CN112280416A - Manufacturing method of transfer film release agent - Google Patents

Manufacturing method of transfer film release agent Download PDF

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Publication number
CN112280416A
CN112280416A CN202011164946.3A CN202011164946A CN112280416A CN 112280416 A CN112280416 A CN 112280416A CN 202011164946 A CN202011164946 A CN 202011164946A CN 112280416 A CN112280416 A CN 112280416A
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wax
grinding
release agent
transfer film
film release
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CN112280416B (en
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吴伟斌
苏国芳
胡锋
刘玫
舒林飞
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Zhejiang Longyou Daoming Optics & Chemical Co ltd
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Zhejiang Longyou Daoming Optics & Chemical Co ltd
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    • 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
    • C09D133/00Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04Homopolymers or copolymers of esters
    • C09D133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/10Homopolymers or copolymers of methacrylic acid esters
    • C09D133/12Homopolymers or copolymers of methyl methacrylate
    • 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
    • C09D133/00Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04Homopolymers or copolymers of esters
    • C09D133/14Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
    • 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
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1656Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662Synthetic film-forming substance
    • C09D5/1668Vinyl-type polymers
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    • 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
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1687Use of special additives
    • 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
    • C09D5/20Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a manufacturing method of a transfer film release agent, which comprises the following steps: a-1, taking acrylic resin, cellulose acetate butyrate, an antistatic agent and butanone A, heating, stirring, cooling and filtering to obtain matrix resin; a-2, uniformly mixing and soaking butanone B, wax powder A, wax powder B and a dispersing agent to obtain a wax powder mixture; a-3, mixing and stirring a wax powder mixture and matrix resin to obtain a pre-dispersed wax slurry mixture; a-4, taking a pre-dispersed wax slurry mixture, and grinding to obtain crude wax slurry; a-5, taking the crude wax slurry, and grinding to obtain fine wax slurry; and A-6, uniformly mixing the fine wax slurry, butanone C, ethyl acetate and cyclohexanone to finally obtain the transfer film release agent. Through the design, the obtained transfer film release agent has strong scratch resistance, strong stability and strong coating uniformity.

Description

Manufacturing method of transfer film release agent
Technical Field
The invention relates to the technical field of release agents, in particular to a manufacturing method of a transfer film release agent.
Background
The release agent used by the carbon ribbon on the market at present generally adopts a mixture of resin and wax. For a resin and wax mixed type release agent, a release agent is generally formed by directly mixing commercially available wax slurry with a resin, so that the wax slurry is unevenly dispersed, and a scribing line is easily generated after coating, so that the coating is uneven. In addition, the solution directly dispersed by the resin and the wax slurry is easy to generate precipitation and delamination phenomena, and uneven coating before and after the solution is also caused. Therefore, the existing release agent has the defects of poor scratch resistance, poor stability, poor coating uniformity and the like, so that the release agent needs to be improved.
Disclosure of Invention
The invention provides a novel preparation method of a transfer film release agent, aiming at the defects of poor scratch resistance, poor stability, poor coating uniformity and the like of a resin and wax mixed release agent in the prior art.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a manufacturing method of a transfer film release agent comprises the following steps:
a-1, taking acrylic resin, cellulose acetate butyrate, an antistatic agent and butanone A, and mixing the components in a proportion of 30-45: 1.5-2: 0.5-0.8: 70-90 weight percent of the mixture is put into a reaction kettle for heating and stirring, the heating temperature is 50-60 ℃, the stirring linear speed is 7-10 m/s, the mixture is stirred for 60-90 minutes until the acrylic resin is completely dissolved, then the stirring is stopped and the mixture is cooled to 20-25 ℃, and the matrix resin with the solid content of 30 percent is obtained after the filtration;
a-2, taking butanone B, wax powder A, wax powder B and a dispersing agent, and mixing the components in a proportion of 30-40: 4-4.8: 6-7.5: 3-3.7, and soaking for 8-12 hours to obtain a wax powder mixture;
a-3, taking the wax powder mixture and the matrix resin, and mixing the wax powder mixture and the matrix resin according to the weight ratio of 40-60: mixing and stirring at the weight ratio of 40-60, wherein the stirring linear speed is 7-10 m/s, the stirring time is 30-60 minutes, and a pre-dispersed wax slurry mixture is obtained after stirring;
a-4, injecting the pre-dispersed wax slurry mixture into a horizontal rod tip type sand mill for grinding, wherein the grinding efficiency is 3 liters per minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.6-0.8 mm and the Mohs hardness of more than 9, the grinding time is 4-6 hours, the rotational linear speed in a grinding cavity is 15-18 m/s, and coarse wax slurry with the particle size distribution D90 being 600nm is obtained after grinding is completed;
a-5, injecting the coarse wax slurry into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 1.5 liters/minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.3-0.5 mm and the Mohs hardness of more than 9, the grinding time is 4-6 hours, the linear speed of rotation in a grinding cavity is 10-15 meters/second, and fine wax slurry with the particle size distribution of D90 being 400nm is obtained after grinding is finished;
a-6, taking the fine wax slurry, butanone C, ethyl acetate and cyclohexanone, and mixing according to the weight ratio of 10-15: 20-28: 8-12: and (2) 2-2.5, and uniformly mixing in a sealed container to finally obtain the transfer film release agent.
And (2) dissolving in the reaction kettle in the step A-1, wherein the acrylic resin is heated to be close to the glass transition temperature of the acrylic resin, so that the acrylic resin is converted into a liquid state from a semi-solid state and is directly and quickly dissolved in the butanone A, meanwhile, the equipment sealing performance is better and the solid content is stable in the heating and cooling processes, and the acrylic resin and the cellulose acetate butyrate are selected to ensure that the scratch resistance of the obtained transfer film release agent is better. The long-time soaking in the step A-2 is more beneficial to the wax powder A and the wax powder B to fully absorb the butanone B expansion, and is also more beneficial to the subsequent working procedure for processing. In the step A-3, the wax powder mixture and the matrix resin are stirred for 30 to 60 minutes at the stirring linear speed of 7 to 10 meters per second, so that the wax powder mixture and the matrix resin are mixed more uniformly. The yttrium-stabilized zirconia beads with the particle size of 0.6-0.8 mm and the Mohs hardness of more than 9 are adopted in the step A-4, so that the pre-dispersed wax slurry mixture can be effectively and fully ground in the cavity, and meanwhile, under the environment that the online speed is 15-18 m/s, the grinding is carried out for 4-6 hours, and the pre-dispersed wax slurry mixture can be quickly ground to reach the D90-600 nm degree. In the step A-5, yttrium stable zirconia beads with the grain diameter of 0.3-0.5 mm and the Mohs hardness of more than 9 are adopted, so that the crude wax slurry can be effectively and fully ground in the cavity, and meanwhile, under the environment that the online speed is 10-15 m/s, the crude wax slurry can be quickly ground for 4-6 hours to reach the D90-400 nm degree. In the step A-6, a mode of mixing in a sealed container is adopted, so that the stability of the transfer film release agent is more facilitated, and the problem of unstable solid content of the final transfer film release agent caused by the fact that butanone C belongs to a quick-drying solvent is solved.
Through the design, the obtained transfer film release agent has strong scratch resistance, strong stability and strong coating uniformity.
Preferably, in the above method for manufacturing the transfer film release agent, the temperature of the water chilling unit of the horizontal rod-tip sand mill in the step a-4 is 15 ℃, the external circulation temperature is 25 ℃ to 30 ℃, the internal circulation temperature is 28 ℃ to 35 ℃, and the temperature of the external cylinder barrel is 35 ℃ to 40 ℃.
The melting point of the pre-dispersed wax pulp mixture is 70-90 ℃, the temperature of a water chilling unit of the horizontal rod-tip type sand mill is 15 ℃, the external circulation temperature is 25-30 ℃, the internal circulation temperature is 28-35 ℃ and the temperature of an external cylinder barrel is 35-40 ℃, so that the pre-dispersed wax pulp mixture can keep certain hardness, and the preliminary grinding of the pre-dispersed wax pulp mixture is facilitated under the condition of low temperature.
Preferably, in the above method for manufacturing the transfer film release agent, the temperature of the water chilling unit of the horizontal rod-tip sand mill in the step a-5 is 5 ℃, the external circulation temperature is 10 ℃ to 15 ℃, the internal circulation temperature is 12 ℃ to 17 ℃, and the temperature of the external cylinder barrel is 20 ℃ to 25 ℃.
The temperature of a water chilling unit of the horizontal rod-tip type sand mill is 5 ℃, the external circulation temperature is 10-15 ℃, the internal circulation temperature is 12-17 ℃ and the temperature of an external cylinder barrel is 20-25 ℃, so that the environmental temperature of the crude wax slurry is reduced to be lower, the nanoscale crude wax slurry keeps certain hardness, and the superfine grinding of the crude wax slurry is facilitated.
Preferably, in the above method for manufacturing the transfer film release agent, the acrylic resin is formed by mixing a methyl methacrylate copolymer and a hydroxyethyl methacrylate copolymer in a weight ratio of 1:1, and the glass transition temperature of the acrylic resin is 90 ℃ to 120 ℃.
The acrylic resin is prepared by mixing a methyl methacrylate copolymer and a hydroxyethyl methacrylate copolymer in a weight ratio of 1:1, and has a glass transition temperature of 90-120 ℃, so that after the release agent is coated and dried, a coating has better edge cutting property and scratch resistance and more excellent solvent resistance.
Preferably, in the above method for producing a transfer film release agent, the cellulose acetate butyrate has a butyryl group content of 37%, an acetyl group content of 13%, and a hydroxyl group content of 1.5%.
The cellulose acetate butyrate with 37 percent of butyryl group content, 13 percent of acetyl group content and 1.5 percent of hydroxyl group content has better compatibility with acrylic resin, and can more effectively play the role of the transfer film release agent.
Preferably, in the above method for producing a transfer film release agent, the antistatic agent is a cationic quaternary ammonium salt compound.
The antistatic agent adopts a cationic quaternary ammonium salt compound, so that the obtained transfer film release agent has strong adsorption force with polymers when in use, and is more wear-resistant and washing-resistant. Cationic quaternary ammonium compounds can be used with the american type cyanoantistatic agent CYASTAT SN.
Preferably, in the above method for manufacturing the transfer film release agent, the wax powder a is 1061 polished wax micropowder of Nanjing Tianshi New science and technology Co.
By adopting 1061 polishing wax micropowder of Nanjing Tianshi New Material science and technology Limited, the scratch resistance and the smoothness of the transfer film release agent are higher, and the transfer film release agent has better luster and light transmittance.
Preferably, in the above method for manufacturing the transfer film release agent, the wax powder B is W501 polyethylene wax micropowder of new material science and technology ltd.
By adopting W501 polyethylene wax micropowder of Nanjing Tianshi new material science and technology Limited, the transfer film release agent has better characteristics of adhesion resistance, scratch resistance, dirt resistance, friction resistance and the like, and the coating of the transfer film release agent is smoother and softer, and the hydrophobicity and the sealing property are improved.
Preferably, in the above method for manufacturing a transfer film release agent, the dispersant is a polyester-based multi-chain polymer dispersant.
The polyester multi-chain high molecular polymer dispersant can adopt the polyester multi-chain high molecular polymer dispersant with 99.99 percent of active content, so that the wax powder A and the wax powder B are more stable in the butanone B.
Detailed Description
The invention is described in further detail below by means of specific embodiments, which are not intended to limit the invention:
example 1
A manufacturing method of a transfer film release agent comprises the following steps:
a-1, taking acrylic resin, cellulose acetate butyrate, an antistatic agent and butanone A, and mixing the components in a proportion of 30: 1.5: 0.5: 70 weight percent of the mixture is put into a reaction kettle for heating and stirring, the heating temperature is 50 ℃, the stirring linear velocity is 7 m/s, the stirring is carried out for 60 minutes until the acrylic resin is completely dissolved, then the stirring is stopped and the mixture is cooled to 20 ℃, and the matrix resin with the solid content of 30 percent is obtained after the filtration;
a-2, taking butanone B, wax powder A, wax powder B and a dispersing agent, and mixing the components in a proportion of 30: 4: 6: 3, uniformly mixing and soaking for 8 hours to obtain a wax powder mixture after soaking;
a-3, taking the wax powder mixture and the matrix resin, and mixing the wax powder mixture and the matrix resin according to the weight ratio of 40: 60, stirring at a stirring linear speed of 7 m/s for 30 minutes to obtain a pre-dispersed wax slurry mixture;
a-4, injecting the pre-dispersed wax slurry mixture into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 3 liters per minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.6mm and the Mohs hardness of more than 9, the grinding time is 4 hours, the rotational linear velocity in a grinding cavity is 15 m/s, and coarse wax slurry with the particle size distribution of D90-600 nm is obtained after grinding is completed;
a-5, injecting the coarse wax slurry into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 1.5 liters/minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.3mm and the Mohs hardness of more than 9, the grinding time is 4 hours, the rotational linear velocity in a grinding cavity is 10 m/second, and fine wax slurry with the particle size distribution of D90-400 nm is obtained after grinding is completed;
a-6, taking the fine wax slurry, butanone C, ethyl acetate and cyclohexanone, and mixing the components in a proportion of 10: 20: 8: 2 in a sealed container, and finally obtaining the transfer film release agent.
Preferably, the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-4 is 15 ℃, the external circulation temperature is 25 ℃, the internal circulation temperature is 28 ℃ and the temperature of an external cylinder barrel is 35 ℃.
Preferably, the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-5 is 5 ℃, the external circulation temperature is 10 ℃, the internal circulation temperature is 12 ℃ and the temperature of an external cylinder barrel is 20 ℃.
Preferably, the acrylic resin is formed by mixing a methyl methacrylate copolymer and a hydroxyethyl methacrylate copolymer according to a weight ratio of 1:1, and the glass transition temperature of the acrylic resin is 90 ℃.
Preferably, the cellulose acetate butyrate has a butyryl group content of 37%, an acetyl group content of 13%, and a hydroxyl group content of 1.5%.
Preferably, the antistatic agent is a cationic quaternary ammonium salt compound.
Preferably, the wax powder A is 1061 polishing wax micropowder of Nanjing Tianshi new material science and technology Co.
Preferably, the wax powder B is W501 polyethylene wax micropowder of Nanjing Tianshi new material science and technology Limited.
Preferably, the dispersant is a polyester-based multi-chain high molecular polymer dispersant.
Example 2
A manufacturing method of a transfer film release agent comprises the following steps:
a-1, taking acrylic resin, cellulose acetate butyrate, an antistatic agent and butanone A, and mixing the components in percentage by weight of 45: 2: 0.8: 90 weight percent of the mixture is put into a reaction kettle for heating and stirring, the heating temperature is 60 ℃, the stirring linear speed is 10 m/s, the mixture is stirred for 90 minutes until the acrylic resin is completely dissolved, then the stirring is stopped and the mixture is cooled to 25 ℃, and the matrix resin with the solid content of 30 percent is obtained after the filtration;
a-2, taking butanone B, wax powder A, wax powder B and a dispersing agent, and mixing the components in a proportion of 40: 4.8: 7.5: 3.7, uniformly mixing and soaking for 12 hours to obtain a wax powder mixture after soaking;
a-3, taking the wax powder mixture and the matrix resin, and mixing the wax powder mixture and the matrix resin according to the weight ratio of 60: 40, stirring at the stirring linear speed of 10 m/s for 60 minutes to obtain a pre-dispersed wax slurry mixture;
a-4, injecting the pre-dispersed wax slurry mixture into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 3 liters per minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.8mm and the Mohs hardness of more than 9, the grinding time is 6 hours, the rotational linear velocity in a grinding cavity is 18 m/s, and coarse wax slurry with the particle size distribution of D90-600 nm is obtained after grinding is completed;
a-5, injecting the coarse wax slurry into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 1.5 liters per minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.5mm and the Mohs hardness of more than 9, the grinding time is 6 hours, the rotational linear velocity in a grinding cavity is 15 m/s, and fine wax slurry with the particle size distribution of D90-400 nm is obtained after grinding is completed;
a-6, taking the fine wax slurry, butanone C, ethyl acetate and cyclohexanone, and mixing the components in a proportion of 15: 28: 12: 2.5, and uniformly mixing in a sealed container to finally obtain the transfer film release agent.
Preferably, the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-4 is 15 ℃, the external circulation temperature is 30 ℃, the internal circulation temperature is 35 ℃ and the temperature of an external cylinder barrel is 40 ℃.
Preferably, the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-5 is 5 ℃, the external circulation temperature is 15 ℃, the internal circulation temperature is 17 ℃ and the temperature of an external cylinder barrel is 25 ℃.
Preferably, the acrylic resin is formed by mixing a methyl methacrylate copolymer and a hydroxyethyl methacrylate copolymer according to a weight ratio of 1:1, and the glass transition temperature of the acrylic resin is 120 ℃.
Preferably, the cellulose acetate butyrate has a butyryl group content of 37%, an acetyl group content of 13%, and a hydroxyl group content of 1.5%.
Preferably, the antistatic agent is a cationic quaternary ammonium salt compound.
Preferably, the wax powder A is 1061 polishing wax micropowder of Nanjing Tianshi new material science and technology Co.
Preferably, the wax powder B is W501 polyethylene wax micropowder of Nanjing Tianshi new material science and technology Limited.
Preferably, the dispersant is a polyester-based multi-chain high molecular polymer dispersant.
Example 3
A manufacturing method of a transfer film release agent comprises the following steps:
a-1, taking acrylic resin, cellulose acetate butyrate, an antistatic agent and butanone A, and mixing the components in a proportion of 37.5: 1.75: 0.65: 80 weight percent of the mixture is put into a reaction kettle for heating and stirring, the heating temperature is 55 ℃, the stirring linear velocity is 8.5 m/s, the stirring is carried out for 75 minutes until the acrylic resin is completely dissolved, then the stirring is stopped, the mixture is cooled to 22.5 ℃, and the matrix resin with the solid content of 30 percent is obtained after the filtration;
a-2, taking butanone B, wax powder A, wax powder B and a dispersing agent, and mixing the components in a proportion of 35: 4.4: 6.75: 3.35, and soaking for 10 hours to obtain a wax powder mixture;
a-3, taking the wax powder mixture and the matrix resin, and mixing the wax powder mixture and the matrix resin according to the weight ratio of 50: 50, stirring at the stirring linear speed of 8.5 m/s for 45 minutes to obtain a pre-dispersed wax slurry mixture;
a-4, injecting the pre-dispersed wax slurry mixture into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 3 liters per minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.7mm and the Mohs hardness of more than 9, the grinding time is 5 hours, the rotational linear velocity in a grinding cavity is 16.5 meters per second, and coarse wax slurry with the particle size distribution of D90-600 nm is obtained after grinding is completed;
a-5, injecting the coarse wax slurry into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 1.5 liters/minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.4mm and the Mohs hardness of more than 9, the grinding time is 5 hours, the linear speed of rotation in a grinding cavity is 12.5 meters/second, and fine wax slurry with the particle size distribution of D90-400 nm is obtained after grinding is completed;
a-6, taking the fine wax slurry, butanone C, ethyl acetate and cyclohexanone, and mixing the components in a proportion of 12.5: 24: 10: 2.25, and uniformly mixing in a sealed container to finally obtain the transfer film release agent.
Preferably, the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-4 is 15 ℃, the external circulation temperature is 27.5 ℃, the internal circulation temperature is 31.5 ℃ and the temperature of an external cylinder barrel is 37.5 ℃.
Preferably, the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-5 is 5 ℃, the external circulation temperature is 12.5 ℃, the internal circulation temperature is 14.5 ℃ and the temperature of an external cylinder barrel is 22.5 ℃.
Preferably, the acrylic resin is formed by mixing a methyl methacrylate copolymer and a hydroxyethyl methacrylate copolymer according to a weight ratio of 1:1, and the glass transition temperature of the acrylic resin is 105 ℃.
Preferably, the cellulose acetate butyrate has a butyryl group content of 37%, an acetyl group content of 13%, and a hydroxyl group content of 1.5%.
Preferably, the antistatic agent is a cationic quaternary ammonium salt compound.
Preferably, the wax powder A is 1061 polishing wax micropowder of Nanjing Tianshi new material science and technology Co.
Preferably, the wax powder B is W501 polyethylene wax micropowder of Nanjing Tianshi new material science and technology Limited.
Preferably, the dispersant is a polyester-based multi-chain high molecular polymer dispersant.
Example 4
Taking the transfer film mold release agent obtained in each example, taking the JY-03 transfer film mold release agent of the existing Jiajun transfer material Co., Ltd, Dongguan city as a comparative example, and carrying out tests on coating, drying, printing and solvent resistance, wherein the test method comprises the following steps:
firstly, coating test: the compounded comparative sample was coated on a 4.5 micron PET surface with occasional small holes; the samples of example 1, example 2 and example 3 were coated on the surface of 4.5 μm PET, respectively, and the coating appearance was good and no abnormality was observed.
Secondly, drying test: and (3) respectively putting the compounded samples of the comparative example, the example 1, the example 2 and the example 3 into an oven at 80 ℃ for baking for 10 seconds by using a coating wire rod, so that the dry thickness of the coating is 1-2 microns. As a result, the comparative example was not completely dried and slightly tacky; the samples of the embodiment 1, the embodiment 2 and the embodiment 3 are completely dried, and the effect is better.
Thirdly, printing and testing: the carbon tapes prepared by the samples of comparative example, example 1, example 2 and example 3 were printed with a zebra ZM600 printer at a printing energy level of 23 and a printing speed of 5cm/s, respectively, as barcodes and two-dimensional codes. As a result, the edge cutting of the comparative example was not perfect, and a jagging phenomenon occurred; the effects of the examples 1, 2 and 3 are good and have no obvious difference.
Fourthly, wear resistance test: the Xinbao OTS alcohol abrasion resistance tester is adopted for testing, four groups of samples printed in the printing test are respectively used for abrasion resistance testing by cotton cloth stained with alcohol. As a result, example 3 was excellent in effect, examples 1 and 2 were excellent in effect, and the comparative example was the least effective.
The transfer film release agent obtained in each embodiment of the invention and the performance parameters of the comparative example are shown in table 1:
TABLE 1
Sample (I) Test one Test two Test three Test four
Example 1 Superior food Superior food Superior food Good wine
Example 2 Superior food Superior food Superior food Good wine
Example 3 Superior food Superior food Superior food Superior food
Comparative example Difference (D) Good wine Good wine Difference (D)
In summary, the above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the present invention.

Claims (9)

1. A manufacturing method of a transfer film release agent is characterized by comprising the following steps: the method comprises the following steps:
a-1, taking acrylic resin, cellulose acetate butyrate, an antistatic agent and butanone A, and mixing the components in a proportion of 30-45: 1.5-2: 0.5-0.8: 70-90 weight percent of the mixture is put into a reaction kettle for heating and stirring, the heating temperature is 50-60 ℃, the stirring linear speed is 7-10 m/s, the mixture is stirred for 60-90 minutes until the acrylic resin is completely dissolved, then the stirring is stopped and the mixture is cooled to 20-25 ℃, and the matrix resin with the solid content of 30 percent is obtained after the filtration;
a-2, taking butanone B, wax powder A, wax powder B and a dispersing agent, and mixing the components in a proportion of 30-40: 4-4.8: 6-7.5: 3-3.7, and soaking for 8-12 hours to obtain a wax powder mixture;
a-3, taking the wax powder mixture and the matrix resin, and mixing the wax powder mixture and the matrix resin according to the weight ratio of 40-60: mixing and stirring at the weight ratio of 40-60, wherein the stirring linear speed is 7-10 m/s, the stirring time is 30-60 minutes, and a pre-dispersed wax slurry mixture is obtained after stirring;
a-4, injecting the pre-dispersed wax slurry mixture into a horizontal rod tip type sand mill for grinding, wherein the grinding efficiency is 3 liters per minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.6-0.8 mm and the Mohs hardness of more than 9, the grinding time is 4-6 hours, the rotational linear speed in a grinding cavity is 15-18 m/s, and coarse wax slurry with the particle size distribution D90 being 600nm is obtained after grinding is completed;
a-5, injecting the coarse wax slurry into a horizontal rod tip type sand mill for grinding, wherein the grinding energy efficiency is 1.5 liters/minute, a grinding medium is yttrium stable zirconia beads with the particle size of 0.3-0.5 mm and the Mohs hardness of more than 9, the grinding time is 4-6 hours, the linear speed of rotation in a grinding cavity is 10-15 meters/second, and fine wax slurry with the particle size distribution of D90 being 400nm is obtained after grinding is finished;
a-6, taking the fine wax slurry, butanone C, ethyl acetate and cyclohexanone, and mixing according to the weight ratio of 10-15: 20-28: 8-12: and (2) 2-2.5, and uniformly mixing in a sealed container to finally obtain the transfer film release agent.
2. The method for manufacturing a transfer film release agent according to claim 1, wherein: the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-4 is 15 ℃, the external circulation temperature is 25-30 ℃, the internal circulation temperature is 28-35 ℃ and the temperature of an external cylinder barrel is 35-40 ℃.
3. The method for manufacturing a transfer film release agent according to claim 1, wherein: the temperature of a water chilling unit of the horizontal rod tip type sand mill in the step A-5 is 5 ℃, the external circulation temperature is 10-15 ℃, the internal circulation temperature is 12-17 ℃ and the temperature of an external cylinder barrel is 20-25 ℃.
4. The method for manufacturing a transfer film release agent according to claim 1, wherein: the acrylic resin is prepared by mixing a methyl methacrylate copolymer and a hydroxyethyl methacrylate copolymer in a weight ratio of 1:1, and the glass transition temperature of the acrylic resin is 90-120 ℃.
5. The method for manufacturing a transfer film release agent according to claim 1, wherein: the cellulose acetate butyrate has a butyryl content of 37%, an acetyl content of 13%, and a hydroxyl content of 1.5%.
6. The method for manufacturing a transfer film release agent according to claim 1, wherein: the antistatic agent is a cationic quaternary ammonium salt compound.
7. The method for manufacturing a transfer film release agent according to claim 1, wherein: the wax powder A is 1061 polishing wax micro powder of Nanjing Tianshi new material science and technology Limited.
8. The method for manufacturing a transfer film release agent according to claim 1, wherein: the wax powder B is W501 polyethylene wax micro powder of Nanjing Tianshi new material science and technology Limited.
9. The method for manufacturing a transfer film release agent according to claim 1, wherein: the dispersant is polyester multi-chain polymer dispersant.
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Publication number Priority date Publication date Assignee Title
US20040214927A1 (en) * 2003-01-24 2004-10-28 Nitzsche Norman E. Compatible multi-functional color concentrate compositions
WO2006012424A2 (en) * 2004-07-20 2006-02-02 Sipix Imaging, Inc. Adhesive layer composition for in-mold decoration
CN103602143A (en) * 2013-11-29 2014-02-26 洋紫荆油墨(浙江)有限公司 Transfer printing ink with release function
CN106700727A (en) * 2015-11-17 2017-05-24 洋紫荆油墨(浙江)有限公司 Gluing-free thermal transfer printing ink with release function
CN110591488A (en) * 2019-10-08 2019-12-20 云南玉溪东魅包装材料有限公司 Antistatic composition for alumite coloring layer and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040214927A1 (en) * 2003-01-24 2004-10-28 Nitzsche Norman E. Compatible multi-functional color concentrate compositions
WO2006012424A2 (en) * 2004-07-20 2006-02-02 Sipix Imaging, Inc. Adhesive layer composition for in-mold decoration
CN103602143A (en) * 2013-11-29 2014-02-26 洋紫荆油墨(浙江)有限公司 Transfer printing ink with release function
CN106700727A (en) * 2015-11-17 2017-05-24 洋紫荆油墨(浙江)有限公司 Gluing-free thermal transfer printing ink with release function
CN110591488A (en) * 2019-10-08 2019-12-20 云南玉溪东魅包装材料有限公司 Antistatic composition for alumite coloring layer and preparation method thereof

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