CN113388138A - High-temperature stable release film and preparation method thereof - Google Patents
High-temperature stable release film and preparation method thereof Download PDFInfo
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- CN113388138A CN113388138A CN202110703317.1A CN202110703317A CN113388138A CN 113388138 A CN113388138 A CN 113388138A CN 202110703317 A CN202110703317 A CN 202110703317A CN 113388138 A CN113388138 A CN 113388138A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—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 a halogen; Derivatives of such polymers
- C08J2327/02—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—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 a halogen; Derivatives of such polymers
- C08J2427/02—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—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 a halogen; Derivatives of such polymers
- C08J2427/02—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/20—Homopolymers or copolymers of hexafluoropropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- Polymers & Plastics (AREA)
- Manufacturing & Machinery (AREA)
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- Wood Science & Technology (AREA)
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- Application Of Or Painting With Fluid Materials (AREA)
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Abstract
The invention belongs to the technical field of release films, and particularly relates to a high-temperature stable release film and a preparation method thereof, wherein the release film comprises a release film layer and a high-temperature resistant resin layer, the high-temperature resistant resin layer is fixedly connected to the release film layer, and the release film layer comprises the following raw material components in percentage by mass: 56-63% of tetrafluoroethylene, 12-15% of hexafluoropropylene, 15-17% of vinylidene fluoride and 10-12% of a toughening agent, wherein the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 35-43% of methyl toluene dimethylsilane, 30-33% of 2- (3, 4-epoxy cyclohexyl) ethyl trimethylsilane, 7-8% of ammonia water, 12-13% of xylene and 8-11% of gamma-glycidyl ether oxygen propyl trimethoxy silane. The stable release film prepared by the invention has good high-temperature stability, has the advantages of no residue of the release film, long-term high temperature resistance, stable size in a high-temperature environment and the like, and the preparation of the high-temperature resistant resin layer not only has good heat resistance, but also has good mechanical properties.
Description
Technical Field
The invention belongs to the technical field of release films, and particularly relates to a high-temperature stable release film and a preparation method thereof.
Background
In the manufacture of printed circuit boards, ceramic electronic components, thermosetting resin products, decorative boards, and the like, release films, also called release films, are often used in processes in which metal plates or resins are sandwiched between them to avoid adhesion between the metal plates or between the resins, and these processes are all carried out under certain high temperature conditions, and release films in the general sense refer to films used for the following purposes: various adhesives, paints, and the like are applied to the film and cured to form a coating film on the film, and then the coating film is peeled off to be used.
The existing release film is easy to deform under the action of high temperature after being used for a long time at high temperature, so that the size of the release film under the high-temperature environment is not stable enough, the conditions of instability, high rejection rate and the like in later use are caused, and the conditions of release layer residue and the like are easy to occur at high temperature.
Therefore, we propose a high temperature stable release film and a preparation method thereof to solve the above problems.
Disclosure of Invention
The present invention is directed to solve the above problems, and an object of the present invention is to provide a high temperature stable release film and a method for manufacturing the same, which has excellent release stability, does not leave a release film, can resist high temperature for a long time, and is dimensionally stable in a high temperature environment.
In order to achieve the purpose, the invention adopts the following technical scheme: the utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 56-63% of tetrafluoroethylene, 12-15% of hexafluoropropylene, 15-17% of vinylidene fluoride and 10-12% of a toughening agent.
In the high-temperature stable release film, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 35-43% of methyl toluene dimethylsilane, 30-33% of 2- (3, 4-epoxy cyclohexyl) ethyl trimethylsilane, 7-8% of ammonia water, 12-13% of xylene and 8-11% of gamma-glycidyl ether oxygen propyl trimethoxy silane.
In a high temperature stable release film, the concentration of ammonia water is 25%.
In the high-temperature stable release film, the toughening agent comprises 45-52% of 1, 4-butanediol diglycidyl ether, 25-26% of toluene diisocyanate, 15-17% of polyether glycol and 8-12% of 2-ethyl-4-methylimidazole.
The invention also discloses a preparation method of the high-temperature stable release film, which comprises the following steps:
s1, adding tetrafluoroethylene, hexafluoropropylene, vinylidene fluoride and a toughening agent in corresponding amounts into a mixer according to the mass percentage of the components, and mixing at the rotating speed of 130-180 rpm;
s2, adding the mixture obtained in the step S1 into a double-screw plastic extruder for melt extrusion, then putting the extruded particles into a hydraulic forming machine for extrusion forming, and forming a film with the thickness of 110-180 mu m after forming;
s3, placing the film obtained in the step S2 in a heating furnace, and heating to 110-120 ℃ to dry the film for 20-30 min;
s4, adding methyl toluene dimethylsilane and 2- (3, 4-epoxy cyclohexyl) ethyltrimethylsilane into a stirrer according to the mass percentage of the components, slowly dropwise adding ammonia water according to a proportion, reacting for 3-4 hours, heating to 60 ℃, vacuumizing, removing the ammonia water in the product, adding xylene according to a proportion, heating to 110 ℃, keeping for 20-30 min, and adding gamma-glycidyl ether oxypropyltrimethoxysilane according to a proportion to obtain a high-temperature-resistant resin layer base material;
s5, uniformly coating the high-temperature-resistant resin layer base material obtained in the step S4 on the film in the step S2, slowly heating the film to 80-90 ℃ in a heating furnace, and keeping the temperature for 30-40 min to completely volatilize the solvent in the high-temperature-resistant resin layer base material;
and after the solvent in the base materials of the high-temperature-resistant resin layers in the S6 and S5 is completely volatilized, continuously heating to 259 ℃, and curing for 0.5-1 h to obtain the high-temperature stable release film.
Compared with the prior art, the invention has the advantages that:
the stable release film prepared by the invention has good high-temperature stability, has the advantages of no residue of the release film, long-term high temperature resistance, stable size in a high-temperature environment and the like, and the preparation of the high-temperature resistant resin layer not only has good heat resistance, but also has good mechanical properties.
Detailed Description
The following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1
The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 63% of tetrafluoroethylene, 12% of hexafluoropropylene, 15% of vinylidene fluoride and 10% of a toughening agent.
Further, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 43% of methyl toluene dimethylsilane, 30% of 2- (3, 4-epoxycyclohexyl) ethyl trimethylsilane, 7% of ammonia water, 12% of xylene and 8% of gamma-glycidoxypropyltrimethoxysilane.
Further, the concentration of the ammonia water is 25%.
Further, the toughening agent comprises 52% of 1, 4-butanediol diglycidyl ether, 25% of toluene diisocyanate, 15% of polyether glycol and 8% of 2-ethyl-4-methylimidazole.
Example 2
The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 59% of tetrafluoroethylene, 13% of hexafluoropropylene, 16% of vinylidene fluoride and 10-12% of a toughening agent.
Further, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 38% of methyl toluene dimethylsilane, 32% of 2- (3, 4-epoxycyclohexyl) ethyl trimethylsilane, 8% of ammonia water, 12% of xylene and 10% of gamma-glycidoxypropyltrimethoxysilane.
Further, the concentration of the ammonia water is 25%.
Further, the toughening agent comprises 50% of 1, 4-butanediol diglycidyl ether, 25% of toluene diisocyanate, 16% of polyether glycol and 9% of 2-ethyl-4-methylimidazole.
Example 3
The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 58% of tetrafluoroethylene, 14% of hexafluoropropylene, 16% of vinylidene fluoride and 12% of a toughening agent.
Further, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 36% of methyl toluene dimethylsilane, 33% of 2- (3, 4-epoxycyclohexyl) ethyl trimethylsilane, 7% of ammonia water, 13% of xylene and 11% of gamma-glycidoxypropyltrimethoxysilane.
Further, the concentration of the ammonia water is 25%.
Further, the toughening agent comprises 48% of 1, 4-butanediol diglycidyl ether, 25% of toluene diisocyanate, 16% of polyether glycol and 11% of 2-ethyl-4-methylimidazole.
Example 3
The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 58% of tetrafluoroethylene, 14% of hexafluoropropylene, 16% of vinylidene fluoride and 12% of a toughening agent.
Further, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 37% of methyl toluene dimethylsilane, 33% of 2- (3, 4-epoxy cyclohexyl) ethyl trimethylsilane, 7% of ammonia water, 13% of xylene and 10% of gamma-glycidyl ether oxygen propyl trimethoxy silane.
Further, the concentration of the ammonia water is 25%.
Further, the toughening agent comprises 47% of 1, 4-butanediol diglycidyl ether, 26% of toluene diisocyanate, 17% of polyether glycol and 10% of 2-ethyl-4-methylimidazole.
Example 4
The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 57% of tetrafluoroethylene, 15% of hexafluoropropylene, 17% of vinylidene fluoride and 11% of a toughening agent.
Further, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 36% of methyl toluene dimethylsilane, 33% of 2- (3, 4-epoxycyclohexyl) ethyl trimethylsilane, 7% of ammonia water, 13% of xylene and 11% of gamma-glycidoxypropyltrimethoxysilane.
Further, the concentration of the ammonia water is 25%.
Further, the toughening agent comprises 46% of 1, 4-butanediol diglycidyl ether, 26% of toluene diisocyanate, 17% of polyether glycol and 11% of 2-ethyl-4-methylimidazole.
Example 5
The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, high temperature resistant resin layer fixed connection is at type rete, from type rete raw materials component mass percent is: 56% of tetrafluoroethylene, 15% of hexafluoropropylene, 17% of vinylidene fluoride and 8% of a toughening agent.
Further, the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 35% of methyl toluene dimethylsilane, 33% of 2- (3, 4-epoxycyclohexyl) ethyl trimethylsilane, 8% of ammonia water, 13% of xylene and 11% of gamma-glycidoxypropyltrimethoxysilane.
Further, the concentration of the ammonia water is 25%.
Further, the toughening agent comprises 45% of 1, 4-butanediol diglycidyl ether, 26% of toluene diisocyanate, 17% of polyether glycol and 12% of 2-ethyl-4-methylimidazole.
In examples 1-5: the preparation method of the high-temperature stable release film comprises the following steps:
s1, adding tetrafluoroethylene, hexafluoropropylene, vinylidene fluoride and a toughening agent in corresponding amounts into a mixer according to the mass percentage of the components, and mixing at the rotating speed of 130-180 rpm;
s2, adding the mixture obtained in the step S1 into a double-screw plastic extruder for melt extrusion, then putting the extruded particles into a hydraulic forming machine for extrusion forming, and forming a film with the thickness of 110-180 mu m after forming;
s3, placing the film obtained in the step S2 in a heating furnace, and heating to 110-120 ℃ to dry the film for 20-30 min;
s4, adding methyl toluene dimethylsilane and 2- (3, 4-epoxy cyclohexyl) ethyltrimethylsilane into a stirrer according to the mass percentage of the components, slowly dropwise adding ammonia water according to a proportion, reacting for 3-4 hours, heating to 60 ℃, vacuumizing, removing the ammonia water in the product, adding xylene according to a proportion, heating to 110 ℃, keeping for 20-30 min, and adding gamma-glycidyl ether oxypropyltrimethoxysilane according to a proportion to obtain a high-temperature-resistant resin layer base material;
s5, uniformly coating the high-temperature-resistant resin layer base material obtained in the step S4 on the film in the step S2, slowly heating the film to 80-90 ℃ in a heating furnace, and keeping the temperature for 30-40 min to completely volatilize the solvent in the high-temperature-resistant resin layer base material;
and after the solvent in the base materials of the high-temperature-resistant resin layers in the S6 and S5 is completely volatilized, continuously heating to 259 ℃, and curing for 0.5-1 h to obtain the high-temperature stable release film.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The utility model provides a high temperature stable form is from type membrane, includes from type rete and high temperature resistant resin layer, its characterized in that, high temperature resistant resin layer fixed connection is at type rete, it is: 56-63% of tetrafluoroethylene, 12-15% of hexafluoropropylene, 15-17% of vinylidene fluoride and 10-12% of a toughening agent.
2. The high-temperature stable release film according to claim 1, wherein the high-temperature resistant resin layer comprises the following raw material components in percentage by mass: 35-43% of methyl toluene dimethylsilane, 30-33% of 2- (3, 4-epoxy cyclohexyl) ethyl trimethylsilane, 7-8% of ammonia water, 12-13% of xylene and 8-11% of gamma-glycidyl ether oxygen propyl trimethoxy silane.
3. The high temperature stable release film according to claim 2, wherein the concentration of ammonia water is 25%.
4. The release film with high temperature stability according to claim 1, wherein the toughening agent comprises 45-52% of 1, 4-butanediol diglycidyl ether, 25-26% of toluene diisocyanate, 15-17% of polyether glycol, and 8-12% of 2-ethyl-4-methylimidazole.
5. The method for preparing a high temperature stable release film according to any one of claims 1-4, wherein the method comprises the following steps:
s1, adding tetrafluoroethylene, hexafluoropropylene, vinylidene fluoride and a toughening agent in corresponding amounts into a mixer according to the mass percentage of the components, and mixing at the rotating speed of 130-180 rpm;
s2, adding the mixture obtained in the step S1 into a double-screw plastic extruder for melt extrusion, then putting the extruded particles into a hydraulic forming machine for extrusion forming, and forming a film with the thickness of 110-180 mu m after forming;
s3, placing the film obtained in the step S2 in a heating furnace, and heating to 110-120 ℃ to dry the film for 20-30 min;
s4, adding methyl toluene dimethylsilane and 2- (3, 4-epoxy cyclohexyl) ethyltrimethylsilane into a stirrer according to the mass percentage of the components, slowly dropwise adding ammonia water according to a proportion, reacting for 3-4 hours, heating to 60 ℃, vacuumizing, removing the ammonia water in the product, adding xylene according to a proportion, heating to 110 ℃, keeping for 20-30 min, and adding gamma-glycidyl ether oxypropyltrimethoxysilane according to a proportion to obtain a high-temperature-resistant resin layer base material;
s5, uniformly coating the high-temperature-resistant resin layer base material obtained in the step S4 on the film in the step S2, slowly heating the film to 80-90 ℃ in a heating furnace, and keeping the temperature for 30-40 min to completely volatilize the solvent in the high-temperature-resistant resin layer base material;
and after the solvent in the base materials of the high-temperature-resistant resin layers in the S6 and S5 is completely volatilized, continuously heating to 250 ℃, and curing for 0.5-1 h to obtain the high-temperature stable release film.
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CN105348946A (en) * | 2015-10-29 | 2016-02-24 | 保定乐凯新材料股份有限公司 | Matt release film |
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CN111002667A (en) * | 2019-12-19 | 2020-04-14 | 宁波长阳科技股份有限公司 | Release film and preparation method thereof |
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2021
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CN105348946A (en) * | 2015-10-29 | 2016-02-24 | 保定乐凯新材料股份有限公司 | Matt release film |
CN106166863A (en) * | 2016-08-11 | 2016-11-30 | 苏州柯创电子材料有限公司 | High temperature resistant compound mould release membrance |
CN109760377A (en) * | 2018-11-22 | 2019-05-17 | 江苏大学 | A kind of high release is without compound release film of silicon and preparation method thereof |
CN110358376A (en) * | 2019-07-22 | 2019-10-22 | 安徽屹珹新材料科技有限公司 | A kind of release coating of fluorine element, fluorine element release film and preparation method thereof |
CN111002667A (en) * | 2019-12-19 | 2020-04-14 | 宁波长阳科技股份有限公司 | Release film and preparation method thereof |
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Title |
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J.弗洛里安等: "《实用热成型原理及应用》", 31 March 1992, 中国石化出版社 * |
杨忠久等: "《硬质塑木复合低发泡产品生产技术和基础知识》", 30 November 2018, 江西科学技术出版社 * |
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