CN111116954A - Preparation method of film with high-light-transmittance frosted coating - Google Patents

Preparation method of film with high-light-transmittance frosted coating Download PDF

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Publication number
CN111116954A
CN111116954A CN201911297420.XA CN201911297420A CN111116954A CN 111116954 A CN111116954 A CN 111116954A CN 201911297420 A CN201911297420 A CN 201911297420A CN 111116954 A CN111116954 A CN 111116954A
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frosted
coating
film
preparing
particles
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陈琪
魏涛
金鑫
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Suzhou Humbert Electronic Technology Co ltd
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Suzhou Humbert Electronic Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/28Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for wrinkle, crackle, orange-peel, or similar decorative effects
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2435/00Characterised 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 a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
    • C08J2435/02Characterised by the use of homopolymers or copolymers of esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00Characterised by the use of epoxy resins; Derivatives of epoxy resins

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a preparation method of a film with a high-light-transmittance frosted coating, wherein the frosted coating comprises frosted coating resin mixed with frosted powder particles and coated on a PET film; the preparation steps are as follows: preparing the frosted particles: preparing frosted particles by adopting 5-15% of MMA, 0.1-0.3% of AIBN, 0.01-0.1% of EGDMA, 25-40% of ETOH and 40-60% of water, and 2, preparing frosted glue: mixing 3-15% of resin, 70-90% of solvent, 1-10% of frosting powder and 0.05-2% of curing agent at normal temperature to obtain frosting glue; 3. drying the frosted coating obtained by coating through a drying tunnel to obtain a film with the frosted coating with high light transmittance, and rolling. The preparation method disclosed by the invention is simple in preparation steps and easy to operate, and the film obtained by coating the frosted glue prepared by the method on a PET film and drying the PET film has a frosted effect and also ensures high light transmittance of the film, wherein the light transmittance of the obtained film is more than 88%, the haze is more than 0.8%, and the roughness RA value is 0.2-5 um.

Description

Preparation method of film with high-light-transmittance frosted coating
Technical Field
The invention relates to preparation of a frosted coating, in particular to a preparation method of a film with a frosted coating with high light transmittance.
Background
Transparent PET films have high light transmittance, but when the film is frosted, for example: the light transmittance of the film can be greatly reduced by treatments such as sand blasting, frosting and coating.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method capable of preparing a high-light-transmittance frosted coating.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention relates to a preparation method of a film with a high-light-transmittance frosted coating, which is characterized by comprising the following steps: the frosted coating comprises frosted coating resin mixed with frosted powder particles and coated on the PET film; the preparation steps are as follows:
(1) preparing the frosted particles: a, uniformly stirring 5 to 15 percent of MMA, 0.1 to 0.3 percent of AIBN, 0.01 to 0.1 percent of EGDMA, 25 to 40 percent of ETOH and 40 to 60 percent of water in a sealed reaction kettle according to the proportion;
b, introducing nitrogen into the reaction kettle for 20min, exhausting air in the reaction kettle, starting stirring at 50rpm/min, starting heating, heating to 60-70 ℃, and continuously reacting for 3 hours to obtain liquid containing particles;
c, filtering the liquid by a filter membrane, washing the particles obtained by filtering, filtering again, and drying for 1 hour at the temperature of 80-100 ℃ to obtain the ground particles for later use;
(2) preparing frosted glue: adding 3-15% of resin, 70-90% of solvent, 1-10% of frosting powder and 0.05-2% of curing agent into a reaction kettle, mixing at normal temperature to obtain frosted glue, stirring for 30min, wherein the stirring speed is 600 plus materials and is 100 rpm/min;
(3) coating to obtain a frosted coating: adding the frosted glue obtained in the step (2) into a coating trough, and coating the glue on a film through anilox rollers, micro-concave rollers or scrapers with different meshes to obtain a frosted coating, wherein the thickness of the coated dry glue is 5-100 um;
(4) and (3) passing the coated film through a drying tunnel, wherein the drying tunnel temperature is 100-150 ℃, the drying tunnel length is 30m, the speed of passing through the drying tunnel is 10-16m/min, the solvent is volatilized, and the film is wound after being cured.
The invention is further improved in that: the frosted powder with different grain diameters is prepared by adjusting the proportion of the raw materials in the step (1), and the microspheres with the grain diameters of 1um to 50um can be prepared.
The invention is further improved in that: the resin in the step (2) is obtained by mixing one or two or more of epoxy resins E20, E44 and E51.
The invention is further improved in that: the solvent in the step (2) is one of ethanol, ethyl acetate and toluene.
The invention is further improved in that: the frosting powder in the step (2) is obtained by mixing one, two or more of frosting particles with the particle size of 1-50 um.
The invention is further improved in that: the curing agent in the step (2) is one of diethylenetriamine, diaminodiphenylmethane and diaminodiphenylsulfone.
The invention has the beneficial effects that: the introduction amount of nitrogen is adjusted according to the size of a reaction kettle when the frosted particles are prepared, the frosted particles with different particle sizes can be prepared by changing the proportion of raw materials for preparing the frosted particles, a film obtained by coating the frosted glue prepared by the method on a PET film and drying has a frosting effect, and simultaneously the high light transmittance of the film is ensured, the light transmittance of the obtained film is more than 88%, the haze is more than 0.8%, and the roughness RA value is 0.2-5 um.
Drawings
Fig. 1 is a film having high light transmittance, which is prepared by the present invention.
Wherein: 1-film, 2-coating.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
As shown in fig. 1, the present invention is a method for preparing a film having a high light transmittance frosted coating layer comprising a frosted coating resin mixed with frosted powder particles coated on a PET film; the preparation steps are as follows:
(1) preparing the frosted particles: a, uniformly stirring 5 to 15 percent of MMA, 0.1 to 0.3 percent of AIBN, 0.01 to 0.1 percent of EGDMA, 25 to 40 percent of ETOH and 40 to 60 percent of water in a sealed reaction kettle according to the proportion;
b, introducing nitrogen into the reaction kettle for 20min, exhausting air in the reaction kettle, starting stirring at 50rpm/min, starting heating, heating to 60-70 ℃, and continuously reacting for 3 hours to obtain liquid containing particles;
c, filtering the liquid by a filter membrane, washing the particles obtained by filtering, filtering again, and drying for 1 hour at the temperature of 80-100 ℃ to obtain the ground particles for later use;
b, preparing the frosted powder with different particle sizes by adjusting the proportion of the raw materials in the step a, and preparing microspheres with particle sizes of 1um to 50um, wherein in the step c, filter membranes with corresponding pore sizes are selected according to the particle sizes of the particles to filter the particles;
(2) preparing frosted glue: adding 3-15% of resin, 70-90% of solvent, 1-10% of frosting powder and 0.05-2% of curing agent into a reaction kettle, mixing at normal temperature to obtain frosted glue, stirring for 30min, wherein the stirring speed is 600 plus materials and is 100 rpm/min;
(3) coating to obtain a frosted coating: adding the frosted glue obtained in the step (2) into a coating trough, and coating the glue on a film through anilox rollers or micro-concave rollers with different meshes to obtain a frosted coating, wherein the coating thickness is 5-100 um;
(4) and (3) passing the coated film through a drying tunnel, wherein the drying tunnel temperature is 100-150 ℃, the drying tunnel length is 20-30m, the speed of passing through the drying tunnel is 10-20m/min, the solvent is volatilized, and the film is wound after being cured.
The resin in the step (2) is obtained by mixing one or two or more of epoxy resins E20, E44 and E51. The solvent is one of ethanol, ethyl acetate and toluene, the frosted powder is obtained by mixing one, two or more of frosted particles with the particle size of 1-50 um, and the curing agent is one of diethylenetriamine, diaminodiphenylmethane and diaminodiphenyl sulfone.
Example 1
1) Preparing the frosted particles: a, uniformly stirring 15% of MMA, 0.27% of AIBN, 0.09% of EGDMA, 35% of ETOH and 49.64% of water in a sealed reaction kettle according to the proportion;
b, introducing nitrogen into the reaction kettle for 20min, exhausting air in the reaction kettle, starting stirring at 50rpm/min, starting heating, heating to 65 ℃, and continuously reacting for 3 hours to obtain liquid containing particles;
c, filtering the liquid by a filter membrane, washing the particles obtained by filtering, filtering again, and drying for 1 hour at the drying temperature of 100 ℃ to obtain the ground particles with the particle size of 2-3 um for later use;
the aperture of the filter membrane in the step c is 2 um;
(2) preparing frosted glue: adding 7% of epoxy resin E44, 87.3% of ethyl acetate, 5% of frosted powder and 0.7% of diethylenetriamine into a reaction kettle, and mixing at normal temperature to obtain frosted glue, wherein the stirring speed is 100rpm/min, and the stirring time is 30 min;
(3) coating to obtain a frosted coating: adding the frosted glue obtained in the step (2) into a coating trough, and coating the glue on a film through a micro-concave roller with the number of 100 meshes to obtain a frosted coating, wherein the coating thickness is 5-100 um;
(4) and (3) passing the coated film through a drying tunnel, wherein the drying tunnel temperature is 150 ℃, the drying tunnel length is 30m, and the drying tunnel speed is 20m/min to volatilize the solvent and carry out winding after curing. The film obtained had a light transmittance of 88.5%, a haze of 0.8% and a roughness RA value of 0.3 um.
Example 2
1) Preparing the frosted particles: a, uniformly stirring 9 percent of MMA, 0.2 percent of AIBN, 0.05 percent of EGDMA, 40 percent of ETOH and 50.75 percent of water in a sealed reaction kettle according to the proportion;
b, introducing nitrogen into the reaction kettle for 20min, exhausting air in the reaction kettle, starting stirring at 50rpm/min, starting heating, heating to 65 ℃, and continuously reacting for 3 hours to obtain liquid containing particles;
c, filtering the liquid by a filter membrane, washing the particles obtained by filtering, filtering again, and drying for 1 hour at the drying temperature of 100 ℃ to obtain the frosted particles with the particle size of 10-12 um for later use;
the aperture of the filter membrane in the step c is 10 um;
(2) preparing frosted glue: adding 14% of epoxy resin E51, 78% of ethyl acetate, 7% of frosted powder and 1% of diaminodiphenylmethane into a reaction kettle, and mixing at normal temperature to obtain frosted glue, wherein the stirring speed is 100rpm/min, and the stirring time is 30 min;
(3) coating to obtain a frosted coating: adding the frosted glue obtained in the step (2) into a coating trough, and coating the glue on a film through a micro-concave roller with the number of 100 meshes to obtain a frosted coating, wherein the coating thickness is 5-100 um;
(4) and (3) passing the coated film through a drying tunnel, wherein the drying tunnel temperature is 150 ℃, the drying tunnel length is 30m, and the solvent is volatilized and solidified at the drying tunnel speed of 16m/min and then is wound. The film had a light transmittance of 89%, a haze of 1.0%, and a roughness RA value of 1.5 μm.
Example 3
1) Preparing the frosted particles: a, uniformly stirring 10 percent of MMA, 0.1 percent of AIBN, 0.01 percent of EGDMA, 40 percent of ETOH and 49.89 percent of water in a sealed reaction kettle according to the proportion;
b, introducing nitrogen into the reaction kettle for 20min, exhausting air in the reaction kettle, starting stirring at 50rpm/min, starting heating, heating to 65 ℃, and continuously reacting for 3 hours to obtain liquid containing particles;
c, filtering the liquid by a filter membrane, washing the particles obtained by filtering, filtering again, and drying for 1 hour at the drying temperature of 100 ℃ to obtain the frosted particles with the particle size of 40um for later use;
the aperture of the filter membrane in the step c is 40 um;
(2) preparing frosted glue: adding 15% of epoxy resin E20, 76% of ethyl acetate, 10% of frosted powder and 1% of diethylenetriamine into a reaction kettle, and mixing at normal temperature to obtain frosted glue, wherein the stirring speed is 100rpm/min, and the stirring time is 30 min;
(3) coating to obtain a frosted coating: adding the frosted glue obtained in the step (2) into a coating trough, and coating the glue on a film through a micro-concave roller with the number of 100 meshes to obtain a frosted coating, wherein the coating thickness is 5-100 um;
(4) and (3) passing the coated film through a drying tunnel, wherein the drying tunnel temperature is 150 ℃, the drying tunnel length is 30m, and the drying tunnel speed is 10m/min to volatilize the solvent and carry out winding after curing. The film had a light transmittance of 89%, a haze of 1.2%, and a roughness RA value of 3.8 μm.

Claims (6)

1. A preparation method of a film with a high-light-transmittance frosted coating is characterized by comprising the following steps: the frosted coating comprises frosted coating resin mixed with frosted powder particles and coated on the PET film; the preparation steps are as follows:
(1) preparing the frosted particles: a, uniformly stirring 5 to 15 percent of MMA, 0.1 to 0.3 percent of AIBN, 0.01 to 0.1 percent of EGDMA, 25 to 40 percent of ETOH and 40 to 60 percent of water in a sealed reaction kettle according to the proportion;
b, introducing nitrogen into the reaction kettle for 20min, exhausting air in the reaction kettle, starting stirring at 50rpm/min, starting heating, heating to 60-70 ℃, and continuously reacting for 3 hours to obtain liquid containing particles;
c, filtering the liquid by a filter membrane, washing the particles obtained by filtering, filtering again, and drying for 1 hour at the temperature of 80-100 ℃ to obtain the ground particles for later use;
(2) preparing frosted glue: adding 3-15% of resin, 70-90% of solvent, 1-10% of frosting powder and 0.05-2% of curing agent into a reaction kettle, mixing at normal temperature to obtain frosted glue, stirring for 30min, wherein the stirring speed is 600 plus materials and is 100 rpm/min;
(3) coating to obtain a frosted coating: adding the frosted glue obtained in the step (2) into a coating trough, and coating the glue on a film through anilox rollers, micro-concave rollers or scrapers with different meshes to obtain a frosted coating, wherein the thickness of the coated dry glue is 5-100 um;
(4) and (3) passing the coated film through a drying tunnel, wherein the drying tunnel temperature is 100-150 ℃, the drying tunnel length is 20-30m, the speed of passing through the drying tunnel is 10-20m/min, the solvent is volatilized, and the film is wound after being cured.
2. The method for preparing a high light transmittance frosted coating according to claim 1, wherein: the frosted powder with different grain diameters is prepared by adjusting the proportion of the raw materials in the step (1), and the microspheres with the grain diameters of 1um to 50um can be prepared.
3. The method for preparing a high light transmittance frosted coating according to claim 2, wherein: the resin in the step (2) is obtained by mixing one or two or more of epoxy resins E20, E44 and E51.
4. The method for preparing a high light transmittance frosted coating according to claim 3, wherein: the solvent in the step (2) is one of ethanol, ethyl acetate and toluene.
5. The method for preparing a high light transmittance frosted coating according to claim 4, wherein: the frosted powder in the step (2) is obtained by mixing one, two or more of frosted particles with the particle size of 1-50 um.
6. The method for preparing a high light transmittance frosted coating according to claim 5, wherein: the curing agent in the step (2) is one of diethylenetriamine, diaminodiphenylmethane and diaminodiphenylsulfone.
CN201911297420.XA 2019-12-17 2019-12-17 Preparation method of film with high-light-transmittance frosted coating Pending CN111116954A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1059073A (en) * 1964-03-20 1967-02-15 Bexford Ltd Improvements in or relating to drafting film
US4614674A (en) * 1984-05-11 1986-09-30 Ciba-Geigy Corporation Powder coating compositions for the preparation of matt coatings
CN104829777A (en) * 2015-05-14 2015-08-12 扬州三涧科贸有限公司 Preparation method of micron-sized highly-crosslinked polymethyl methacrylate (PMMA) microspheres
CN107267055A (en) * 2017-05-26 2017-10-20 吴永芬 A kind of sand streak paint
CN107779051A (en) * 2017-11-15 2018-03-09 黄腾飞 A kind of wear-resistant paint of epoxy transparent frosted
CN108047909A (en) * 2017-12-06 2018-05-18 曹结宾 A kind of processing technology of ground glass
CN108084858A (en) * 2017-12-06 2018-05-29 曹结宾 For the frosted coating of glass surface

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1059073A (en) * 1964-03-20 1967-02-15 Bexford Ltd Improvements in or relating to drafting film
US4614674A (en) * 1984-05-11 1986-09-30 Ciba-Geigy Corporation Powder coating compositions for the preparation of matt coatings
CN104829777A (en) * 2015-05-14 2015-08-12 扬州三涧科贸有限公司 Preparation method of micron-sized highly-crosslinked polymethyl methacrylate (PMMA) microspheres
CN107267055A (en) * 2017-05-26 2017-10-20 吴永芬 A kind of sand streak paint
CN107779051A (en) * 2017-11-15 2018-03-09 黄腾飞 A kind of wear-resistant paint of epoxy transparent frosted
CN108047909A (en) * 2017-12-06 2018-05-18 曹结宾 A kind of processing technology of ground glass
CN108084858A (en) * 2017-12-06 2018-05-29 曹结宾 For the frosted coating of glass surface

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
梁悦等: "三羟甲基丙烷三丙烯酸酯-甲基丙烯酸甲酯沉淀聚合制备单分散聚合物微球", 《高分子学报》 *

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