CN114456422B - Preparation method of high-adhesiveness thick brightening polyester base film - Google Patents

Preparation method of high-adhesiveness thick brightening polyester base film Download PDF

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CN114456422B
CN114456422B CN202210229751.5A CN202210229751A CN114456422B CN 114456422 B CN114456422 B CN 114456422B CN 202210229751 A CN202210229751 A CN 202210229751A CN 114456422 B CN114456422 B CN 114456422B
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coating
base film
extrusion
parts
film
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CN114456422A (en
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张玲
杨彪
李彬彬
刘金伟
张凝
孙楠楠
董相岗
魏永波
王锐
宋晓燕
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Shandong Snton Optical Material Technology Co ltd
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Shandong Snton Optical Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C37/00—Component parts, details, accessories or auxiliary operations, not covered by group B29C33/00 or B29C35/00
    • B29C37/0092—Drying moulded articles or half products, e.g. preforms, during or after moulding or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
    • B29C55/06—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique parallel with the direction of feed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/10—Surface shaping of articles, e.g. embossing; Apparatus therefor by electric discharge treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/048—Forming gas barrier coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2300/00—Characterised by the use of unspecified polymers
    • C08J2300/12—Polymers characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2400/00—Characterised by the use of unspecified polymers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2475/04—Polyurethanes
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
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    • C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract

The invention relates to the technical field of polyester optical films, in particular to a preparation method of a high-adhesiveness thick brightening polyester base film. The method comprises the steps of raw material preparation, extrusion, longitudinal stretching, coating, drying and transverse stretching, wherein the raw material preparation comprises resin and inorganic nano material defoamer; the extrusion comprises the steps of first extrusion raw material mixing extrusion and second extrusion raw material mixing extrusion, wherein melt of the first extrusion and the second extrusion are filtered and then are gathered in a coextrusion system to be longitudinally stretched; coating, namely, coating an uncoated substrate film to form a base film after electrostatic adsorption of the longitudinally stretched substrate film; the drying is to carry out hot air drying on the coated base film and then transversely stretching the base film. The product is mainly a thick brightening base film product with the thickness of 180-260um, is applied to liquid crystal screens, mobile phones, flat plates, vehicle navigation, cloth film plates, engineering marks and the like, can also be applied to liquid crystal displays and other electronic fields, and has high surface tension and adhesive force.

Description

Preparation method of high-adhesiveness thick brightening polyester base film
Technical Field
The invention relates to the technical field of polyester optical films, in particular to a preparation method of a high-adhesiveness thick brightening polyester base film.
Technical Field
The brightness enhancement film is a key component of a liquid crystal display backlight module, is applied to a TFT-LCD backlight module, is a film or a sheet aiming at improving the luminous efficiency of the whole backlight system, utilizes a special prism structure of the brightness enhancement film, concentrates light rays in all aspects to a central viewing angle through optical principles such as refraction, total reflection, light accumulation and the like, recycles the light which is not utilized outside the viewing angle through light reflection, reduces the loss of light, improves the overall brightness and uniformity, plays the effects of increasing the brightness and controlling the visual angle for the display of an LCD panel, and further improves the brightness and the control of the visual angle of the LCD panel. The existing base film production generally comprises the processes of raw material configuration, extrusion, stretching, coating, drying and the like, because the temperature set by each section (a feeding section, a compression section and a metering section) of the extruder is too high or too low, sometimes the extrusion screw and the materials are interwoven together to lock the screw, if the screw extruder lacks a good protection device, a strong driving force can twist the screw, the screw can be jammed to generate unusually large resistance, and serious damage to the surface of the screw and serious scratch of a machine barrel are caused; secondly, in the coating process, the traditional coating is that a coating roller and a base film run at the same speed and in the same direction, so that the shearing force generated by the coating liquid can generate wiredrawing and small liquid drops, and the wiredrawing and the small liquid drops splash on the base film again, so that the appearance of the base film is defective; thirdly, in the coating liquid formula, no nano particles such as regulator are added in many enterprises or search patents, so that the adhesion force between the coating and the base film is poor, and the coating falls off in the subsequent processing of the base film. Due to the defects in the process, the brightness enhancement base film sometimes has poor adhesive force or defects such as crystal points or bubbles on the film surface, which cause the defects of brightness and definition, and the phenomena of unqualified polyester base film such as poor hardness, tension and stripping force performance, and the like. In view of the drawbacks of the prior art, there is a need for improvements in processes related to film adhesion and the like in polyester-based film processes.
Disclosure of Invention
The invention aims to solve the technical problem of the defects existing in the prior art and provides a preparation method of a high-adhesiveness thick brightening polyester base film. The method utilizes the physical adsorption principle to pre-coat a layer of base film with stable orientation, and the distance between molecules of the coating liquid is shortened, so that the wettability of the film is increased, and the adhesive force of the pre-coating film is increased.
The technical scheme of the invention comprises the following steps:
the preparation method of the high-adhesiveness thick brightening polyester base film comprises the steps of raw material preparation, extrusion, longitudinal stretching, coating, drying and transverse stretching, wherein: the raw material configuration comprises: the first extrusion raw material comprises 80-90 parts by weight of resin and 10-20 parts by weight of inorganic nano material; the second extrusion raw material comprises 70-90 parts by weight of resin, 5-20 parts by weight of inorganic nano material and 5-10 parts by weight of defoamer;
the extrusion comprises: after the first extrusion raw materials are mixed, the thickness of the extruded melt is 50-100um under the conditions that the temperature is 300-350 ℃ and the extrusion pressure is 2-10MPa by a first extruder; mixing the second extrusion raw materials, and extruding the mixture into a melt with the thickness of 60-150um by a second extruder under the conditions that the temperature is 290-340 ℃ and the extrusion pressure is 2-9 MPa; the first extruded melt and the second extruded melt are respectively filtered with the filtering precision of 10-25um and then are gathered into a two-layer co-extrusion system;
The longitudinal stretching is to pass the extruded polyester film through a preheating zone of 60-90 ℃, a stretching zone of 90-120 ℃ and a cooling zone of 30-60 ℃ to form a substrate film with a stretching multiple of 3.6-4.0;
the coating is to coat the uncoated substrate membrane to form a base membrane after electrostatic adsorption of the longitudinally stretched substrate membrane;
the drying is to carry out hot air drying on the coated base film, wherein the drying time is 2-10 s, and the temperature of hot air drying is set to be 80-145 ℃;
the transverse stretching is formed by coating and drying a base film, and then passing through a preheating section with the temperature of 100-130 ℃, a stretching section with the temperature of 130-160 ℃, a shaping section with the temperature of 260-280 ℃ and a cooling section with the temperature of 30-60 ℃ and controlling the stretching multiple to be 3.0-4.0.
The preparation method of the high-adhesiveness thick brightening polyester base film also comprises the following steps: flattening and corona treating the transversely stretched base film to make the surface roughness Rmax=0.210-0.50, eliminating static electricity and rolling to obtain the double-layer polyester base film with thickness of 180-260 microns.
The technical scheme further comprises the following steps:
the resin comprisesOne or more of polyethylene (EP), polyethylene terephthalate (PET), high Density Polyethylene (HDPE), liquid Crystal Polymer (LCP), aromatic polyester (ARP); the inorganic nanomaterial includes silica (SiO 2 ) Aluminum oxide (Ai) 2 O 3 ) Barium sulfate (BaSO) 4 ） 、 One or more of aluminum nitride (AlN);
the defoaming agent comprises one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene alcohol amine ether, methyl silicone oil, ethyl silicone oil and organic silicon defoaming agent.
The coating is to coat the coating on the surface of the substrate membrane in a shearing mode, and the coating liquid on the surface layer is controlled to be neat and uniform by a coating scraper.
Further, the included angle alpha between the uncoated substrate film and the coating roller in the coating process is less than or equal to 80 ℃, the rotating direction of the coating roller is opposite to the running direction of the substrate film, the substrate film is coated on one side or both sides, and the coating parameters are all 5-10g/m 2 。
The coating liquid components in the coating process comprise: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propylene glycol, 5-10 parts of flatting agent, 1-5 parts of silane coupling agent, 1-5 parts of regulator, 1-5 parts of adhesion promoter and 1-5 parts of nano aluminum oxide.
Further, the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol, polyvinyl alcohol (Z-200H) and polyvinyl alcohol (Z-200); the leveling agent is one or more of polydimethylsiloxane, alkyl modified organosiloxane, acrylic acid, organosilicon leveling agent and polyether modified silicone oil; the silane coupling agent is one or more of a multifunctional silane coupling agent, a water-based silane coupling agent, an epoxy silane coupling agent and a protective silane coupling agent; the regulator comprises one or more of oleamide, a silicon dioxide opening agent, dodecanol and polyoxyethylene oleate; the adhesion promoter is one or more of phosphoric acid methacrylate, amino organosilicon polymer, PP adhesion treating agent, adhesion enhancer (LT-1736), phosphate compound (ADP-S479), organic metal ester chelate (ADP-S478) and organic compound (ADP-S481).
Further, the preparation of the coating liquid is to add 3-20wt% of aqueous solution into 10-20wt% of aqueous polyurethane solution to obtain mixed solution; adding a silane coupling agent, stirring to enable the pH value of the solution to be 7-9, standing for 20-40 minutes, adding a regulator, stirring while adding a leveling agent, enabling the pH value of the solution to be 7-9, standing for 8-15 minutes, adding propylene glycol, stirring for 3-8 minutes, and adding an adhesion promoter and nano aluminum oxide to obtain the high-adhesion polymer coating liquid.
Further, the two-layer co-extrusion system in the extrusion process adopts a composite membrane head, the melt of the first extruder and the melt of the second extruder enter the upper side of a membrane cavity of the composite membrane head, the melt is symmetrical by the center line of the membrane cavity, the co-extrusion temperature is controlled to be 350-370 ℃, the first material conveying pipeline in the first fine filter and the second material conveying pipeline in the second fine filter are converged and overlapped in the composite membrane head under the condition of 3-10Mpa, the overlapped surfaces flow in each layer of flow channel, the melt of the flow channel is extruded after reaching a membrane lip, and the polyester membrane is formed by cooling at 60-100 ℃.
Further, the longitudinally stretched uncoated substrate film is subjected to electrostatic adsorption, and then the uncoated substrate film is coated.
The invention solves the problem of the adhesive force of the thick brightening base film, enhances the adhesion and crosslinking combination of materials through the molecular interaction between the coating and the base material, and the treated coating process ensures that the coating has good water resistance, strong adhesive force, good leveling property, good glossiness and strong oxidation resistance, can keep excellent gas barrier property, and has the characteristics of mechanical combination, physical adsorption and the like. Products have been successfully developed and adopted by flat-panel televisions, electronic equipment and other industries, and a brighter, lighter and more power-saving solution is provided for the field of liquid crystal display. The thickness of the thick brightening base film product prepared by the invention is within 180-260um, and the thick brightening base film product can be applied to mobile phones, flat plates, vehicle navigation, cloth film plates, engineering marks and the like, and can also be applied to liquid crystal displays and other electronic fields. The invention adopts the aqueous coating liquid and the metal oxide nano particles on the coating material, so that the product has higher hardness and good surface tension and adhesive force.
Drawings
FIG. 1 is a schematic diagram of a two-layer coextrusion system according to one embodiment of the present invention;
FIG. 2 is a schematic diagram of an embodiment of a coating system according to the present invention;
FIG. 3 is an enlarged view of the structure of a base film product of the present invention;
FIG. 4 is a graph showing the relationship between the temperature and the adhesion of the product prepared by the invention;
FIG. 5 is a graph showing the relationship between the coating time and the adhesion of the product prepared by the invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the attached drawings and specific embodiments.
Example 1, a method for preparing a high adhesion thick brightness enhancement polyester base film, the prepared product is structurally a two-layer structure, namely a base film 17 and a coating layer 18 (refer to fig. 3), and the main technical indexes are as follows: an average thickness of 180-260um; surface roughness rmax=0.210-0.50.
Referring to fig. 1, the extrusion system according to the present invention comprises a composite membrane head (also called a double-layer co-extrusion system) 2, a first material conveying pipeline 3, a first extruder fine filter 4, a first extruder 5, a second extruder 6, a second extruder fine filter 7, and a second material conveying pipeline 8, wherein in the extrusion system, the first layer extruder 5 is connected with the first extruder fine filter 4 and is connected with the composite membrane head 2 through the first material conveying pipeline 3; the second layer extruder 6 is connected with the second extruder fine filter 7 and is connected with the composite membrane head 2 through a second material conveying pipeline 8, and the two layers of solution membranes enter the next process after the composite membrane head 2 is extruded to synthesize the integral membrane 1.
Referring to fig. 2, the coating system includes a coating liquid tank 9, a coating roller 10, a guide roller 11, a pull roller 13, a coating blade 14, and a frame 16. In the coating system, a traction roller 13, a guide roller 11 and a coating roller 10 are arranged on a frame 16, a coating liquid groove 9 is arranged right below the coating roller 10 between the two guide rollers 11 and is a single entity, and the center of the coating liquid groove is vertical to the center of the coating roller 10. The coating roller 10 is immersed in the liquid in the coating liquid tank 9, and about 1/10 of the diameter of the coating roller 10 is immersed in the coating liquid tank 9. In operation, the pull roll 13, the guide roll 11, and the coating roll 10 are connected by the uncoated substrate 12 and the post-coating base film 15.
Referring to fig. 1-3, a method for preparing a high adhesion thick brightness enhancing polyester base film, wherein the raw material configuration comprises a resin, an inorganic nanomaterial and a defoaming agent. Wherein: the resin material is one or more of polyethylene EP, polyethylene terephthalate PET, high-density polyethylene HDPE, liquid crystal polymer LCP and aromatic polyester ARP;
the inorganic nano material is SiO 2 、Ai 2 O 3 、BaSO 4、 AlN (one or more of silicon dioxide, aluminum oxide, barium sulfate and aluminum nitride respectively);
the defoaming agent is one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene alcohol amine ether, methyl silicone oil, ethyl silicone oil and organic silicon defoaming agent.
The preparation method of the high-adhesiveness thick brightening polyester base film comprises the following steps:
firstly, raw materials are matched, wherein the raw material formula of the first extruder comprises 80-90 parts by weight of resin and 10-20 parts by weight of inorganic nano material;
the raw material formula of the second extruder comprises 70-90 parts by weight of resin, 5-20 parts by weight of inorganic nano material and 5-10 parts by weight of defoamer.
The preparation method comprises the following steps:
step S1, raw materials of a first extruder are stirred and metered and then enter a first extruder 5, raw materials of a second extruder are stirred and metered and then enter a second extruder 6, the specifications and the models of the two extruders are the same, but the temperature of the first extruder is set to 300-350 ℃, and the extrusion pressure is set to 2-10MPa; the temperature of the second extruder is set to 290-340 ℃ and the extrusion pressure is set to 2-9MPa; the thickness of the melt extruded by the first layer extruder is 50-100um, and the thickness of the melt extruded by the second layer extruder is 60-150um; the extruded melt enters a first extruder fine filter 4 and a second extruder fine filter 7 respectively, the specifications and types of the two fine filters are the same, the filtering precision is 10-25um, the moisture, the oligomer and the impurity in the raw materials are removed, and the two layers of co-extrusion systems (composite membrane heads) 2 are collected after the filtration.
And S2, feeding the melt into the inner cavity of the film head from the side of the composite film head 2, wherein the melt is symmetrical along the center line of the film cavity, the temperature in the film head is set to be 350-370 ℃, the pressure is 3-10Mpa, a first material conveying pipeline 3 in a first fine extruder filter 4 and a second material conveying pipeline 8 in a second fine extruder filter 7 are converged and overlapped in the side of the composite film head, the overlapped surfaces flow in each layer of flow channels, the melt in the flow channels is extruded after reaching the film lips, and the melt is cooled at 60-100 ℃ to form the polyester film 1. The polyester film sheet 1 formed is fed into a longitudinal stretching process through a melt feed line.
Step S3, a longitudinal stretching system (also called a longitudinal stretching system) comprises a plurality of rotating roller components (20 rollers are selected in the embodiment), and the number of the rotating rollers is 1-8 # The roller is a preheating zone, the temperature is set to be 60-90 ℃ and 8-16 DEG C # The roller is a stretching region, the temperature is set to be 90-120 ℃ and 16-20 DEG C # The roller is a cooling zone, the temperature is set to be 30-60 ℃, and the stretching multiple is 3-4.
Step S4, after stretching in the longitudinal direction, the uncoated base material film sheet 12 is first corona-adsorbed and then coated. The uncoated substrate film 12 is drawn by the drawing roller 13 and passes through the guide rail 11 to the upper surface of the coating liquid tank, 1/10 of the diameter of the coating roller 10 is immersed into the liquid surface of the coating liquid tank, the contact point of the coating roller 10 and the substrate film forms an arc surface smaller than 90 degrees, and the included angle alpha between the substrate and the coating roller is preferably smaller than or equal to 80 degrees. The coating roller 10 rotates in the opposite direction to the substrate, the coating is to apply the coating on the surface of the substrate in a shearing manner, the coating scraper 14 makes the surface coating liquid neat and uniform, and the substrate film is coated on one side or both sides, wherein the coating parameters are 5-10g/m 2 The coated base film 15 enters a hot air drying device through a guide roller 11 and a traction roller 13, the drying time is 2-10 s, and the temperature of hot air drying is set to be 80-145 ℃.
S5, drying and then entering a transverse stretching system (also called a transverse stretching system), wherein the transverse stretching system is divided into a preheating section, a stretching section, a shaping section and a cooling section, the temperature of the preheating section is 100-130 ℃, the temperature of the stretching section is 130-160 ℃, the temperature of the shaping section is 260-280 ℃, the temperature of the cooling section is 30-60 ℃, and the stretching multiple is 3-4.
And S6, flattening the film through the transverse drawing system, carrying out corona treatment to enable the base film to reach a certain roughness, eliminating static electricity and rolling the base film, wherein the surface roughness Rmax=0.210-0.50, and obtaining the polyester base film with standard thickness (120-260 um). Referring to fig. 3, a base film 17 and a coating layer 18.
Example 2, a preparation method of a high-adhesiveness thick brightening polyester base film, comprises the following components in percentage by mass: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propylene glycol, 5-10 parts of flatting agent, 1-5 parts of silane coupling agent, 1-5 parts of regulator, 1-5 parts of adhesion promoter and 1-5 parts of nano aluminum oxide.
Specifically, the regulator is one or more of oleamide, silicon dioxide opening agent, dodecanol and polyoxyethylene oleate.
Specifically, the leveling agent is one or more of polydimethylsiloxane, alkyl modified organosiloxane, acrylic acid, organosilicon leveling agent and polyether modified silicone oil.
Specifically, the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymer compound JSC-1062 (produced by Jieka chemical Co., ltd., hangzhou), PP adhesion treating agent ( plastic technology Co., ltd.), adhesion enhancer LT-1736 (produced by Lobata New material Co., ltd., buddha), phosphate compound ADP-S479, organic metal ester chelate ADP-S478 and organic compound ADP-S481 (produced by Nanjing Netherlands New material Co., ltd.).
Specifically, the silane coupling agent is one or more of a polyfunctional silane coupling agent (X-12-981S polyfunctional silane coupling agent provided by Dongguan chemical Co., ltd.), an aqueous silane coupling agent (more organosilicon oligomer of ShinEtsu information of Japan provided by Dongguan chemical Co., ltd.), an epoxy silane coupling agent (KBM-903, japanese letter), and a protective silane coupling agent (X-12-967C protective silane coupling agent provided by Dongguan chemical Co., ltd.).
Specifically, the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (Japanese synthesis), and polyvinyl alcohol Z-200 (Japanese synthesis).
Specifically, a preparation method of the coating liquid based on the formula comprises the following steps: adding 3-20wt% aqueous solution of modified polyvinyl alcohol into 10-20wt% aqueous polyurethane solution to obtain 20-30 parts of mixed solution; adding 2-5 parts of silane coupling agent, stirring to enable the pH value of the solution to be 7-9, adding 5 parts of regulator when standing for 30 minutes, adding 10 parts of flatting agent while stirring to enable the pH value of the solution to be 7-9, adding 20 parts of propylene glycol after standing for 10 minutes, stirring for 5 minutes, adding 5 parts of adhesion promoter and 5 parts of nano aluminum oxide (the parts by weight are all above), and promoting the adhesive force of the coating to obtain the high-adhesion polymer coating liquid.
Example 3 this example provides a method for preparing a high adhesion thick brightness enhancing polyester base film, which is structurally two layers, including a base film 17 and a coating layer 18. The extrusion system and the coating system are particularly important in each process of the preparation method. The extrusion and coating system (see fig. 1 and 2) comprises a composite film head 2, a first feed delivery line 3, a first extruder fine filter 4, a first extruder 5, a second extruder 6, a second extruder fine filter 7, a second feed delivery line 8, a coating liquid tank 9, a coating roller 10, a guide roller 11, a pull roller 13, a coating blade 14 and a frame 16.
The application system of the embodiment is as follows: in the extrusion system, a first extruder 5 is connected with a first extruder fine filter 4 and is also connected with a composite membrane head 2 through a first conveying pipeline 3; the second extruder 6 is connected with the second extruder fine filter 7 and is connected with the composite membrane head 2 through a second material conveying pipeline 8, the first material conveying pipeline 3 and the second material conveying pipeline 8 are overlapped and enter the composite membrane head 2, and two layers of cast sheets are extruded and synthesized by the composite membrane head 2 to form an integral membrane 1 and then enter the next longitudinal stretching process.
In the coating system, the drawing roll 13, the guide roll 11 and the coating roll 10 are mounted on a frame 16, the coating liquid tank 9 is a single entity below the frame 16 (below the coating roll 10), the center of the coating liquid tank is vertical to the center of the coating roll 10, the coating roll 10 is immersed in the liquid in the coating liquid tank 9, and about 1/10 of the diameter of the coating roll 10 is immersed in the coating liquid tank 9. In operation, the web is connected by the pull roll 13, the guide roll 11, the coating roll 10, the uncoated substrate 12 and the post-coating base film 15.
The main components of the raw materials of the high-adhesiveness thick brightening polyester base film of the embodiment are resin, inorganic nano material and defoamer.
Specifically, the resin raw material is one or more of EP, PET, HDPE, LCP, ARP (respectively polyethylene, polyethylene terephthalate, high-density polyethylene, liquid crystal polymer and aromatic polyester);
Specifically, the inorganic nanomaterial is SiO 2 、Ai 2 O 3 、BaSO 4、 AlN (respectively silicon dioxide, aluminum oxide, barium sulfate and aluminum nitride) or a plurality of AlN;
wherein, the alumina technical index of this embodiment: the appearance is white loose powder; crystalline form, alpha phase; the content is more than or equal to 99.9 weight parts; particle size = 30um; aluminum nitride technical index: the average crystal grain was 19.47nm, and the thermal conductivity was 320W/mk.
Specifically, the defoaming agent is one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene alcohol amine ether, methyl silicone oil, ethyl silicone oil and organic silicon defoaming agent.
The raw material formula of the first extruder of the embodiment comprises 80-90 parts by weight of resin and 10-20 parts by weight of inorganic nano material;
the raw material formulation of the second extruder in this embodiment is 70-90 parts by weight of resin, 10-20 parts by weight of inorganic nanomaterial, and 5-10 parts by weight of defoamer.
The main technical indexes of the final product of the embodiment are as follows: an average thickness of 180-260um; surface roughness rmax=0.210-0.50.
Specifically, the preparation method of the high-adhesiveness thick brightening polyester base film of the embodiment comprises the following steps:
step S1, the production line runs, wherein 80-90 parts by weight of resin and 10-20 parts by weight of inorganic nano material are mixed according to a raw material formula, the raw material of the first extruder enters a first extruder hopper, the raw material enters a first extruder 5 after stirring and metering, and 70-90 parts by weight of resin, 5-20 parts by weight of inorganic nano material and 5-10 parts by weight of defoaming agent are mixed according to a raw material formula, and the raw material enters a second extruder hopper. The raw materials of the second extruder are stirred and metered and then enter the second extruder 6, the specifications and the models of the two extruders are the same, but the temperature of the first extruder is set to 300-350 ℃, the extrusion pressure is 2-10MPa, the temperature of the second extruder is set to 290-340 ℃, the extrusion pressure is 2-9MPa, the thickness of a melt extruded by the first extruder is 50-100um, and the thickness of a melt extruded by the second extruder is 60-150 um; the extruded melt enters a first extruder fine filter 4 and a second extruder fine filter 7 respectively, the specifications and types of the two fine filters are the same, the filtering precision is 10-25um, the purpose is to remove moisture, oligomers and impurities in raw materials below 10um, and the raw materials are filtered and then collected into a co-extrusion system (composite membrane head) 2.
And S2, feeding the melt into the inner cavity of the die head from the side of the composite film head 2, wherein the melt is symmetrical along the central line of the film cavity, the temperature in the film head is set to be 350-370 ℃, the pressure is 3-10Mpa, after the melt of the first extruder pipeline 3 and the second extruder pipeline 8 enters the upper side of the film cavity of the co-extrusion system 2, the melt flows on the overlapped surface in each layer of flow channel, and the melt of the flow channel is cooled at 60-100 ℃ after reaching the film lip, so as to form the polyester film 1. The polyester film sheet 1 formed is passed through a melt transfer line down-draw longitudinal stretching process.
Step S3, a longitudinal stretching system comprises a plurality of rotating roller components, 1-8 # The roller is a preheating zone, the temperature is set to be 60-90 ℃ and 8-16 DEG C # The roller is a stretching region, the temperature is set to be 90-120 ℃ and 16-20 DEG C # The roller is a cooling zone, the temperature is set to be 30-60 ℃, and the stretching multiple is 3.0-4.0.
In step S4, referring to fig. 2, the film sheet 1 is stretched in the longitudinal direction and then formed into a base film, and electrostatic adsorption is required to adhere the coating liquid to the base film. The Chinese patents CN201610400465.5, CN202120059639.2, CN202110030866.7, CN202110537649.7, CN202110905954.7 and the like all have the expression of film electrostatic adsorption, the direct current voltage u generated by a high voltage generator is used, the electrostatic voltage is set to be 2-4KV, the direct current voltage forms a strong electrostatic field in an electrostatic adsorption device, positive ions cannot pass through a base film and are accumulated on the surface of the film to form film charges, and the like charges repel each other to form repulsive force between the two charges, so that the surface area of the film is increased and the film is electrostatically charged.
The uncoated base material 12 is led to the upper surface of the coating liquid groove 9 through the guide roller 11 under the traction of the traction roller 13, 1/10 of the diameter of the coating roller 10 is immersed into the coating liquid groove page, the contact point of the coating roller 10 and the base film forms an arc surface, and the included angle alpha between the base material and the coating roller is less than or equal to 80 degrees. The coating roller 10 rotates in the opposite direction to the substrate, the coating is to apply the coating on the surface of the substrate in a shearing manner, the coating scraper 14 makes the surface coating liquid neat and uniform, the substrate film is coated on one side or both sides, wherein the coating density parameters are 5-10g/m 2 The coated base film 15 enters a hot air drying device through a guide roller and a traction roller, the drying time is 2-10s, and the temperature of hot air drying is set to 80-145 ℃.
S5, drying and then entering a transverse stretching system, wherein the transverse stretching system is divided into a preheating section, a stretching section, a shaping section and a cooling section, the temperature of the preheating section is 100-130 ℃, the temperature of the stretching section is 130-160 ℃, the temperature of the shaping section is 260-280 ℃, the temperature of the cooling section is 30-60 ℃, and the stretching multiple is 3.0-4.0.
And S6, flattening the film through the transverse drawing system, and carrying out corona treatment (refer to patent numbers CN201610400465.5, CN202120059639.2, CN202110030866.7, CN202110537649.7, CN202110905954.7 and the like) to enable the base film to reach a certain roughness, wherein the surface roughness Rmax=0.210-0.50, eliminating static electricity and rolling to obtain the polyester base film with standard thickness (180-260 um). Reference is made to fig. 3, base film 17, coating layer 18.
In particular, the coating technology of this embodiment is the key of the technology of the present invention, and the coating liquid formula comprises the following components in mass: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propylene glycol, 5-10 parts of flatting agent, 1-5 parts of silane coupling agent, 1-5 parts of regulator, 1-5 parts of adhesion promoter and 1-5 parts of nano aluminum oxide.
Wherein, the regulator of the embodiment is one or more of oleamide, silicon dioxide opening agent, dodecanol and oleic polyoxyethylene ester; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organosiloxane, acrylic acid, organosilicon leveling agent and polyether modified silicone oil; the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymerization compound JSC-1062 (produced by JieXeca chemical Co., ltd., hangzhou), PP adhesion treating agent ( plastic technology Co., ltd.), adhesion enhancer LT-1736 (produced by Lintey New Material Co., ltd., buddha), phosphate compound ADP-S479, organic metal ester chelate ADP-S478, and organic compound ADP-S481 (produced by Nanjing Netherlands New Material technology Co., ltd.); the silane coupling agent is one or more of multifunctional silane coupling agent (X-12-981S multifunctional silane coupling agent provided by Dongguan chemical Co., ltd.), aqueous silane coupling agent (organosilicon oligomer of ShinEtsu letter in Japan provided by Dongguan chemical Co., ltd.), epoxy silane coupling agent (KBM-903, japanese letter, yue.), protective silane coupling agent (X-12-967C protective silane coupling agent provided by Dongguan chemical Co., ltd.); the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (Japanese synthesis), and polyvinyl alcohol Z-200 (Japanese synthesis).
Specifically, the high adhesion thick brightening polyester base film coating liquid synthesis technology of this embodiment: adding 3wt% aqueous solution of modified polyvinyl alcohol into 10wt% aqueous polyurethane solution to obtain 20 parts of mixed solution; adding 2.5 parts of silane coupling agent, stirring to enable the pH value of the solution to be 7-9, adding 1.5 parts of regulator when standing for 30 minutes, adding 5 parts of flatting agent while stirring to enable the pH value of the solution to be 7-9, adding 10 parts of propylene glycol after standing for 10 minutes, stirring for 5 minutes, adding 1.5 parts of adhesion promoter and 1.5 parts of nano aluminum oxide, and promoting the adhesion of the coating to obtain the high-adhesion polymer coating liquid.
The high adhesion thick brightness enhancement polyester base film coating technology of this example: the prepared coating liquid is poured into the coating liquid tank 9, the uncoated substrate 12 is fed onto the coating liquid tank 9 through the drawing roll 13 and the guide roll 11, and the coating roll 10 is rotated in the opposite direction to the substrate. Coating is to apply the coating to the substrate surface in a shear mode. The coating blade 14 makes the surface coating liquid clean and uniform, and no overflow phenomenon occurs. The reverse coating method ensures that the running directions of the coating roller 10 and the base material 12 are different, the supported contact surface of the coating roller 10 is very small, and the pinch roller is not arranged, so that the generated shearing force can not generate wiredrawing and small liquid drops, the coating is relatively uniform, the coating mode overcomes certain defects of the traditional coating, the coating is more uniform, the running speed of equipment is improved, and the pollution caused by external factors can be prevented.
The diameter of the applicator roll 10 is 40-60mm. In the coating, an arc surface is formed from the contact point of the coating roller 10 and the base film, and the included angle alpha between the base material and the coating roller is less than or equal to 60 degrees. In coating, it is most important to control the coating amount, so to speak, the ratio of the running speed of the base film to the speed of the coating roller. Technician test assay: when the speed ratio is 40-60%, coating starts; when the speed ratio=95 to 120%, uniform and regular coating is performed; when the speed ratio=130 to 210%, the coating amount increases; when the speed ratio=200% or more, the coating amount decreases, and an unstable phenomenon occurs.
Typically at a ratio of 90 to 130%, the thickness or weight of the coating can be effectively controlled and a uniform and consistent coating surface can be ensured. In practical conditions, the coating amount of the coating roll may vary within a range of ±10%. Different coating amounts can be obtained through a certain number of coating rollers with different line numbers, the economic effect is achieved, and the coating rollers are adjusted by combining the transmission ratio, so that the continuous coating amount can be basically obtained.
Example 4 based on the above example 3, this example is specifically based on raw material ratios and parameter adjustment.
The preparation method of the high-adhesiveness thick brightening polyester base film comprises the following steps:
Step S1, the production line runs, 90 parts by weight of resin and 20 parts by weight of inorganic nano material are fed into a first extruder hopper according to a raw material formula, raw materials of the first extruder are stirred and metered and fed into a first extruder 5, and 90 parts by weight of resin, 20 parts by weight of inorganic nano material and 10 parts by weight of defoamer are fed into a second extruder hopper according to the raw material formula. The raw materials of the second extruder are stirred and metered and then enter the second extruder 6, the specifications and the models of the two extruders are the same, but the temperature of the first extruder is set to 350 ℃, the extrusion pressure is 2MPa, the temperature of the second extruder is set to 340 ℃, the extrusion pressure is 3MPa, the thickness of a melt extruded by the first layer extruder is 100um, and the thickness of a melt extruded by the second layer extruder is 60um; the extruded melt enters a first extruder fine filter 4 and a second extruder fine filter 7 respectively, the specifications and the types of the two fine filters are the same, the filtering precision is 25um, the purpose is to remove moisture, oligomers and impurities in raw materials below 25um, and the co-extrusion system (composite membrane head) 2 is collected after filtration.
And S2, feeding the melt into the inner cavity of the die head from the side of the composite film head 2, wherein the melt is symmetrical along the central line of the film cavity, the temperature in the film head is set to be 370 ℃, the pressure is 3Mpa, after the melt of the first extruder pipeline 3 and the second extruder pipeline 8 enters the upper side of the film cavity of the co-extrusion system 2, the melt flows on the overlapped surface in each layer of flow channel, and after the melt of the flow channel reaches the film lip, the melt is cooled at 100 ℃ to form the polyester film 1. The polyester film sheet 1 formed is passed through a melt transfer line down-draw longitudinal stretching process.
Step S3, a longitudinal stretching system comprises a plurality of rotating roller components, 1-8 # The roller is a preheating zone, the temperature is set to 90 ℃ and 8-16 DEG C # The roller is a stretching area, the temperature is set to 120 ℃ and 16-20 DEG C # The rolls were cooled, the temperature was set at 60℃and the draw ratio was 4.0.
In step S4, referring to fig. 2, the film sheet 1 is stretched in the longitudinal direction and then formed into a base film, and electrostatic adsorption is required to adhere the coating liquid to the base film.
The uncoated substrate 12 is drawn by the drawing roll 13 and passed over the coating liquid tank 9 by the guide roll 11, 1/10 of the diameter of the coating roll 10 is immersed in the coating liquid tank page, and the contact point of the coating roll 10 with the base film forms a cambered surface. The included angle alpha between the substrate and the coating roller is less than or equal to 50 degrees. The coating roller 10 rotates in the opposite direction to the substrate, and the coating is performed by applying the coating material to the surface of the substrate in a shearing manner, and the coating blade 14 applies the surface layer coating liquidNeat and uniform, the base film is coated on one side or two sides, wherein the coating parameters are 10g/m 2 The coated base film 15 was fed into a hot air drying apparatus by a guide roller and a pull roller for 10 seconds, and the temperature of hot air drying was set to 145 ℃.
And S5, drying and then entering a transverse stretching system, wherein the transverse stretching system is divided into a preheating section, a stretching section, a shaping section and a cooling section, the temperature of the preheating section is 130 ℃, the temperature of the stretching section is 160 ℃, the temperature of the shaping section is 280 ℃, the temperature of the cooling section is 60 ℃, and the stretching multiple is 4.0.
And S6, flattening the film through the transverse drawing system, carrying out corona treatment to enable the base film to reach a certain roughness, eliminating static electricity and rolling the base film, wherein the surface roughness Rmax=0.210-0.50, and obtaining the polyester base film with standard thickness (180-260 um). Reference is made to fig. 3, base film 17, coating layer 18.
Specifically, the coating technology of this embodiment is the key of the technology of the present invention, and the coating liquid formula comprises the following components in mass: 20 parts of modified polyvinyl alcohol, 15 parts of waterborne polyurethane, 10 parts of propylene glycol, 5 parts of flatting agent, 1 part of silane coupling agent, 1 part of regulator, 1.5 parts of adhesion promoter and 1.5 parts of nano aluminum oxide.
Wherein, the regulator of the embodiment is one or more of oleamide, silicon dioxide opening agent, dodecanol and oleic polyoxyethylene ester; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organosiloxane, acrylic acid, organosilicon leveling agent and polyether modified silicone oil; the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymerization compound JSC-1062 (produced by JieXeca chemical Co., ltd., hangzhou), PP adhesion treating agent ( plastic technology Co., ltd.), adhesion enhancer LT-1736 (produced by Lintey New Material Co., ltd., buddha), phosphate compound ADP-S479, organic metal ester chelate ADP-S478, and organic compound ADP-S481 (produced by Nanjing Netherlands New Material technology Co., ltd.); the silane coupling agent is one or more of polyfunctional silane coupling agent, aqueous silane coupling agent, epoxy silane coupling agent and protective silane coupling agent; the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (Japanese synthesis), and polyvinyl alcohol Z-200 (Japanese synthesis).
The high-adhesiveness thick brightening polyester base film coating liquid synthesis technology of the embodiment: adding 3-20wt% aqueous solution of modified polyvinyl alcohol into 10-20wt% aqueous polyurethane solution to obtain mixed solution; adding a silane coupling agent, stirring to enable the pH value of the solution to be 7-9, adding a regulator when standing for 30 minutes, adding a leveling agent while stirring to enable the pH value of the solution to be 7-9, standing for 10 minutes, adding propylene glycol, stirring for 5 minutes, adding an adhesion promoter part and a nanometer aluminum oxide part, and promoting the adhesion of a coating to obtain the high-adhesion polymer coating liquid.
Example 5 based on the above example 3, this example is specifically based on raw material ratios and parameter adjustment.
The preparation method of the high-adhesiveness thick brightening polyester base film comprises the following steps:
step S1, the production line runs, and according to the raw material formula, 85 parts by weight of resin and 24.5 parts by weight of inorganic nano materials enter a hopper of a first extruder, and raw materials of the first extruder enter a first extruder 5 after being stirred and metered. 86 parts of resin, 15.5 parts of inorganic nano material and 8 parts of defoamer are fed into a second extruder hopper according to the raw material formula. The raw materials of the second extruder enter the second extruder 6 after being stirred and metered, the specifications and the models of the two extruders are the same, but the temperature of the first extruder is set to 330 ℃, the extrusion pressure is 7MPa, the temperature of the second extruder is set to 325 ℃, the extrusion pressure is 4.5MPa, the thickness of a melt extruded by the first extruder is 70um, and the thickness of a melt extruded by the second extruder is 65 um; the extruded melt enters a first fine filter 4 and a second fine filter 7 respectively, the specifications and types of the two fine filters are the same, the filtering precision is 20um, the purpose is to remove moisture, oligomers and impurities in raw materials below 20um, and the raw materials are filtered and then collected into a co-extrusion system (composite membrane head) 2.
And S2, feeding the melt into the inner cavity of the die head from the side of the composite film head 2, wherein the melt is symmetrical along the central line of the film cavity, the temperature in the film head is set to be 350 ℃, the pressure is 5Mpa, after the melt of the first extruder pipeline 3 and the second extruder pipeline 8 enters the upper side of the film cavity of the co-extrusion system 2, the melt flows on the overlapped surface in each layer of flow channel, and the melt of the flow channel is cooled at 80 ℃ after reaching the film lip, so as to form the polyester film 1. The polyester film sheet 1 formed is passed through a melt transfer line down-draw longitudinal stretching process.
Step S3, a longitudinal stretching system comprises a plurality of rotating roller components, 1-8 # The roller is a preheating zone, the temperature is set at 85 ℃ and 8-16 DEG C # The roller is a stretching zone, the temperature is set to 110 ℃, and the temperature is 16-20 DEG C # The rolls were cooled, the temperature was set at 80℃and the draw ratio was 3.9.
In step S4, referring to fig. 2, the film sheet 1 is stretched in the longitudinal direction and then formed into a base film, and electrostatic adsorption is required to adhere the coating liquid to the base film.
The uncoated substrate 12 is drawn by the drawing roll 13 and passed over the coating liquid tank 9 by the guide roll 11, 1/10 of the diameter of the coating roll 10 is immersed in the coating liquid tank surface, and the contact point of the coating roll 10 with the base film forms a cambered surface. The included angle alpha between the substrate and the coating roller is less than or equal to 75 degrees. The coating roller 10 rotates in the opposite direction to the substrate, the coating is to apply the coating on the surface of the substrate in a shearing manner, the coating scraper 14 makes the surface coating liquid neat and uniform, and the substrate film is coated on one side or both sides, wherein the coating parameters are 8.5g/m 2 The coated base film 15 was fed to a hot air drying apparatus by a guide roller and a pull roller for 10 seconds, and the temperature of hot air drying was set to 125 ℃.
And S5, drying and then entering a transverse stretching system, wherein the transverse stretching system is divided into a preheating section, a stretching section, a shaping section and a cooling section, the temperature of the preheating section is 110 ℃, the temperature of the stretching section is 140 ℃, the temperature of the shaping section is 260 ℃, the temperature of the cooling section is 50 ℃, and the stretching multiple is 4.0.
And S6, flattening the film through the transverse drawing system, carrying out corona treatment to enable the base film to reach a certain roughness, eliminating static electricity and rolling the base film, wherein the surface roughness Rmax=0.210-0.50, and obtaining the polyester base film with standard thickness (180-260 um). Reference is made to fig. 3, base film 17, coating layer 18.
Specifically, the coating liquid formulation of this embodiment comprises the following components in mass: 25 parts of modified polyvinyl alcohol, 18 parts of waterborne polyurethane, 15 parts of propylene glycol, 8 parts of flatting agent, 3 parts of silane coupling agent, 3 parts of regulator, 3.5 parts of adhesion promoter and 2.5 parts of nano aluminum oxide.
Wherein, the regulator of the embodiment is one or more of oleamide, silicon dioxide opening agent, dodecanol and oleic polyoxyethylene ester; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organosiloxane, acrylic acid, organosilicon leveling agent and polyether modified silicone oil; the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymerization compound JSC-1062 (produced by JieXeca chemical Co., ltd., hangzhou), PP adhesion treating agent ( plastic technology Co., ltd.), adhesion enhancer LT-1736 (produced by Lintey New Material Co., ltd., buddha), phosphate compound ADP-S479, organic metal ester chelate ADP-S478, and organic compound ADP-S481 (produced by Nanjing Netherlands New Material technology Co., ltd.); the silane coupling agent is one or more of polyfunctional silane coupling agent, aqueous silane coupling agent, epoxy silane coupling agent and protective silane coupling agent; the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (Japanese synthesis), and polyvinyl alcohol Z-200 (Japanese synthesis).
The high-adhesiveness thick brightening polyester base film coating liquid synthesis technology of the embodiment: adding 10wt% aqueous solution of modified polyvinyl alcohol into 15wt% aqueous polyurethane solution to obtain mixed solution; adding a silane coupling agent, stirring to enable the pH value of the solution to be 7-9, adding a regulator when standing for 30 minutes, adding a leveling agent while stirring to enable the pH value of the solution to be 7-9, standing for 10 minutes, adding propylene glycol, stirring for 5 minutes, adding an adhesion promoter part and a nanometer aluminum oxide part, and promoting the adhesion of a coating to obtain the high-adhesion polymer coating liquid.
Referring to fig. 4 and 5, in summary of the foregoing embodiments, the present invention innovatively uses reverse coating in the coating process, i.e., the direction of the coating roll 10 and the substrate are different, and the generated shearing force does not generate stringing and droplet generation, so that the coating is relatively uniform. In the reverse coating, the configurationThe polymer coating liquid of (2) adopts a coating mode of combining a winding rod scraper 14 and a base film to carry out single-side or double-side coating, wherein the coating parameters are all 5-10g/m 2 Namely, a coating solution having a coating amount of 5-10g per square meter of the base film is coated, and then the coating solution is dried for 2-5s at a temperature of 80-110 ℃. The treated and coated base film 15 has strong adhesive force, good leveling property, good coating uniformity, strong oxidation resistance and can maintain excellent gas barrier property.
Film adhesion indicates how strongly the coating adheres to the substrate, which is a concern, and among the main factors affecting film adhesion, researchers have found that: the morphology of the film-substrate bonding interface has an important effect on the adhesion properties of the film, which involves various problems such as coating materials, surface conditions, process methods and parameters, and the interface formation process determined by the process. The adaptability of the coating liquid and the matrix material is influenced, and the precondition of obtaining good adhesive force is that the formula problem of the coating liquid is considered, firstly, the proportion of a coating liquid regulator is considered, secondly, the surface roughness of the base film is considered, electrostatic adsorption is carried out before coating, the surface of the base film has certain roughness, the friction coefficient mu s of the base film is kept between 0.30 and 0.41, and mu d is kept between 0.40 and 0.43, so that the deposition atoms of the coating liquid have enough mobility after coating, and the atoms of the film material can enter pores and gaps of the matrix to form an interface for embedding the coating. The surface of the film has compact matrix structure and smooth surface, and forms a clear and flat interface.
When the coating liquid enters the film substrate, the composition of the coating liquid molecules changes due to the influence of temperature, particularly in hot air drying. The adhesiveness between the coating and the base film is strong, but the coating time is also related to a certain extent, when the coating time t is less than or equal to 1min, the coating instantaneously enters the base film, and after the base film enters the drying, the adhesive force of the base film increases along with the increase of the hot air drying temperature (as shown in fig. 4). When the coating liquid and the film matrix have mutual solubility or partial mutual solubility, if the energy of 1-15eV is given to the atoms of the interface layer, the atoms can be mutually diffused through the interface. The interface layer formed by diffusion is favorable for forming firm combination between the film and the matrix, and can reduce the thermal stress caused by different linear expansion coefficients of the film and the matrix material. The molecules can be promoted to diffuse by the measures of heating the matrix, attracting the charged particles by an electric field, carrying out post-coating treatment and the like during coating. In the research, the technicians find that the high-hardness substances have larger surface free energy, and if two substances with similar structures form a film-based combination, larger attachment energy is obtained. The technical personnel carry out experiments for several times, and the adhesion promoter and the nano aluminum oxide are added into the coating liquid to ensure that the base film has very high adhesion, and meanwhile, the cleanliness of the base film is also a main factor in many factors influencing the adhesion under the same combination condition of coating liquid substances. In the operation of the base film, the surface of the base film can absorb a molecular layer of water or oil, if the molecular layer cannot be removed, the adhesive strength of the film is greatly reduced. In order to obtain the due adhesive force, corona treatment is carried out before winding, so that the base film reaches a certain roughness, and the surface roughness Rmax=0.210-0.50, so that the base film has more adhesive force in the processing of downstream enterprises.
According to the invention, through the given embodiments, only the specific application embodiments in the technical scheme are based, and the raw material options and the proportioning range and the related temperature, pressure, time and other parameter ranges listed in the technical scheme are based, other specific application embodiments can be derived without creative labor, and all the application embodiments belong to the protection scope of the invention.
Table 1 shows the experimental numbers of the thick brightness enhancement polyester base film prepared by the invention
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Claims (5)

1. The preparation method of the high-adhesiveness thick brightening polyester base film comprises the steps of raw material preparation, extrusion, longitudinal stretching, coating, drying and transverse stretching, and is characterized in that:
the raw material configuration comprises: the first extrusion raw material comprises 80-90 parts by weight of resin and 10-20 parts by weight of inorganic nano material; the second extrusion raw material comprises 70-90 parts by weight of resin, 5-20 parts by weight of inorganic nano material and 5-10 parts by weight of defoamer;
the extrusion comprises: after the first extrusion raw materials are mixed, the thickness of the extruded melt is 50-100um under the conditions that the temperature is 300-350 ℃ and the extrusion pressure is 2-10MPa by a first extruder; mixing the second extrusion raw materials, and extruding the mixture into a melt with the thickness of 60-150um by a second extruder under the conditions that the temperature is 290-340 ℃ and the extrusion pressure is 2-9 MPa; the first extruded melt and the second extruded melt are respectively filtered with the filtering precision of 10-25um and then are gathered into a two-layer co-extrusion system;
The longitudinal stretching is to pass the extruded polyester film through a preheating zone of 60-90 ℃, a stretching zone of 90-120 ℃ and a cooling zone of 30-60 ℃ to form a substrate film with a stretching multiple of 3.6-4.0;
the coating is to coat the uncoated substrate membrane to form a base membrane after electrostatic adsorption of the longitudinally stretched substrate membrane;
the drying is to carry out hot air drying on the coated base film, wherein the drying time is 2-10 s, and the temperature of hot air drying is set to be 80-145 ℃;
the transverse stretching is formed by coating and drying a base film, and then passing through a preheating section with the temperature of 100-130 ℃, a stretching section with the temperature of 130-160 ℃, a shaping section with the temperature of 260-280 ℃ and a cooling section with the temperature of 30-60 ℃ and controlling the stretching multiple to be 3.0-4.0;
the base film after transverse stretching is flattened and subjected to corona treatment, so that the surface roughness Rmax=0.210-0.50 of the base film is achieved, static electricity is eliminated, and the base film is rolled to obtain a polyester base film with a thickness of 180-260 mu m and a double-layer structure consisting of the base film and a coating layer;
the coating is to coat the coating on the surface of the substrate membrane in a shearing mode, and the coating liquid on the surface layer is controlled to be neat and uniform by a coating scraper;
the included angle alpha between the uncoated substrate film and the coating roller in the coating process is less than or equal to 80 ℃, the rotating direction of the coating roller is opposite to the running direction of the substrate film, the substrate film is coated on one side or both sides, and the coating parameters are all the same Is 5-10g/m 2 ；
The coating liquid components in the coating process comprise: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propylene glycol, 5-10 parts of flatting agent, 1-5 parts of silane coupling agent, 1-5 parts of regulator, 1-5 parts of adhesion promoter and 1-5 parts of nano aluminum oxide.
2. The method for preparing a high adhesion thick type brightening polyester base film according to claim 1, wherein: the resin is aromatic polyester; the inorganic nano material comprises silicon dioxide, aluminum oxide and barium sulfate 、 One or more of aluminum nitride; the defoaming agent comprises one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene alcohol amine ether, methyl silicone oil and ethyl silicone oil.
3. The method for preparing a high adhesion thick type brightening polyester base film according to claim 1, wherein: the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal and water-soluble polyvinyl alcohol; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organosiloxane, acrylic acid and polyether modified silicone oil; the silane coupling agent is one or more of a multifunctional silane coupling agent, a water-based silane coupling agent, an epoxy silane coupling agent and a protective silane coupling agent; the regulator comprises one or more of oleamide, a silicon dioxide opening agent, dodecanol and polyoxyethylene oleate; the adhesion promoter is one or more of phosphoric acid methacrylate, amino organosilicon polymer, PP adhesion treating agent, phosphate compound and organic metal ester chelate.
4. The method for producing a high adhesion thick type brightness enhancing polyester base film according to claim 3, wherein: the preparation of the coating liquid is to add 3-20wt% aqueous solution of modified polyvinyl alcohol into 10-20wt% aqueous polyurethane solution to obtain mixed solution; adding a silane coupling agent, stirring to enable the pH value of the solution to be 7-9, standing for 20-40 minutes, adding a regulator, stirring while adding a leveling agent, enabling the pH value of the solution to be 7-9, standing for 8-15 minutes, adding propylene glycol, stirring for 3-8 minutes, and adding an adhesion promoter and nano aluminum oxide to obtain the high-adhesion polymer coating liquid.
5. The method for preparing a high adhesion thick type brightening polyester base film according to claim 1, wherein: the two-layer co-extrusion system in the extrusion process adopts a composite membrane head, the melt of the first extruder and the melt of the second extruder enter the upper side of a membrane cavity of the composite membrane head, the melt is symmetrical by the center line of the membrane cavity, the co-extrusion temperature is controlled to be 350-370 ℃, the first material conveying pipeline in the first fine filter and the second material conveying pipeline in the second fine filter are converged and overlapped in the composite membrane head under the condition of 3-10Mpa, the overlapped surfaces flow in each layer of flow channel, the melt of the flow channel is extruded after reaching a membrane lip, and the polyester membrane is formed by cooling at 60-100 ℃.
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