CN114456422A - Preparation method of high-adhesion thick brightening polyester base film - Google Patents

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

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CN114456422A
CN114456422A CN202210229751.5A CN202210229751A CN114456422A CN 114456422 A CN114456422 A CN 114456422A CN 202210229751 A CN202210229751 A CN 202210229751A CN 114456422 A CN114456422 A CN 114456422A
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coating
base film
parts
adhesion
extrusion
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CN114456422B (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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    • 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
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    • 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
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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    • C08J2300/00—Characterised by the use of unspecified polymers
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    • 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
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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
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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
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    • 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
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    • 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
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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    • C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
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    • C08K3/20—Oxides; Hydroxides
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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-adhesion 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 an inorganic nano material defoaming agent; the extrusion comprises the mixed extrusion of a first extrusion raw material and the mixed extrusion of a second extrusion raw material, and melts of the first extrusion and the second extrusion are collected into a co-extrusion system after being filtered and longitudinally stretched; coating, namely coating the uncoated base material film to form a base film after electrostatic adsorption of the longitudinally stretched base material film; the drying is formed by drying the coated base film by hot air and then transversely stretching. The product is mainly a thick brightening base film product, has the thickness of within 180-.

Description

Preparation method of high-adhesion 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-adhesion 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 which aims at improving the luminous efficiency of the whole backlight system, and utilizes a special prism structure of the brightness enhancement film to concentrate light rays in all aspects to a central visual angle through refraction, total reflection, light accumulation and other optical principles, and realizes recycling of light which is not utilized outside the visual angle through reflection of the light, thereby reducing the loss of the light, simultaneously improving the whole luminance and uniformity, playing a role in increasing the luminance and controlling the visual angle for the display of an LCD panel, and further improving the luminance of the LCD panel and controlling the visual angle. The existing production of the base film usually comprises the processes of raw material configuration, extrusion, stretching, coating, drying and the like, because the set temperature of each section (a feeding section, a compression section and a metering section) of an extruder is too high or too low, sometimes an extrusion screw and a material are interwoven together to lock the screw, if the screw extruder is lack of a good protection device, a strong driving force is likely to twist off the screw, and the locking can generate extraordinary huge resistance, so that the surface of the screw is seriously damaged and a machine barrel is seriously scratched; secondly, in the coating process, the coating roller and the base film run at the same speed and in the same direction in the traditional coating process, so that the shearing force generated by the coating liquid can generate wire drawing and small liquid drops which are splashed on the base film again, and the appearance of the base film has defects; and thirdly, in the coating liquid formula, because nano particles such as a regulator and the like are not added in many enterprises or retrieval patents, the adhesion force of the coating and the base film is poor, and the coating layer falls off in the subsequent processing of the base film. Due to the defects in the process, poor adhesion sometimes occurs in the process of coating the base film for brightening, defects such as crystal points or air bubbles occur on the film surface, which results in insufficient brightness and definition, and the polyester base film has poor hardness, tension and stripping force performance. In view of the defects in the prior art, there is a need for improvement of the processes related to film adhesion and the like in the polyester-based film process.
Disclosure of Invention
The invention aims to technically overcome the defects in the prior art and provides a preparation method of a thick brightening polyester base film with high adhesion. The method uses the physical adsorption principle to pre-coat a layer of base film with stable orientation, draws the distance between the molecules of the coating liquid, and increases the wettability of the film, thereby increasing the adhesive force of the pre-coated film.
The technical scheme of the invention comprises the following steps:
a preparation method of a thick brightening polyester base film with high adhesion comprises the steps of raw material preparation, extrusion, longitudinal stretching, coating, drying and transverse stretching, wherein: the raw material preparation comprises the following steps: 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 defoaming agent;
the extruding comprises: after the first extrusion raw material is 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; after the second extrusion raw material is mixed, the thickness of the extruded melt is 60-150um under the conditions that the temperature is 290-340 ℃ and the extrusion pressure is 2-9MPa by a second extruder; filtering the first extruded melt and the second extruded melt with the filtering precision of 10-25um respectively and then converging the two layers of co-extrusion systems;
the longitudinal stretching is a base material membrane formed by controlling the stretching multiple to be 3.6-4.0 after the extruded polyester membrane passes through a preheating zone at 60-90 ℃, a stretching zone at 90-120 ℃ and a cooling zone at 30-60 ℃;
the coating is to coat the uncoated base material film after electrostatic adsorption of the longitudinally stretched base material film to form a base film;
the drying is to carry out hot air drying on the coated base film, wherein the drying time is 2-10s, and the temperature of the hot air drying is set to be 80-145 ℃;
the transverse stretching is formed by coating and drying a base film, and then passing the base film through a preheating section at the temperature of 100-130 ℃, a stretching section at the temperature of 130-160 ℃, a shaping section at the temperature of 260-280 ℃ and a cooling section at the temperature of 30-60 ℃, wherein the stretching multiple is controlled to be 3.0-4.0.
The preparation method of the high-adhesion thick brightening polyester base film further comprises the following steps: flattening the transversely stretched base film, carrying out corona treatment to ensure that the surface roughness Rmax of the base film is =0.210-0.50, eliminating static electricity, and rolling to prepare the polyester base film with the thickness of 180-.
The above technical solution further comprises:
the resin comprises one or more of polyethylene (EP), polyethylene terephthalate (PET), High Density Polyethylene (HDPE), Liquid Crystal Polymer (LCP) and aromatic polyester (ARP); the inorganic nanomaterial comprises silicon dioxide (SiO)2) Aluminum oxide (Ai)2O3) Barium sulfate (BaSO)4）、One or more of aluminum nitride (AlN);
the defoaming agent comprises one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene ether, methyl silicone oil, ethyl silicone oil and an 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.
Furthermore, the included angle alpha between the uncoated substrate diaphragm and the coating roller in the coating process is less than or equal to 80 ℃, the rotation direction of the coating roller is opposite to the running direction of the substrate diaphragm, the substrate diaphragm is coated on one side or two sides, and the coating parameters are 5-10g/m 2。
The coating liquid in the coating process comprises the following components: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propyl alcohol, 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 organic siloxane, acrylic acid, an organic silicon 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 methacrylic acid phosphate, amino organic silicon 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 coating liquid is prepared by adding 3 wt% -20 wt% of aqueous solution into 10 wt% -20 wt% 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, adding a leveling agent while stirring to enable the pH value of the solution to be 7-9, standing for 8-15 minutes, adding propyl alcohol, stirring for 3-8 minutes, adding an adhesion promoter and nano aluminum oxide, and obtaining the high-adhesion polymer coating liquid.
Furthermore, a composite membrane head is adopted in the two-layer co-extrusion system in the extrusion process, the melts of the first extruder and the second extruder enter the upper side of a membrane cavity of the composite membrane head, the melts are symmetrical along the central line of the membrane cavity, the co-extrusion temperature is controlled to be at 350-370 ℃ and the pressure is controlled to be 3-10Mpa, the first material conveying pipeline in the first fine filter and the second material conveying pipeline in the second fine filter are converged and superposed in the composite membrane head, the superposed surfaces flow in each layer of flow channel, the melts of the flow channels are extruded after arriving at a membrane lip, and the melts are cooled at 60-100 ℃ to form the polyester membrane.
Further, the uncoated substrate film after longitudinal stretching is subjected to electrostatic adsorption, and then the uncoated substrate film is coated.
The invention solves the problem of thick brightening base film adhesion, enhances the adhesion of materials by the molecular interaction between the coating and the base material and combines the materials in a cross-linking way, and ensures that the coating has good water resistance, strong adhesion, good leveling property, good glossiness, strong oxidation resistance, excellent gas barrier property and the like by the coating process after treatment. The product has been developed successfully and is adopted by industries such as flat-panel televisions, electronic equipment and the like, and a brighter, lighter and more power-saving solution is provided for the field of liquid crystal display. The thick brightening base film product prepared by the invention has the thickness of 180-. The invention adopts aqueous coating liquid on the coating material, and adds metal oxide nano particles, so that the product has higher hardness and good surface tension and adhesive force.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of a two-layer co-extrusion system according to the present invention;
FIG. 2 is a schematic diagram of a coating system according to an embodiment of 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 temperature and adhesion of the product according to the present invention;
FIG. 5 is a graph showing the relationship between coating time and adhesion of the product of the present invention.
Detailed Description
The technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
Example 1, a method for preparing a high-adhesion thick type brightened polyester base film, the product prepared by the method 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: average thickness 180-; surface roughness Rmax = 0.210-0.50.
Referring to fig. 1, the extrusion system according to the present invention includes a composite membrane head (also called a dual-layer co-extrusion system) 2, a first material delivery 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 delivery pipeline 8, wherein in the extrusion system, the first layer extruder 5 is connected to the first extruder fine filter 4, and is further connected to the composite membrane head 2 through the first material delivery pipeline 3; the second layer of 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 melt membranes enter the next process after the composite membrane head 2 is extruded to form 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 drawing roller 13, a coating blade 14, and a frame 16. In the coating system, a drawing roll 13, guide rolls 11 and a coating roll 10 are mounted on a frame 16, and a coating liquid tank 9 is provided directly below the coating roll 10 between the two guide rolls 11 and is a single entity, and the center of the coating liquid tank is vertically vertical to the center of the coating roll 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, guide roll 11, and applicator roll 10 are connected by an uncoated substrate 12 and a coated base film 15.
Referring to fig. 1-3, a method for preparing a high-adhesion thick brightening polyester-based film, wherein raw material configurations include resin, inorganic nano-materials and 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;
inorganic nano material is SiO2、Ai2O3、BaSO4、AlN (silicon dioxide, aluminum oxide, barium sulfate and aluminum nitride respectively);
the defoaming agent is one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene ether, methyl silicone oil, ethyl silicone oil and organic silicon defoaming agent.
The preparation method of the high-adhesion thick brightening polyester base film comprises the following steps:
firstly, raw materials are matched, and the raw material formula of a 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 defoaming agent.
The preparation steps are as follows:
step S1, the raw material of the first extruder is stirred and metered and then enters the first extruder 5, the raw material of the second extruder is stirred and metered and then enters the second extruder 6, the specification models of the two extruders are the same, but the temperature of the first extruder is set to be 300-350 ℃, and the extrusion pressure is 2-10 MPa; the temperature of the second extruder is set to be 290-340 ℃, and the extrusion pressure is 2-9 MPa; 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 60-150 um; the extruded melt respectively enters a first extruder fine filter 4 and a second extruder fine filter 7, the specification and the model of the two fine filters are the same, the filtering precision is 10-25um, moisture, oligomer and impurities in the raw materials are removed, and the two layers of co-extrusion systems (composite membrane heads) 2 are collected after filtering.
And step S2, enabling the melt to enter the inner cavity of the composite membrane head from the side of the composite membrane head 2, enabling the melt to be symmetrical about the central line of the membrane cavity, setting the temperature in the membrane head to be 350-370 ℃, setting the pressure to be 3-10Mpa, enabling the first material conveying pipeline 3 in the fine filter 4 of the first extruder and the second material conveying pipeline 8 in the fine filter 7 of the second extruder to be converged and overlapped in the composite membrane head, enabling the overlapped surfaces to flow in each layer of flow channel, enabling the melt in the flow channel to come to the membrane lip and then be extruded, and cooling at 60-100 ℃ to form the polyester membrane 1. The polyester film 1 thus formed is subjected to a longitudinal stretching process via a melt feed line.
Step S3, the longitudinal stretching system (also called longitudinal stretching system) comprises a plurality of rollers (20 rollers are selected in this embodiment) 1-8#The roller is a preheating zone with a temperature of 60-90 deg.C and a temperature of 8-16 deg.C#The roller is a stretching zone, and the temperature is set to 90-120 ℃ and 16-20 DEG C#The roller is a cooling zone, the temperature is set to be 30-60 ℃, and the stretching ratio is 3-4.
In step S4, after the longitudinal stretching, the uncoated base material film 12 is corona-adsorbed and then coated. Under the traction of a traction roller 13, an uncoated substrate film 12 passes through a guide rail 11 to the upper surface of a coating liquid groove, 1/10 of the diameter of a coating roller 10 is immersed into the liquid surface of the coating liquid groove, a contact point of the coating roller 10 and a base film forms an arc surface less than 90 degrees, and the included angle alpha between the substrate and the coating roller is preferably less than or equal to 80 degrees. The rotation direction of the coating roller 10 is opposite to the direction of the substrate, the coating is to coat the coating on the surface of the substrate in a cutting mode, a coating scraper 14 ensures that the surface layer coating liquid is neat and uniform, and the base film is coated on one side or two sides, wherein the coating parameters are 5-10g/m 2After coating, the base film 15 enters a hot air drying device through a guide roller 11 and a traction roller 13 for drying timeAnd 2-10s, and setting the temperature of hot air drying to be 80-145 ℃.
Step S5, drying and then entering a transverse stretching system (also called 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-.
And step S6, flattening the film by the transverse pulling system, carrying out corona treatment to ensure that the base film reaches certain roughness, the surface roughness Rmax =0.210-0.50, eliminating static electricity, and rolling to obtain the polyester base film with standard thickness (120-. Referring to fig. 3, a base film 17, and a coating layer 18.
Embodiment 2, a method for preparing a high-adhesion thick brightening polyester base film, the coating liquid formulation of which comprises the following components in parts by mass: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propyl alcohol, 5-10 parts of a flatting agent, 1-5 parts of a silane coupling agent, 1-5 parts of a regulator, 1-5 parts of an adhesion promoter and 1-5 parts of nano aluminum oxide.
Specifically, the regulator is one or more of oleamide, a silicon dioxide opening agent, lauryl alcohol and polyoxyethylene oleate.
Specifically, the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane, acrylic acid, an organic silicon 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 Jessica chemical Co., Ltd., Hangzhou), PP adhesion treating agent ( Sheng plastics science and technology Co., Ltd., Dongguan), adhesion enhancer LT-1736 (Ringtai new material Co., Ltd., Fushan), phosphate compound ADP-S479, organic metal ester chelate ADP-S478, and organic compound ADP-S481 (Nanjing Needde new material technology Co., Ltd.).
Specifically, the silane coupling agent is one or more of a multifunctional silane coupling agent (X-12-981S multifunctional silane coupling agent provided by chemical Co., Ltd. of architecture of Dongguan city), an aqueous silane coupling agent (ShinEtsu silicone oligomer provided by chemical Co., Ltd. of architecture of Dongguan city, Japan), an epoxy silane coupling agent (KBM-903, Nippon Xinyue), and a protective silane coupling agent (X-12-967C protective silane coupling agent provided by chemical Co., Ltd. of architecture of Dongguan city).
Specifically, the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (synthesized in Japan), and polyvinyl alcohol Z-200 (synthesized in Japan).
Specifically, a preparation method of the coating liquid based on the formula comprises the following steps: adding a 3-20 wt% aqueous solution of modified polyvinyl alcohol into a 10-20 wt% aqueous polyurethane solution to obtain 20-30 parts of a mixed solution; adding 2-5 parts of silane coupling agent, stirring to adjust the pH value of the solution to 7-9, adding 5 parts of regulator when standing for 30 minutes, adding 10 parts of flatting agent while stirring to adjust the pH value of the solution to 7-9, adding 20 parts of propyl alcohol after standing for 10 minutes, stirring for 5 minutes, adding 5 parts of adhesion promoter and 5 parts of nano aluminum oxide (the above parts are parts by weight), and promoting the adhesion of the coating to obtain the high-adhesion polymer coating liquid.
Example 3 this example provides a method for preparing a high adhesion, thick, brightened polyester base film, which is structurally two-ply, comprising 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 (refer to the attached figures 1 and 2) comprises a composite film head 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, a second material conveying pipeline 8, a coating liquid tank 9, a coating roller 10, a guide roller 11, a traction roller 13, a coating scraper 14 and a machine 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 material conveying pipeline 3; the second extruder 6 is connected with a second extruder fine filter 7 and is also 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 die head 2, and two layers of cast pieces 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, a traction roller 13, a guide roller 11 and a coating roller 10 are mounted on a frame 16, a coating liquid tank 9 is a separate entity below the frame 16 (below the coating roller 10), the center of the coating liquid tank is vertically 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 web is passed over a take-off roll 13, a guide roll 11, an applicator roll 10, over an uncoated substrate 12, and over a coated base film 15.
The high-adhesion thick brightening polyester-based film raw material of the embodiment mainly comprises resin, inorganic nano-materials and defoaming agents.
Specifically, the resin raw material is one or more of EP, PET, HDPE, LCP and ARP (respectively polyethylene, polyethylene terephthalate, high density polyethylene, liquid crystal polymer and aromatic polyester);
specifically, the inorganic nano material is SiO2、Ai2O3、BaSO4、AlN (silicon dioxide, aluminum oxide, barium sulfate and aluminum nitride respectively);
wherein, the technical indexes of the aluminum oxide are as follows: the appearance is white loose powder; crystal form, alpha phase; the content is more than or equal to 99.9 weight parts; particle size =30 um; technical indexes of aluminum nitride: the average crystal grain is 19.47nm, and the thermal conductivity is 320W/mk.
Specifically, the defoaming agent is one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene amine ether, methyl silicone oil, ethyl silicone oil and an organic silicon defoaming agent.
The raw material formula of the first extruder in this embodiment is 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 example 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: average thickness 180-; surface roughness Rmax = 0.210-0.50.
Specifically, the preparation method of the thick brightening polyester base film with high adhesion of the embodiment includes the following steps:
and step S1, operating a production line, feeding 80-90 parts by weight of resin and 10-20 parts by weight of inorganic nano material into a hopper of a first extruder according to the raw material formula, feeding the raw materials of the first extruder into a first extruder 5 after stirring and metering, and feeding 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 into a hopper of a second extruder according to the raw material formula. The raw materials of the second extruder are stirred and metered and then enter a second extruder 6, the specification models of the two extruders are the same, but the temperature of the first extruder is set to be 350 ℃ plus-300 ℃, the extrusion pressure is 2-10MPa, the temperature of the second extruder is set to be 290 ℃ plus-340 ℃, the extrusion pressure is 2-9MPa, the thickness of the melt extruded by the first extruder is 50-100um, and the thickness of the melt extruded by the second extruder is 60-150 um; the extruded melt respectively enters a first extruder fine filter 4 and a second extruder fine filter 7, the specifications and the models 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 filtered melt is collected in a co-extrusion system (composite membrane head) 2.
And step S2, enabling the melt to enter the inner cavity of the die head from the side of the composite film head 2, enabling the melt to be symmetrical about the central line of the film cavity, setting the temperature in the film head to be 350-370 ℃, and the pressure to be 3-10Mpa, enabling the melt of the first extruder pipeline 3 and the second extruder pipeline 8 to enter the upper side of the film cavity of the co-extrusion system 2, enabling the melt to flow in the superimposed surface of each layer of runner, and cooling the melt of the runner at 60-100 ℃ after the melt comes to the film lip to form the polyester film 1. The formed polyester film 1 is longitudinally stretched through a melt conveying pipeline.
Step S3, the longitudinal stretching system is composed of a plurality of rollers 1-8#The roller is a preheating zone with a temperature of 60-90 deg.C and a temperature of 8-16 deg.C#The roller is a stretching zone, and the temperature is set to 90-120 ℃ and 16-20 DEG C#The roller is a cooling zone, the temperature is set to be 30-60 ℃, and the stretching ratio is 3.0-4.0.
In step S4, referring to fig. 2, the film sheet 1 is stretched in the longitudinal direction and then molded into a base film, and electrostatic adsorption is required to adhere the coating liquid to the base film. Chinese patents CN201610400465.5, CN202120059639.2, CN202110030866.7, CN202110537649.7, CN202110905954.7, etc. all have the expression of electrostatic adsorption of thin film, and the dc voltage u generated by a high voltage generator is set to 2-4KV, and the dc voltage forms a strong electrostatic field in the electrostatic adsorption device, because the base film has good insulating property, positive ions cannot pass through the base film and accumulate on the surface of the film to form film charges, and because like charges repel each other, a repulsive force is formed between the two charges to increase the surface area of the film and bring static electricity.
Under the traction of a traction roller 13, an uncoated base material 12 enters the upper surface of a coating liquid groove 9 through a guide roller 11, 1/10 of the diameter of a coating roller 10 is immersed into the page of the coating groove, the contact point of the coating roller 10 and a base film forms a cambered surface, and the included angle alpha between the base material and the coating roller is less than or equal to 80 degrees. The rotation direction of the coating roller 10 is opposite to the direction of the substrate, the coating is to coat the coating on the surface of the substrate in a cutting mode, a coating scraper 14 ensures that the surface layer coating liquid is neat and uniform, and the base film is coated on one side or two sides, wherein the coating density parameters are 5-10g/m 2After coating, the 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 be 80-145 ℃.
Step S5, drying and then entering a transverse drawing system, wherein the transverse drawing system is divided into a preheating section, a drawing section, a shaping section and a cooling section, the temperature of the preheating section is 100-130 ℃, the temperature of the drawing section is 130-160 ℃, the temperature of the shaping section is 260-280 ℃, the temperature of the cooling section is 30-60 ℃, and the drawing multiple is 3.0-4.0.
Step S6, flattening the film by the horizontal drawing system, performing corona treatment (refer to patent numbers CN201610400465.5, CN202120059639.2, CN202110030866.7, CN202110537649.7, CN202110905954.7, etc.), making the base film reach a certain roughness, with surface roughness Rmax =0.210-0.50, eliminating static electricity, and rolling to obtain a polyester base film with standard thickness (180-. Referring to fig. 3, the base film 17 and the coating layer 18 are shown.
In particular, the coating technology of the embodiment is the technical key of the invention, and the coating liquid formula comprises the following components in mass percentage: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propyl alcohol, 5-10 parts of a flatting agent, 1-5 parts of a silane coupling agent, 1-5 parts of a regulator, 1-5 parts of an adhesion promoter and 1-5 parts of nano aluminum oxide.
Wherein, the regulator of the embodiment is one or more of oleamide, a silicon dioxide opening agent, dodecanol and oleic acid polyoxyethylene ester; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane, acrylic acid, an organic silicon leveling agent and polyether modified silicone oil; the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymer compound JSC-1062 (produced by Jessica chemical Co., Ltd., Hangzhou), PP adhesion treating agent ( plastic science and technology Co., Ltd., Dongguan), adhesion enhancer LT-1736 (Ringtai new material Co., Ltd., Fushan), phosphate compound ADP-S479, organic metal ester chelate ADP-S478 and organic compound ADP-S481 (Nanjing Needt new material technology Co., Ltd.); the silane coupling agent is one or more of a multifunctional silane coupling agent (X-12-981S multifunctional silane coupling agent provided by chemical Co., Ltd. of architecture of Dongguan city), an aqueous silane coupling agent (ShinEtsu believing organosilicon oligomer provided by chemical Co., Ltd. of architecture of Dongguan city), an epoxy silane coupling agent (KBM-903, Nippon believes), and a protective silane coupling agent (X-12-967C protective silane coupling agent provided by chemical Co., Ltd. of architecture of Dongguan city); the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (synthesized in Japan) and polyvinyl alcohol Z-200 (synthesized in Japan).
Specifically, the synthesis technique of the high-adhesion thick brightening polyester-based film coating liquid of the embodiment comprises the following steps: adding a 3 wt% aqueous solution of modified polyvinyl alcohol into a 10 wt% aqueous polyurethane solution to obtain 20 parts of a 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 propyl alcohol after standing for 10 minutes, stirring for 5 minutes, adding 1.5 parts of adhesion promoter and 1.5 parts of nano aluminum oxide to promote the adhesion of a coating, and obtaining the high-adhesion polymer coating liquid.
The high-adhesion thick brightening polyester base film coating technology of the embodiment comprises the following steps: the prepared coating liquid is poured into a coating liquid tank 9, an uncoated substrate 12 is fed onto the upper surface of the coating liquid tank 9 through a traction roller 13 and a guide roller 11, and the rotation direction of a coating roller 10 is opposite to the direction of the substrate. The coating is to apply the coating on the surface of the substrate in a shearing mode. The coating blade 14 makes the surface layer coating liquid neat and uniform without overflow. 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, a pressing roller is not arranged, the generated shearing force cannot generate wire drawing and small liquid drops, the coating is relatively uniform, the coating mode overcomes certain defect 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 coating roll 10 is 40-60 mm. In the coating process, a cambered surface is formed from a contact point of the coating roll 10 and the base film, and the included angle alpha between the base material and the coating roll is less than or equal to 60 degrees. In coating, it is most important to control the amount of coating, also referred to as the ratio of the running speed of the base film to the speed of the coating roll. The skilled person tests and determines: when the speed ratio is 40-60%, coating is started; when the speed ratio is = 95-120%, uniformly and regularly coating; when the speed ratio is = 130-210%, the coating weight is increased; when the speed ratio = 200% or more, the coating amount decreases, and an unstable phenomenon occurs.
Generally, at a ratio of 90 to 130%, the thickness or weight of coating can be effectively controlled and a uniform coating surface can be ensured. In actual conditions, the coating amount of the coating roll may vary within a range of ± 10%. Different coating weights can be obtained through a certain number of coating rollers with different linear numbers, a relatively economic effect is achieved, and the coating rollers are adjusted in combination with a transmission ratio, so that relatively continuous coating weights can be basically obtained.
Example 4, based on the above example 3, this example specifically includes the raw material ratio and parameter adjustment.
The preparation method of the thick brightening polyester base film with high adhesion provided by the embodiment comprises the following steps:
and step S1, operating a production line, feeding 90 parts by weight of resin and 20 parts by weight of inorganic nano-material into a hopper of a first extruder according to the raw material formula, feeding the raw materials of the first extruder into a first extruder 5 after stirring and metering, and feeding 90 parts by weight of resin, 20 parts by weight of inorganic nano-material and 10 parts by weight of defoaming agent into a hopper of a second extruder according to the raw material formula. The raw materials of the second extruder are stirred and metered and then enter a second extruder 6, the specification and the model of the two extruders are the same, but the temperature of the first extruder is set to be 350 ℃, the extrusion pressure is 2MPa, the temperature of the second extruder is set to be 340 ℃, the extrusion pressure is 3MPa, the thickness of the melt extruded by the first layer of extruder is 100um, and the thickness of the melt extruded by the second layer of extruder is 60 um; the extruded melt respectively enters a first extruder fine filter 4 and a second extruder fine filter 7, the specifications and the models 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 filtered melt is collected into a co-extrusion system (composite membrane head) 2.
And step S2, enabling the melt to enter the inner cavity of the die head from the side of the composite film head 2, enabling the melt to be symmetrical about the central line of the film cavity, setting the temperature in the film head to be 370 ℃, enabling the pressure to be 3Mpa, enabling the melts of the first extruder pipeline 3 and the second extruder pipeline 8 to enter the upper side of the film cavity of the co-extrusion system 2, enabling the melts to flow on the superimposed surface in each layer of runner, enabling the melts in the runners to enter the film lip and then cooling at 100 ℃ to form the polyester film 1. The formed polyester film 1 is longitudinally stretched through a melt conveying pipeline.
Step S3, the longitudinal stretching system is composed of a plurality of rollers 1-8#The roller is a preheating zone with a temperature of 90 deg.C and a temperature of 8-16 deg.C#The roller is a stretching zone, and the temperature is set at 120 ℃ and is 16-20 DEG C#The roll was a cooling zone, 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 base material 12 is fed onto the coating liquid tank 9 through the guide roll 11 under the traction of the traction roll 13, 1/10 of the diameter of the coating roll 10 is immersed into the coating tank page, and the contact point shape of the coating roll 10 and the base film isForming a cambered surface. The included angle alpha between the base material and the coating roller is less than or equal to 50 degrees. The rotation direction of the coating roller 10 is opposite to the direction of the substrate, the coating is to coat the coating on the surface of the substrate in a cutting mode, a coating scraper 14 ensures that the surface coating liquid is neat and uniform, and the base film is coated on one side or two sides, wherein the coating parameters are all 10g/m 2After coating, the base film 15 enters a hot air drying device through a guide roller and a traction roller, the drying time is 10s, and the temperature of hot air drying is set to be 145 ℃.
And step S5, drying and then entering a transverse drawing system, wherein the transverse drawing system is divided into a preheating section, a drawing section, a shaping section and a cooling section, the temperature of the preheating section is 130 ℃, the temperature of the drawing section is 160 ℃, the temperature of the shaping section is 280 ℃, the temperature of the cooling section is 60 ℃, and the drawing multiple is 4.0.
And step S6, flattening the film by the transverse pulling system, carrying out corona treatment to ensure that the base film reaches certain roughness, the surface roughness Rmax =0.210-0.50, eliminating static electricity, and rolling to obtain the polyester base film with standard thickness (180-. Referring to fig. 3, the base film 17 and the coating layer 18 are shown.
Specifically, the coating technology of this embodiment is the technical key of the present invention, and the coating liquid formulation thereof comprises the following components by mass: 20 parts of modified polyvinyl alcohol, 15 parts of waterborne polyurethane, 10 parts of propyl alcohol, 5 parts of a leveling agent, 1 part of a silane coupling agent, 1 part of a regulator, 1.5 parts of an adhesion promoter and 1.5 parts of nano aluminum oxide.
Wherein, the regulator of the embodiment is one or more of oleamide, a silicon dioxide opening agent, dodecanol and oleic acid polyoxyethylene ester; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane, acrylic acid, an organic silicon leveling agent and polyether modified silicone oil; the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymer compound JSC-1062 (produced by Jessica chemical Co., Ltd., Hangzhou), PP adhesion treating agent ( plastic science and technology Co., Ltd., Dongguan), adhesion enhancer LT-1736 (Ringtai new material Co., Ltd., Fushan), phosphate compound ADP-S479, organic metal ester chelate ADP-S478 and organic compound ADP-S481 (Nanjing Needt new material technology Co., Ltd.); 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 modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (synthesized in Japan) and polyvinyl alcohol Z-200 (synthesized in Japan).
The synthesis technology of the high-adhesion thick brightening polyester base film coating liquid of the embodiment: adding 3-20 wt% of modified polyvinyl alcohol aqueous solution into 10-20 wt% 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, 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, adding propylene alcohol after standing for 10 minutes, stirring for 5 minutes, adding an adhesion promoter part and a nano aluminum oxide part to promote the adhesion of a coating, and obtaining the high-adhesion polymer coating liquid.
Example 5, based on the above example 3, this example specifically relates to the adjustment of the raw material ratio and the parameters.
The preparation method of the thick brightening polyester base film with high adhesion provided by the embodiment comprises the following steps:
and step S1, operating a production line, feeding 85 parts by weight of resin and 24.5 parts by weight of inorganic nano-material into a hopper of a first extruder according to the formula of the raw materials, and feeding the raw materials of the first extruder into the first extruder 5 after stirring and metering. The raw materials comprise 86 parts by weight of resin, 15.5 parts by weight of inorganic nano material and 8 parts by weight of defoaming agent which enter a hopper of a second extruder. The raw materials of the second extruder are stirred and metered and then enter a second extruder 6, the specification and the model of the two extruders are the same, but the temperature of the first extruder is set to be 330 ℃, the extrusion pressure is 7 MPa, the temperature of the second extruder is set to be 325 ℃, the extrusion pressure is 4.5MPa, the thickness of the melt extruded by the first extruder is 70 um, and the thickness of the melt extruded by the second extruder is 65 um; the extruded melt respectively enters a first fine filter 4 and a second fine filter 7, the specifications and the models of the two fine filters are the same, the filtering precision is 20um, the purpose is to remove moisture, oligomer and impurities in the raw materials below 20um, and the filtered melt is collected into a co-extrusion system (composite membrane head) 2.
And step S2, enabling the melt to enter the inner cavity of the die head from the side of the composite film head 2, enabling the melt to be symmetrical about the central line of the film cavity, setting the temperature in the film head to be 350 ℃, setting the pressure to be 5Mpa, enabling the melts of the first extruder pipeline 3 and the second extruder pipeline 8 to enter the upper side of the film cavity of the co-extrusion system 2, enabling the melts to flow on the superimposed surface in each layer of runner, and cooling the melts in the runners at 80 ℃ after the melts come to the film lips to form the polyester film 1. The formed polyester film 1 is longitudinally stretched through a melt conveying pipeline.
Step S3, the longitudinal stretching system is composed of a plurality of rollers 1-8#The roller is a preheating zone with a temperature of 85 deg.C and a temperature of 8-16 deg.C#The roller is a stretching zone, the temperature is set at 110 ℃ and is 16-20 DEG C#The roll was a cooling zone, 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.
Under the traction of a traction roller 13, an uncoated base material 12 enters the upper surface of a coating liquid groove 9 through a guide roller 11, 1/10 with the diameter of a coating roller 10 is immersed into the liquid surface of the coating liquid groove, and the contact point of the coating roller 10 and a base film forms a cambered surface. The included angle alpha between the base material and the coating roller is less than or equal to 75 degrees. The rotation direction of the coating roller 10 is opposite to the direction of the substrate, the coating is to coat the coating on the surface of the substrate in a cutting mode, a coating scraper 14 ensures that the surface coating liquid is neat and uniform, and the base film is coated on one side or two sides, wherein the coating parameters are 8.5g/m 2After coating, the base film 15 enters a hot air drying device through a guide roller and a traction roller, the drying time is 10s, and the temperature of hot air drying is set to be 125 ℃.
And step S5, drying and then entering a transverse drawing system, wherein the transverse drawing system is divided into a preheating section, a drawing section, a shaping section and a cooling section, the temperature of the preheating section is 110 ℃, the temperature of the drawing section is 140 ℃, the temperature of the shaping section is 260 ℃, the temperature of the cooling section is 50 ℃, and the drawing multiple is 4.0.
And step S6, flattening the film by the transverse pulling system, carrying out corona treatment to ensure that the base film reaches certain roughness, the surface roughness Rmax =0.210-0.50, eliminating static electricity, and rolling to obtain the polyester base film with standard thickness (180-. Referring to fig. 3, the base film 17 and the coating layer 18 are shown.
Specifically, the coating liquid formulation of the present example comprises the following components by mass: 25 parts of modified polyvinyl alcohol, 18 parts of waterborne polyurethane, 15 parts of propyl alcohol, 8 parts of a leveling agent, 3 parts of a silane coupling agent, 3 parts of a regulator, 3.5 parts of an adhesion promoter and 2.5 parts of nano aluminum oxide.
Wherein, the regulator of the embodiment is one or more of oleamide, a silicon dioxide opening agent, dodecanol and oleic acid polyoxyethylene ester; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane, acrylic acid, an organic silicon leveling agent and polyether modified silicone oil; the adhesion promoter is one or more of methacrylic acid phosphate, amino organosilicon polymer compound JSC-1062 (produced by Jessica chemical Co., Ltd., Hangzhou), PP adhesion treating agent ( plastic science and technology Co., Ltd., Dongguan), adhesion enhancer LT-1736 (Ringtai new material Co., Ltd., Fushan), phosphate compound ADP-S479, organic metal ester chelate ADP-S478 and organic compound ADP-S481 (Nanjing Needt new material technology Co., Ltd.); 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 modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water soluble polyvinyl alcohol, polyvinyl alcohol Z-200H (synthesized in Japan) and polyvinyl alcohol Z-200 (synthesized in Japan).
The synthesis technology of the high-adhesion thick brightening polyester base film coating liquid of the embodiment: adding 10 wt% of modified polyvinyl alcohol aqueous solution into 15 wt% 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, 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, adding propylene alcohol after standing for 10 minutes, stirring for 5 minutes, adding an adhesion promoter part and a nano aluminum oxide part to promote the adhesion of a coating, and obtaining the high-adhesion polymer coating liquid.
The foregoing embodiments are summarized with reference to FIGS. 4 and 5The invention creatively uses reverse coating in the coating process, namely the directions of the coating roller 10 and the substrate are different, the generated shearing force does not generate wire drawing and small liquid drops, and the coating is more uniform. In reverse coating, the prepared polymer coating liquid adopts a coating mode of combining a winding bar scraper 14, and the base film is coated on one side or two sides, wherein the coating parameters are 5-10g/m 2I.e. coating 5-10g of coating liquid on each square meter of base film, drying the coating liquid for 2-5s, and setting the temperature of hot air drying at 80-110 ℃. The treated and coated base film 15 has strong adhesive force, good leveling property, good coating uniformity and strong oxidation resistance, and can keep excellent gas barrier property.
The adhesion of the thin film indicates how strong the coating adheres to the substrate, which concerns the problem of adhesion of the coating, and among the main factors affecting the adhesion of the thin film, researchers found that: the morphology of the film-substrate bonding interface has a significant influence on the adhesion performance of the film, which involves problems such as coating materials, surface conditions, process methods and process parameters, and interface formation determined thereby. The method has the advantages that the adaptability of the coating liquid and the base material is influenced as a precondition for obtaining good adhesive force, the problem of the formula 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 coating liquid deposited atoms after coating have enough mobility, and the film material atoms can enter into small holes and gaps of the base body to form a coating layer mosaic interface. In appearance, the matrix structure on the surface of the film is compact, the surface is smooth, and a clear and flat interface is formed.
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 of the coating and the base film is strong, but has a certain relation with the coating time, when the coating time t is less than or equal to 1min, the coating instantly enters the base film, and after the base film is dried, the adhesive force of the base film is increased along with the increase of the hot air drying temperature (as shown in figure 4). When the coating solution and the film substrate have mutual solubility or partial mutual solubility, atoms can diffuse into each other through the interface by giving energy of 1-15eV to the atoms at the interface layer. The interface layer formed by diffusion is beneficial to forming firm combination between the film and the substrate, and can reduce the thermal stress caused by different coefficients of linear expansion between the film and the substrate. Molecular diffusion can be promoted by heating the substrate during coating, electric field attraction of energetic particles, post-coating treatment, and the like. In the research, the skilled person finds that the high hardness substance mostly has larger surface free energy, and if the substances with similar structures are combined to form a film base, the larger adhesion energy is obtained. After a plurality of experiments, technicians add the adhesion promoter and the nano-alumina into the coating liquid to enable the base film to have high adhesion, and meanwhile, under the same condition of combination of coating liquid substances, the cleanliness of the base film is also a main factor in a plurality of factors influencing the adhesion. During the operation of the base film, the surface of the base film can absorb a molecular layer of water or oil, and the molecular layer can not be removed, so that the adhesion strength of the film is greatly reduced. In order to obtain the proper adhesive force, corona treatment is carried out before rolling to ensure that the base film achieves certain roughness, wherein the surface roughness Rmax =0.210-0.50, so that downstream enterprises can ensure that the base film has more adhesive force in the processing.
According to the invention, the given embodiments are only based on a plurality of specific application embodiments in the technical scheme of the invention, and other specific application embodiments can be derived without creative labor based on the raw material options and the proportioning range listed in the technical scheme of the invention and the parameter ranges of relevant temperature, pressure, time and the like, and the embodiments belong to the protection scope of the invention.
Table 1 shows the number of experiments related to the thick brightening polyester-based film prepared by the invention
Figure 227749DEST_PATH_IMAGE001

Claims (10)

1. A preparation method of a thick brightening polyester base film with high adhesion comprises the steps of raw material preparation, extrusion, longitudinal stretching, coating, drying and transverse stretching, and is characterized in that:
the raw material preparation comprises the following steps: 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 defoaming agent;
the extruding comprises: after the first extrusion raw material is 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; after the second extrusion raw material is mixed, the thickness of the extruded melt is 60-150um under the conditions that the temperature is 290-340 ℃ and the extrusion pressure is 2-9MPa by a second extruder; filtering the first extruded melt and the second extruded melt with the filtering precision of 10-25um respectively and then converging the two layers of co-extrusion systems;
the longitudinal stretching is a base material membrane formed by controlling the stretching multiple to be 3.6-4.0 after the extruded polyester membrane passes through a preheating zone at 60-90 ℃, a stretching zone at 90-120 ℃ and a cooling zone at 30-60 ℃;
the coating is to coat the uncoated base material film after electrostatic adsorption of the longitudinally stretched base material film to form a base film;
the drying is to carry out hot air drying on the coated base film, wherein the drying time is 2-10s, and the temperature of the hot air drying is set to be 80-145 ℃;
the transverse stretching is formed by coating and drying a base film, and then passing the base film through a preheating section at the temperature of 100-130 ℃, a stretching section at the temperature of 130-160 ℃, a shaping section at the temperature of 260-280 ℃ and a cooling section at the temperature of 30-60 ℃, wherein the stretching multiple is controlled to be 3.0-4.0.
2. The method for preparing the high-adhesion thick brightening polyester base film according to claim 1, is characterized in that: flattening the transversely stretched base film, performing corona treatment to ensure that the surface roughness Rmax of the base film is =0.210-0.50, eliminating static electricity, and rolling to prepare the polyester base film with the thickness of 180-.
3. The method for preparing the high-adhesion thick brightening polyester base film according to claim 1 or 2, is characterized in that: the resin comprises one or more of polyethylene, polyethylene terephthalate, high-density polyethylene, liquid crystal polymer and 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 ether, methyl silicone oil, ethyl silicone oil and an organic silicon defoaming agent.
4. The method for preparing the high-adhesion thick brightening polyester base film according to claim 1 or 2, is characterized in that: the coating is to coat the coating on the surface of the substrate film in a shearing mode, and the surface layer coating liquid is controlled to be neat and uniform by a coating scraper.
5. The method for preparing the high-adhesion thick brightening polyester base film according to claim 4, is characterized in that: in the coating process, the included angle alpha between the uncoated substrate diaphragm and the coating roller is less than or equal to 80 ℃, the rotation direction of the coating roller is opposite to the running direction of the substrate diaphragm, the substrate diaphragm is coated on one side or two sides, and the coating parameters are 5-10g/m 2。
6. The method for preparing the high-adhesion thick brightening polyester base film according to claim 1 or 2, is characterized in that: the coating liquid in the coating process comprises the following components: 20-30 parts of modified polyvinyl alcohol, 15-20 parts of waterborne polyurethane, 10-20 parts of propyl alcohol, 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.
7. The method for preparing the high-adhesion thick brightening polyester base film according to claim 6, is characterized in that: the modified polyvinyl alcohol is one or more of instant polyvinyl alcohol, polyvinyl acetal, water-soluble polyvinyl alcohol and polyvinyl alcohol; the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane, acrylic acid, an organic silicon 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 methacrylic acid phosphate, amino organic silicon polymer, PP adhesion treating agent, adhesion enhancer, phosphate compound, organic metal ester chelate and organic compound.
8. The method for preparing the high-adhesion thick brightening polyester base film according to claim 7, characterized in that: the coating liquid is prepared by adding 3-20 wt% of aqueous solution into 10-20 wt% 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, adding a leveling agent while stirring to enable the pH value of the solution to be 7-9, standing for 8-15 minutes, adding propyl alcohol, stirring for 3-8 minutes, adding an adhesion promoter and nano aluminum oxide, and obtaining the high-adhesion polymer coating liquid.
9. The method for preparing the high-adhesion thick brightening polyester base film according to claim 1 or 2, is characterized in that: the two-layer co-extrusion system in the extrusion process adopts a composite membrane head, melts of a first extruder and a second extruder enter the upper side of a membrane cavity of the composite membrane head, the melts are symmetrical by the central line of the membrane cavity, the co-extrusion temperature is controlled to be at 350-370 ℃ and the pressure is 3-10Mpa, a first material conveying pipeline in a first fine filter and a second material conveying pipeline in a second fine filter are converged and superposed in the composite membrane head, the superposed surface flows in each layer of flow channel, the melts of the flow channels come to a membrane lip and then are extruded, and the melts are cooled at 60-100 ℃ to form the polyester membrane.
10. The method for preparing the high-adhesion thick brightening polyester base film according to claim 1 or 2, is characterized in that: and the uncoated substrate film after longitudinal stretching is subjected to electrostatic adsorption, and then is coated.
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