CN107722864B - Release film with medium release force and high residual adhesion rate and preparation method thereof - Google Patents
Release film with medium release force and high residual adhesion rate and preparation method thereof Download PDFInfo
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
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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
- 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
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/005—Presence of polyester in the release coating
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
- C09J2483/005—Presence of polysiloxane in the release coating
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
The invention provides a release film with medium release force and high residual adhesion rate, which comprises a film substrate and a release layer, wherein the release layer comprises 45-65 parts of liquid silicone resin, 45-25 parts of vinyl silicone oil, 5-25 parts of hydrogen-containing silicone oil, 0.1-0.3 part of catalyst, 0.005-0.02 part of inhibitor, 0.05-0.10 part of tackifier and 300-400 parts of organic solvent, and the liquid silicone resin is prepared by dissolving methyl vinyl MQ silicone resin and methyl vinyl silicone oil according to the mass ratio of 0.05-0.15:1 at the temperature of 100-150 ℃; the catalyst is platinum chelate; the inhibitor is an alkynol compound; the tackifier is a silane coupling agent containing hydroxyl, methoxy or ethoxy. The release film has high mechanical strength of the release layer and less low molecular substances, so the residual adhesion rate is high, and the phenomena of reverse peeling and oil production are greatly reduced.
Description
Technical Field
The invention relates to a release film, in particular to a release film used in the fields of die cutting and photoelectric product deep processing, and more particularly relates to a release film with medium release force and high residual adhesion rate used in the fields of die cutting and photoelectric product deep processing. The invention also relates to a preparation method of the release film with medium release force and high residual adhesion rate.
Background
The release film refers to a film having a surface with separability, and the release film is not sticky or slightly sticky after being contacted with a specific material under limited conditions. The release film generally comprises a film substrate and a release agent coated on the substrate, and can be divided into a light release film, a medium release film and a heavy release film according to the release force; the release film with medium release force is generally used in the fields of die cutting and deep processing of photoelectric products. The release agent used as the release film at present is mainly a silicone release agent, the release agent can be heated and cured, and compared with a photocuring acrylic acid system material, the silicone gel formed by thermosetting processing can have lower release force and lower cost. However, the release film produced in China at present and adopting organic silicon as a release agent often has the phenomena of reverse peeling, uneven coating and oil production; the reverse stripping is that the coating on the release film is taken away by the adhesive film with larger binding force, and a release film coating area which is difficult to clean is formed on the local part of the adhesive film, so that the overall purity and consistency of the adhesive film are damaged; the oil yielding phenomenon is that unreacted micromolecules in the release agent permeate out, so that the release surface of the release film is greasy, and even the back of the base material is greasy through the film base material with deep concave holes after corona treatment; all these phenomena are related to the material system of the release agent. The existing material system of the release agent is mostly a material system which is formed by taking vinyl organic silicon resin as a main raw material and matching with some functional additives according to functions required by the application field of the release film, and because the vinyl organic silicon resin is directly liquid resin with small molecular weight, the resin with small molecular weight has low crosslinking degree, the mechanical strength of colloid is not high enough, and a release layer with low mechanical strength is easy to generate the phenomena of reverse peeling and oil production; the vinyl organic silicon resin with large molecular weight can increase the crosslinking degree, but is not easy to disperse when being directly used because of being powdery.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a release film with medium release force and high residual adhesion rate, the coating of the release film is uniform, and the phenomena of anti-stripping and oil production are greatly reduced.
The invention also aims to provide a preparation method of the release film with medium release force and high residual adhesion rate.
In order to achieve the above purpose, the release film with medium release force and high residual adhesion rate of the invention comprises a film substrate and a release layer, and is characterized in that: the film base material is one of BOPET, BOPP, PP, PE and PC films, and the release layer comprises the following components in parts:
45-65 parts of liquid silicone resin
45-25 parts of vinyl silicone oil
5-25 parts of hydrogen-containing silicone oil
0.1 to 0.3 portion of catalyst
0.005-0.02 portion of inhibitor
0.05 to 0.10 portion of tackifier
Organic solvent 300-400 parts
Wherein the liquid silicone resin is a liquid silicone resin with the viscosity of 2500-3000 mpa.s, which is obtained by stirring methyl vinyl MQ silicone resin with the relative molecular weight of between 15000-20000 and M/Q =1.2 and methyl vinyl silicone oil with the viscosity of 200-5000 mpa.s and the vinyl mole percent of 0.1-1.0% according to the mass ratio of 0.05-0.15:1 at the temperature of 100-150 ℃ and the stirring speed of 500-1000rpm for 1-1.5 hours; the catalyst is platinum chelate; the inhibitor is an alkynol compound; the tackifier is a silane coupling agent containing hydroxyl, methoxy or ethoxy; the structural formula of the methyl vinyl MQ silicon resin is as follows:
the vinyl silicone oil is terminal vinyl silicone oil with the viscosity of 500-5000mpas and the vinyl mole percentage of 0.2-1.0 percent, and the structural formula is as follows:
the hydrogen-containing silicone oil has the viscosity of 200-500mpas and the hydrogen-containing molar ratio percentage of 0.2-1.4 percent, and the structural formula is as follows:
the catalyst is preferably a reaction product of chloroplatinic acid and tetramethyldivinyldisiloxane.
The above inhibitor is preferably ethynylcyclohexanol.
The solvent is preferably one or both of toluene and methyl ethyl ketone.
The film substrate is preferably a BOPET film having a thickness of 25 μm to 100. mu.m.
The invention also provides a preparation method of the release film with medium release force and high residual adhesion, which comprises the following steps:
(1) preparation of film substrate: purifying and corona or plasma treating the surface of the film base material;
(2) preparation of a release agent: weighing the components according to the weight of the formula of the release agent, adding liquid silicone resin, vinyl silicone oil, a catalyst, an inhibitor, a tackifier and an organic solvent into a reactor, stirring and mixing uniformly at the rotating speed of 400rpm/60min, then adding hydrogen-containing silicone oil, and stirring and mixing uniformly at 800rpm/60 min;
(3) coating a release agent on the surface of the film base material treated in the step (1) and drying, wherein the wet coating amount of the release agent is 3g/m2-15g/m2The drying temperature is 80-150 ℃;
(4) and rolling and packaging the dried release film.
In the preparation method, the surface of the film base material in the step (1) is cleaned by removing surface dust by using a dust adhering roller; the surface tension of the corona or plasma treated film is more than or equal to 50 dyne.
In the preparation method, the drying in the step (3) is carried out by sectional heating, the speed of a dryer is 20m/min-80m/min, the sectional heating is 80 ℃, 100 ℃, 120 ℃, 150 ℃, and the temperature of a final cooling zone is 130 ℃.
According to the release film with medium release force and high residual adhesion rate, the methyl vinyl silicone oil with specific viscosity and specific vinyl content is used for dissolving the methyl vinyl MQ silicone resin with large molecular weight at high temperature, so that the powdery MQ silicone resin is easy to disperse and can be directly added into a formula for use, macromolecules of the MQ silicone resin can be well spread, the uniform dispersion of a macromolecular structure is facilitated, and the crosslinking reaction can be carried out more thoroughly. The release film adopts the methyl vinyl MQ silicon resin with high molecular weight and the reactive group of-CH = CH2 as a base material, the crosslinking degree of the groups is high, the mechanical strength of the coating is increased, a small amount of uncapped-OH on the periphery of the methyl vinyl MQ silicon resin is also beneficial to improving the adhesive force of the release agent and the base film, and the phenomenon of reverse peeling is greatly reduced, meanwhile, the stereoscopic spherical cage-shaped structure of the methyl vinyl MQ silicon resin is also beneficial to improving the overall leveling property of colloid, is also beneficial to winding some linear low molecular substances, and reduces the phenomenon of oil production. The release film disclosed by the invention has the advantages of dry and smooth surface, no stickiness and high residual adhesion rate.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific examples, which are not intended to limit the scope of the present invention, and equivalent substitutions for the functional additives of the release layer should be included without departing from the concept of the present invention.
Preparation of liquid silicone resin
Mixing and stirring methyl vinyl MQ silicon resin with the relative molecular weight of 17000-19000 and M/Q =1.2 and terminal methyl vinyl silicone oil with the viscosity of 500mpa.s (25 ℃), the vinyl mole percentage of 0.2 percent and the volatility of 200 ℃ of less than or equal to 1.5 according to the mass ratio of 0.1:1 at the temperature of 130 ℃ and the stirring speed of 1000rpm for 1 hour to obtain the liquid silicon resin with the viscosity of 2500-3000mpas (25 ℃).
Second, preparation of release film
1. Formula of release layer
Wherein the viscosity of the vinyl-terminated silicone oil is 800 mpa.s (25 ℃), the mol percentage of the vinyl is 0.45 percent, and the volatile matter at 200 ℃ is less than or equal to 1.5; the viscosity of the hydrogen-containing silicone oil is 200mpas, and the hydrogen-containing molar ratio is 0.20%.
2. Preparation of Release agent
Weighing the components according to the weight of the formula, adding liquid silicone resin, terminal vinyl silicone oil, a platinum catalyst, ethynylcyclohexanol, dimethyldiethoxysilane and an organic solvent into a reactor, stirring and mixing uniformly at the rotation speed of 400 plus materials at 450rpm/60min, then adding hydrogen-containing silicone oil, stirring and mixing uniformly at the rotation speed of 800 plus materials at 850rpm/60min, and obtaining the coating liquid with the viscosity of 50-105 mPas.
3. Preparation of release film
(1) Selecting a BOPET base film with the thickness of 25-100 μm, removing dust on the surface of the BOPET base film by using a dust adhering roller, and performing corona or plasma treatment on the clean surface of the BOPET base film to ensure that the surface tension of the BOPET base film is more than or equal to 50 dynes;
(2) coating the release agent on the surface of the BOPET base film treated in the step (1), and controlling the wet coating amount to be 3g/m2-15g/m2The drying temperature is 80-150 ℃, the step heating is carried out, the speed of a dryer is 20-80 m/min, the step heating is 80 ℃, 100 ℃, 120 ℃, 150 ℃ and the temperature of a final cooling zone is 130 ℃;
(3) and rolling and packaging the dried release film.
Third, product performance test
The products obtained in examples a to d and comparative example and the commercial products were subjected to the tests of the corresponding items, and the results were as follows:
as can be seen from the above table, in example c and comparative example where the Si-H: Vi indices are the same, the peel strength and residual tack of the product obtained without the addition of MQ silicone in the formulation of the comparative example are lower than those of the product obtained with the addition of MQ silicone in example c; the release force of the commercial products between examples b and c is significantly lower than that of the products according to the invention. The release film has dry and smooth surface and no stickiness, and the release layer has high mechanical strength and less low molecular substances, so the release film has high residual adhesion rate and does not produce oil.
Claims (10)
1. The utility model provides a well from type membrane of type force and high residual adhesion rate, includes film substrate and from type layer, its characterized in that: the film base material is one of BOPET, BOPP, PP, PE and PC films, and the release layer comprises the following components in parts:
45-65 parts of liquid silicone resin
45-25 parts of vinyl silicone oil
5-25 parts of hydrogen-containing silicone oil
0.1 to 0.3 portion of catalyst
0.005-0.02 portion of inhibitor
0.05 to 0.10 portion of tackifier
Organic solvent 300-400 parts
Wherein the liquid silicone resin is a liquid silicone resin with the viscosity of 2500-3000 mPa.s, which is obtained by stirring methyl vinyl MQ silicone resin with the relative molecular weight of between 15000-20000 and M/Q =1.2 and methyl vinyl silicone oil with the viscosity of 200-5000 mPa.s and the vinyl mole percent of 0.1-1.0% for 1-1.5 hours at the temperature of 100-150 ℃ and the stirring speed of 500-1000rpm according to the mass ratio of 0.05-0.15: 1; the catalyst is platinum chelate; the inhibitor is an alkynol compound; the tackifier is a silane coupling agent containing hydroxyl, methoxy or ethoxy; the structural formula of the methyl vinyl MQ silicon resin is as follows:
2. the release film with medium release force and high residual adhesion according to claim 1, wherein: the vinyl silicone oil is terminal vinyl silicone oil with the viscosity of 500-5000mPa.s and the vinyl mole percentage of 0.2-1.0%.
3. The release film with medium release force and high residual adhesion according to claim 1 or 2, wherein: the hydrogen-containing silicone oil has the viscosity of 200-500mPa.s and the hydrogen-containing molar ratio percentage of 0.2-1.4%.
4. The release film with medium release force and high residual adhesion according to claim 3, wherein: the method is characterized in that: the catalyst is a reaction product of chloroplatinic acid and tetramethyldivinyldisiloxane.
5. The release film with medium release force and high residual adhesion according to claim 4, wherein: the inhibitor is ethynyl cyclohexanol.
6. The release film with medium release force and high residual adhesion according to claim 5, wherein: the solvent is one or two of toluene or butanone.
7. The release film with medium release force and high residual adhesion according to claim 1 or 2, wherein: the film substrate is preferably a BOPET film with a thickness of 25-100 μm.
8. A method for preparing the release film with the release force and the high residual adhesion rate of any one of claims 1 to 7, which comprises the following steps:
(1) preparation of film substrate: purifying and corona or plasma treating the surface of the film base material;
(2) preparation of a release agent: weighing the components according to the weight of the formula of the release agent, adding liquid silicone resin, vinyl silicone oil, a catalyst, an inhibitor, a tackifier and an organic solvent into a reactor, stirring for 60min at the rotating speed of 400rpm, uniformly mixing, adding hydrogen-containing silicone oil, stirring for 60min at the rotating speed of 800rpm, and uniformly mixing;
(3) coating a release agent on the surface of the film base material treated in the step (1) and drying, wherein the wet coating amount of the release agent is 3g/m2-15g/m2The drying temperature is 80-150 ℃;
(4) and rolling and packaging the dried release film.
9. The method for preparing the release film with medium release force and high residual adhesion according to claim 8, is characterized in that: in the preparation method, the surface purification of the film base material in the step (1) is to remove surface dust by using a dust adhering roller; corona or plasma treated films having a dyne value of greater than or equal to 50 dynes.
10. The method for preparing the release film with medium release force and high residual adhesion according to claim 9, is characterized in that: in the preparation method, the drying in the step (3) is carried out by adopting sectional heating, the speed of a dryer is 20m/min-80m/min, the sectional heating is 80 ℃, 100 ℃, 120 ℃, 150 ℃, and the temperature of a final cooling zone is 130 ℃.
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| CN115160616A (en) * | 2022-07-06 | 2022-10-11 | 苏州市星辰科技有限公司 | Special release film for anisotropic conduction and preparation method |
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