% by weight, of 4,4'-MDI, from 0 to 20% by weight, in particular from 1 to 17% by weight, particularly preferably from 1 to 12% by weight, very particularly preferably from 1 to 10% by weight of 2,4'-MDI and from 10 to 80% by weight, in particular from 30 to 70% by weight, most preferably from 40 to 60% by weight of multinuclear MDI, in each case based on the total weight of component D.
  • Such binders are known and are sold, for example, by BASF SE and BASF Polyurethanes GmbH under the name Lupranat®.
  • the content of isocyanate groups of component D is preferably from 5 to 10 mmol / g, in particular from 6 to 9 mmol / g, particularly preferably from 7 to 8.5 mmol / g. It is known to the person skilled in the art that the content of isocyanate groups in mmol / g and the so-called equivalence weight in g / equivalent are in a reciprocal ratio. The content of isocyanate groups in mmol / g is calculated from the content in% by weight according to ASTM D-5155-96 A.
  • the viscosity of the component D used can vary within a wide range.
  • the component D has a viscosity of 10 to 1000 mPa * s, more preferably from 100 to 650, in particular from 150 to 250 mPa * s at 25 ° C, on.
  • component D is used completely or partially in the form of polyisocyanate prepolymers.
  • polyisocyanate prepolymers are obtainable by reacting all or some of the polyisocyanates described above in advance with isocyanate-reactive polymeric compounds to form the isocyanate prepolymer.
  • the reaction takes place in excess of the polyisocyanate component, for example at temperatures of 30 to 100 ° C., preferably at about 80 ° C.
  • Suitable polymeric compounds having isocyanate-reactive groups are known to the person skilled in the art and are described, for example, in "Kunststoffhandbuch, 7, Polyurethane", Carl Hanser-Verlag, 3rd edition 1993, Chapter 3.1.
  • Suitable polymeric compounds containing isocyanate-reactive groups are in principle all known compounds having at least two isocyanate-reactive hydrogen atoms, for example those having a functionality of 2 to 8 and a number average molecular weight M n of 400 to 15,000 g / mol.
  • compounds selected from the group of polyether polyols, polyester polyols or mixtures thereof can be used.
  • Suitable prepolymers are for example carried out in DE 10314762.
  • the NCO content of the prepolymers used is preferably in the range from 20 to 32.5%, particularly preferably from 25 to 31%.
  • the NCO content is determined according to ASTM D-5155-96 A).
  • oligomeric diphenylmethane diisocyanate or diphenylmethane diisocyanates can be used in admixture with other binders.
  • suitable binders are, for example, other organic isocyanates having two or more isocyanate groups, mixtures thereof and prepolymers of isocyanates and polyols or amines having at least two isocyanate groups and mixtures thereof, in particular all those skilled in the art, preferably those for the production of wood-based materials or polyurethanes known, organic isocyanates or mixtures thereof into consideration.
  • Suitable ammonium salts are all ammonium salts known per se. These show a latent hardening of aminoplast resins (M. Dunky, P. Niemz, wood materials and glues, Springer 2002, pages 265 to 269), and are therefore also referred to as latent hardeners.
  • latent means that the curing reaction does not occur immediately after the aminoplast resin and the hardener have been mixed, but is delayed, or after activation of the hardener by, for example, Temperature. The delayed cure increases the processing time of an aminoplast resin-hardener mixture.
  • latent hardeners can also have an advantageous effect for the mixture of the lignocellulose particles with aminoplast resin, hardener and the other components, since it can lead to a lower precuring of the aminoplast resin before process step (IV).
  • Preferred latent hardeners are ammonium chloride, ammonium bromide, ammonium iodide, ammonium sulfate, ammonium sulfite, ammonium methanesulfonate, ammonium phosphate, ammonium nitrate or mixtures thereof, preferably ammonium sulfate, ammonium nitrate, ammonium chloride or mixtures thereof, more preferably ammonium sulfate, ammonium nitrate or mixtures thereof.
  • ammonium salts which have an acidic counterion such as ammonium hydrogensulfite, ammonium hydrogenphosphate or ammonium hydrogencarbonate.
  • ammonium hydrogensulfite such as ammonium hydrogensulfite, ammonium hydrogenphosphate or ammonium hydrogencarbonate.
  • ammonium hydrogencarbonate such as ammonium hydrogensulfite, ammonium hydrogenphosphate or ammonium hydrogencarbonate.
  • Formaldehyde scavengers are understood as meaning all chemical compounds of any molecular weight which generally have a free electron pair which reacts chemically with the formaldehyde, ie binds the formaldehyde chemically, as a rule virtually irreversibly.
  • Such lone pairs of electrons can be found, for example, on the following functional groups of organic or inorganic compounds: primary, secondary and tertiary amino group, hydroxyl group, sulfite group, amides, imines, imides.
  • a preferred group of formaldehyde scavengers is that which contains chemical compounds of any molecular weight, the chemical compounds containing at least one N atom having at least one lone pair of electrons, for example: ammonia, urea, melamine, organic C to Cio amines , Polymers carrying at least one amino group, such as polyamines, polyimines, polyureas, poly-lysines, polyvinylamine, polyethyleneimine.
  • formaldehyde scavengers are sulfur-containing salts such as alkali metal sulfite, for example sodium sulfite, alkali metal thiosulfate, for example sodium thiosulfate or salts of organic sulfur compounds, for example thiocarboxylates.
  • alkali metal sulfite for example sodium sulfite
  • alkali metal thiosulfate for example sodium thiosulfate
  • salts of organic sulfur compounds for example thiocarboxylates.
  • Ammonium salts with these sulfur-containing anions are also suitable in principle, but are to be assigned to component D in the context of the invention.
  • component F is urea.
  • the urea can be used either in solid form or in the form of an aqueous solution. If urea is added to the binder system, then the molar ratio of formaldehyde to NH 2 group in the binder system changes, since the urea groups are added to the NH 2 groups of the aminoplast resin.
  • the molar ratio of formaldehyde to NH 2 group (from urea and melamine) in the binder system results from the molar ratio of formaldehyde to NH 2 group of component A and the urea (component F) and is preferably in the range of 0.25 : 1 to 1: 1, preferably from 0.25: 1 to 0.55: 1, more preferably from 0.25: 1 to 0.45: 1, most preferably from 0.25: 1 to 0.40: 1.
  • Suitable additives are all additives known per se with the exception of component L, component A, component B and component C and also component D, component E and component F.
  • Suitable additives are e.g. Release agents, water repellents such as paraffin emulsions, wood preservatives, dyes, pigments, fillers, rheology aids, flame retardants, cellulose, e.g. nanocrystalline cellulose or cellulose-i-cellulose.
  • component G preferably only paraffin emulsions are used.
  • Another object of the present invention are the lignocellulosic materials which are obtainable according to the inventive method.
  • the wood-based materials according to the invention are used in particular in furniture construction, house construction, interior work and trade fair construction.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Forests & Forestry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dry Formation Of Fiberboard And The Like (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

La présente invention concerne un procédé pour produire des matières lignocellulosiques monocouches ou multicouches à partir d'une couche centrale (KS) et, le cas échéant, d'autres couches (WS), le mélange des composants A, B, C et, le cas échéant, D, E et F, qui sont utilisés pour la production du mélange pour la couche centrale, présente un temps de gélification à 60 °C (GZ60) de 10 à 450 secondes et des conditions spéciales étant respectées à l'étape (IV) du procédé.
PCT/EP2018/083277 2017-12-13 2018-12-03 Procédé de production de matières lignocellulosiques monocouches ou multicouches dans des conditions spéciales sous presse chaude WO2019115261A1 (fr)

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US4117200A (en) * 1973-06-21 1978-09-26 American Cyanamid Company Fire retardant wood products
WO1997028936A1 (fr) 1996-02-08 1997-08-14 Kramer Juergen Procede et dispositif de production continue de plaques de particules contenant de la lignocellulose
DE10314762A1 (de) 2003-03-31 2004-10-14 Basf Ag Verfahren zur Herstellung von Polyurethan-Weichschaumstoffen
EP1852231B1 (fr) 2006-05-02 2013-10-02 Kronotec AG Procédé de fabrication de matériaux dérivés du bois dotés d'une faible émission en composés organiques volatiles, matériaux dérivés du bois ainsi disponibles tout comme utilisation d'additifs définis pour éviter la libération de composés organiques volatiles en matériaux dérivés du bois et produits de concassage du bois en lignocellulose
WO2015000913A1 (fr) 2013-07-05 2015-01-08 Basf Se Substances à base de lignocellulose comportant des particules de matière plastique expansées munies d'un revêtement
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US4117200A (en) * 1973-06-21 1978-09-26 American Cyanamid Company Fire retardant wood products
WO1997028936A1 (fr) 1996-02-08 1997-08-14 Kramer Juergen Procede et dispositif de production continue de plaques de particules contenant de la lignocellulose
DE10314762A1 (de) 2003-03-31 2004-10-14 Basf Ag Verfahren zur Herstellung von Polyurethan-Weichschaumstoffen
EP1852231B1 (fr) 2006-05-02 2013-10-02 Kronotec AG Procédé de fabrication de matériaux dérivés du bois dotés d'une faible émission en composés organiques volatiles, matériaux dérivés du bois ainsi disponibles tout comme utilisation d'additifs définis pour éviter la libération de composés organiques volatiles en matériaux dérivés du bois et produits de concassage du bois en lignocellulose
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