A kind of organic silicon release film and preparation method thereof

By preparing the epoxyl -based fluorophytic silicide as a ionizer, it is mixed with the curing agent and acid catalyst to form a solidar with a three -dimensional associative structure, which solves the stable The lack of nature and adhesion realizes better adhesion and mechanical stability, and meets the needs of long -term use and durability.

CN119176971BActive Publication Date: 2025-01-28SHANDONG JINSHOUFENG NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202411701998.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-26
Publication Date
2025-01-28
Estimated Expiration
2044-11-26

AI Technical Summary

Technical Problem

The existing fluorosilic release agents have shortcomings in terms of stability and anchoring properties, and their adhesion to the substrate is low, making it difficult to meet the needs of long-term use and durability.

Method used

By preparing fluorophythel ether as a modified monomer, combined with silicon hydrogen bonus and tetrahydrial tetrahydride tetraxane reactions, the epoxyl epoxy -based fluorophytic silicoxane is prepared, and The catalyst is mixed with a separate agent, coated on the PE film, forming curing agapus with a three -dimensional connection structure, which improves its adhesion and stability.

Benefits of technology

A better adhesion and mechanical stability are realized, the stability of the ionizing membrane and the performance of hydrophobic oil and oil and oil are improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of release film preparation, and specifically relates to an organosilicon release film and a preparation method thereof, wherein a terminal epoxy-containing fluorinated polysiloxane is used as a release agent main agent, and is mixed with a curing agent and an acid catalyst to form a release agent, wherein the mass ratio of the terminal epoxy-containing fluorinated polysiloxane, the curing agent, and the acid catalyst is 8:1.5~1.8:0.8~1; a film coating rod is used to coat the diluted release agent on a PE substrate, and the film is baked at 80°C for 2 minutes, and then cured at 60°C for 36 hours, and the release agent is cured on the PE film to form a film to obtain a release film. In the present invention, the epoxy group in the terminal epoxy-containing fluorinated polysiloxane reacts with the curing agent to generate a cured product with a three-dimensional cross-linked structure, and a thin film is formed on the surface of the PE film, which has better adhesion to the release film.
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Description

Technical Field

[0001] The invention belongs to the technical field of release film preparation, and particularly relates to an organosilicon release film and a preparation method thereof. Background Art

[0002] Release film is a film with anti-sticking effect. It has no adhesion or slight adhesion to certain materials under certain conditions. Commonly used release films include silicone release film, fluorine release film, non-silicone release film, etc. Among them, silicone release film has become one of the most popular release materials in current research due to its good peeling force, heat resistance and stability, and its low cost makes it widely used.

[0003] Fluorine atoms have strong electronegativity, and the fluorine nucleus has a strong binding effect on extranuclear electrons and bonding electron clouds. The polarizability of the CF bond is low, so the intermolecular force of fluorine-containing polymers is low, showing extremely low surface free energy, and it is difficult to be wetted or adhered by liquids or solids. Fluorine-containing polymers also have good stability, heat resistance and weather resistance.

[0004] However, although the existing fluorosilicone release agent has low release force, its stability and anchoring property are poor. CN107619479A discloses a fluorosilicone release agent and a preparation method thereof. This invention provides a silane-modified polymer and a preparation method thereof that is easy to use and does not require an anchoring agent, so as to ensure long-term use and durability. However, the disadvantage is that the adhesion between the release agent and the substrate is low. Although the fluorosilicone release agent itself has excellent anti-adhesion properties, sometimes it may be necessary to further improve its adhesion. Summary of the invention

[0005] The object of the present invention is to provide a silicone release film and a preparation method thereof to solve the problems raised in the above background technology.

[0006] In order to achieve the above technical objectives, the technical solution of the present invention is:

[0007] A method for preparing a silicone release film comprises the following steps:

[0008] S1. Preparation of the main release agent;

[0009] Fluorinated styrene ether was prepared from trifluoropropanol, sodium hydride and pentafluorostyrene under nitrogen protection.

[0010] The fluorinated styrene ether is used as a modified monomer and reacted with tetramethyltetrahydrocyclotetrasiloxane by hydrosilylation to prepare fluorinated cyclosiloxane;

[0011] The fluorinated cyclosiloxane and octamethylcyclotetrasiloxane are used as polymerization monomers, tetramethyldihydrodisiloxane is used as a capping agent, and trifluoromethanesulfonic acid is used as a catalyst, and the polymerization reaction is carried out at 75° C. for 8 hours to obtain a hydrogen-terminated fluorinated polysiloxane;

[0012] Using allyl glycidyl ether as a modified monomer, reacting with the hydrogen-terminated fluorinated polysiloxane through hydrosilylation to prepare an epoxy-terminated fluorinated polysiloxane;

[0013] S2. Preparation of release agent;

[0014] The terminal epoxy-containing fluorinated polysiloxane is used as a main agent of a release agent, and is mixed with a curing agent and an acid catalyst to form a release agent, wherein the mass ratio of the terminal epoxy-containing fluorinated polysiloxane, the curing agent, and the acid catalyst is 8:1.5-1.8:0.8-1;

[0015] S3, preparation of release film;

[0016] A PE film is used as a substrate, and the surface of the substrate is cleaned with deionized water and ethanol. After drying, the PE film is subjected to ultraviolet irradiation, and then the release agent is diluted with a diluent to a solution with a mass fraction of 5%, and the diluted release agent is coated on the PE substrate, baked at 80°C for 2 minutes, and then cured at 60°C for 36 hours. The release agent is cured on the PE film to obtain a release film, wherein the thickness of the cured film of the release agent is 1.5~3μm.

[0017] As an improvement, in step S1, the preparation method of the fluorinated styrene ether is specifically as follows: dissolving sodium hydride in a three-necked flask containing tetrahydrofuran, slowly dropping trifluoropropanol into the three-necked flask under nitrogen protection, reacting at room temperature for 1 hour, then cooling to 0°C, adding a tetrahydrofuran solution containing pentafluorostyrene into the three-necked flask, continuing to react at 0°C for 1 hour, then heating under reflux at 70°C for 19 hours, after the reaction is completed, cooling the reaction solution to room temperature, then quenching with ice water, washing with saturated brine, and then extracting with anhydrous ether three times, combining the organic phases, adding anhydrous sodium sulfate thereto to dry and remove the organic solvent, and finally purifying the residue by silica gel column chromatography to obtain the fluorinated styrene ether;

[0018] The molar ratio of the trifluoropropanol to the pentafluorostyrene is 1.1:1.

[0019] As a further improvement, in step S1, the preparation method of the fluorinated cyclosiloxane is specifically as follows: taking the fluorinated styrene ether into a dry three-necked flask, adding tetramethyltetrahydrocyclotetrasiloxane, 5 mL of solvent 1,3-bis(trifluoromethyl)benzene and 1 mL of platinum catalyst, placing the three-necked flask in an oil bath, heating to 80° C., reacting for 12 hours, and after the reaction is completed, distilling off the solvent to obtain the fluorinated cyclosiloxane;

[0020] The molar ratio of the fluorine-containing styrene ether to the tetramethyltetrahydrocyclotetrasiloxane is 5:1.

[0021] As a further improvement, in step S1, the preparation method of the terminal hydrogen-containing fluorine-containing polysiloxane is specifically as follows: the fluorine-containing cyclosiloxane, octamethylcyclotetrasiloxane and tetramethyldihydrodisiloxane are placed in a dry three-necked flask, the system is sealed and filled with nitrogen, the three-necked flask is placed in an oil bath under nitrogen protection, the temperature is raised to 75°C, stirred for 30 minutes to make the system temperature constant, and then the catalyst trifluoromethanesulfonic acid is added, and the reaction is continued for 8 hours. After the reaction is completed, it is cooled to room temperature, and then n-heptane is added to neutralize the trifluoromethanesulfonic acid in the system, and then filtered and distilled to remove the solvent, and the pressure is reduced at 180°C for 30 minutes to obtain the terminal hydrogen-containing fluorine-containing polysiloxane.

[0022] As a further improvement, in step S1, the preparation method of the terminal epoxy fluorinated polysiloxane is specifically as follows: taking the terminal hydrogen fluorinated polysiloxane into a dry three-necked flask, adding allyl glycidyl ether, 5 ppm Karstedt catalyst and 5 mL 1,3-bis(trifluoromethyl)benzene thereto, and then placing the three-necked flask in an oil bath, heating to 80°C, reacting for 10 hours, and distilling at 116°C after the reaction to obtain the terminal epoxy fluorinated polysiloxane, wherein the molar ratio of the terminal hydrogen fluorinated polysiloxane to the allyl glycidyl ether is 1:1.1.

[0023] As a further improvement, the molar ratio of the fluorinated cyclosiloxane to the octamethylcyclotetrasiloxane is 7:3, the amount of the catalyst trifluoromethanesulfonic acid added is 5% of the total molar amount of the fluorinated cyclosiloxane and the octamethylcyclotetrasiloxane, and the amount of the tetramethyldihydrodisiloxane added is 2% of the total molar amount of the fluorinated cyclosiloxane and the octamethylcyclotetrasiloxane.

[0024] As a further improvement, in step S2, the acid catalyst is benzoic acid or phenol, and the curing agent is ethylamine or n-butylamine.

[0025] As a further improvement, in step S3, the diluent is n-heptane.

[0026] The invention also provides an organic silicon release film.

[0027] The relevant reaction equation in the present invention is as follows:

[0028] Preparation of fluorinated styrene ethers;

[0029] ;

[0030] Preparation of fluorinated cyclosiloxanes;

[0031] ;

[0032] Where Rf is ;

[0033] Preparation of hydrogen-terminated fluorinated polysiloxane:

[0034] ;

[0035] Preparation of epoxy-terminated fluorinated polysiloxane;

[0036] .

[0037] Due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0038] The present invention provides a bulk release film, wherein terminal epoxy-containing fluorinated polysiloxane, a curing agent and an acid catalyst are mixed in a specific proportion to form a release agent, which is coated on the surface of a PE film. The epoxy groups in the terminal epoxy-containing fluorinated polysiloxane react with the curing agent to generate a cured product with a three-dimensional cross-linked structure, and a thin film is formed on the surface of the PE film, which has better adhesion to the release film.

[0039] The present invention introduces a benzene ring into the side chain of the terminal epoxy fluorinated polysiloxane, and because the benzene ring has high mechanical strength, the mechanical stability of the release agent and the adhesion between the release agent and the surface of the PE film are further improved.

[0040] The invention adopts trifluoropropanol and pentafluorostyrene to react to obtain fluorinated styrene ether, and then introduces the fluorinated styrene ether as a modified monomer into the side chain of the terminal epoxy fluorinated polysiloxane, the fluorinated styrene ether side chain enables the release agent to have better hydrophobic and oleophobic properties, and improves the stability of the release agent, the introduction of the benzene ring on the side chain can make the arrangement of the fluorinated chain segment more orderly through the π-π interaction of the benzene ring, and the attachment on the surface of the PE film is more uniform, and the fluorine atoms on the benzene ring have an important promoting effect on the hydrophobic and oleophobic properties and thermal stability of the release agent. DETAILED DESCRIPTION

[0041] The technical scheme of the present invention will be clearly and completely described below in conjunction with specific embodiments, but it will be appreciated by those skilled in the art that the following described embodiments are part of embodiments of the present invention, rather than all embodiments, and are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work, all belong to the scope of protection of the present invention. If specific conditions are not indicated in the embodiments, they are carried out according to normal conditions or conditions recommended by the manufacturer. If the manufacturer is not indicated in the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0042] Embodiment 1 A method for preparing a release agent comprises the following steps:

[0043] S1. Preparation of the main release agent;

[0044] Preparation of fluorinated styrene ether: 0.8 g of sodium hydride was dissolved in a three-necked flask containing 55 mL of tetrahydrofuran. Under nitrogen protection, 1.255 g of trifluoropropanol was slowly added to the three-necked flask, and the mixture was reacted at room temperature for 1 h. The mixture was then cooled to 0°C. A tetrahydrofuran solution containing 1.941 g of pentafluorostyrene was added to the three-necked flask, and the mixture was reacted at 0°C for 1 h. The mixture was then heated under reflux at 70°C for 19 h. After the reaction was completed, the reaction solution was cooled to room temperature, quenched with ice water, washed with saturated brine, and then extracted with anhydrous ether for three times. The organic phases were combined, and then dried with anhydrous sodium sulfate to remove the organic solvent. Finally, the residue was purified by silica gel column chromatography to obtain fluorinated styrene ether, wherein the molar ratio of trifluoropropanol to pentafluorostyrene was 1.1:1.

[0045] Preparation of fluorinated cyclosiloxane: The fluorinated styrene ether prepared above was placed in a dry three-necked flask, 0.481 g of tetramethyltetrahydrocyclotetrasiloxane, 5 mL of solvent 1,3-bis(trifluoromethyl)benzene and 1 mL of platinum catalyst were added, the three-necked flask was placed in an oil bath, the temperature was raised to 80°C, and the reaction was carried out for 12 hours. After the reaction was completed, the solvent was distilled off to obtain fluorinated cyclosiloxane, wherein the molar ratio of fluorinated styrene ether to tetramethyltetrahydrocyclotetrasiloxane was 5:1;

[0046] Preparation of hydrogen-terminated fluorinated polysiloxane: The above-prepared fluorinated cyclosiloxane, 0.254 g of octamethylcyclotetrasiloxane, and 7.68 mg of tetramethyldihydrodisiloxane were placed in a dry three-necked flask, the system was sealed and filled with nitrogen, and the three-necked flask was placed in an oil bath under nitrogen protection, the temperature was raised to 75°C, stirred for 30 min, the system temperature was kept constant, and then 0.02 g of catalyst trifluoromethanesulfonic acid was added, and the reaction was continued for 8 h. After the reaction was completed, it was cooled to room temperature, and then Adding n-heptane to neutralize trifluoromethanesulfonic acid in the system, then filtering and distilling to remove the solvent, and then reducing the pressure at 180° C. for 30 minutes to obtain terminal hydrogen-containing fluorine-containing polysiloxane, wherein the molar ratio of fluorine-containing cyclosiloxane to octamethylcyclotetrasiloxane is 7:3, the amount of catalyst trifluoromethanesulfonic acid added is 5% of the total molar amount of fluorine-containing cyclosiloxane and octamethylcyclotetrasiloxane, and the amount of tetramethyldihydrodisiloxane added is 2% of the total molar amount of fluorine-containing cyclosiloxane and octamethylcyclotetrasiloxane;

[0047] Preparation of epoxy-terminated fluorinated polysiloxane: The prepared hydrogen-terminated fluorinated polysiloxane is placed in a dry three-necked flask, and an excess of allyl glycidyl ether, 5 ppm Karstedt catalyst and 5 mL 1,3-bis(trifluoromethyl)benzene are added thereto. The three-necked flask is then placed in an oil bath, heated to 80° C., and reacted for 10 hours. After the reaction is completed, the mixture is distilled at 116° C. to obtain epoxy-terminated fluorinated polysiloxane. Specifically, the molar ratio of allyl glycidyl ether to hydrogen-terminated fluorinated polysiloxane may be 1.1:1.

[0048] S2. Preparation of release agent;

[0049] The prepared terminal epoxy fluorinated polysiloxane is used as the main agent of the release agent and mixed with a curing agent and an acid catalyst to form a release agent, wherein the mass ratio of the terminal epoxy fluorinated polysiloxane, the curing agent and the acid catalyst is 8:1.5:0.8, wherein the acid catalyst is phenol and the curing agent is ethylamine.

[0050] Example 2 This example prepares a release film, and the specific steps are: using a PE film as a substrate, cleaning the surface of the substrate with deionized water and ethanol, then wiping it clean with a non-woven fabric, drying it naturally, and then irradiating the PE film with ultraviolet light for 10 minutes, and then using n-heptane as a diluent to dilute the release agent prepared in Example 1 into a solution with a mass fraction of 5%, using a coating rod to coat the diluted release agent on the PE substrate, baking at 80°C for 2 minutes, and then curing at 60°C for 36 hours. The release agent is cured on the PE film to form a film to obtain a release film, wherein the thickness of the cured film of the release agent is 1.5μm.

[0051] Example 3 This example provides a method for preparing a release agent. The specific steps are the same as those of Example 1, except that in this example, the mass ratio of the epoxy-terminated fluorinated polysiloxane, the curing agent, and the acid catalyst is 8:1.8:1, wherein the acid catalyst is benzoic acid and the curing agent is n-butylamine.

[0052] Example 4 This example provides a method for preparing a release film. The specific steps are the same as those of Example 2, except that the thickness of the film formed by curing the release agent in this example is 3 μm.

[0053] Example 5 The hydrophobic and oleophobic properties of the release agent in Example 1 were evaluated by measuring the contact angle of the release film prepared in Example 2. The specific method is as follows:

[0054] Water and oil were dropped on the release film prepared in Example 2, and then measured by a fully automatic contact angle measuring instrument, wherein water and oil were respectively taken at five different positions, and each position was measured once to obtain the water contact angle and oil contact angle of the release film. The volume of the test water droplet and oil droplet was 2 μL, and the test temperature was 25°C. The experimental results are shown in Table 1. Then, the surface free energy was calculated by the Owens-Wendt geometric mean method, and the surface energy of the release film was 14.357 mJ / m 2 In this embodiment, paraffin oil is used as the oil.

[0055]

[0056] It can be seen from Table 1 that the release film prepared in the present invention has good hydrophobic and oleophobic properties and high stability.

[0057] Example 6 In this example, the release performance of the release film prepared in Example 2 was tested.

[0058] The specific steps of the 180° peeling force test are as follows: a clean PE film without a release agent, a common release film on the market, and the release film prepared in Example 2 are tested for 180° peeling force using an electronic universal tester, and a release force test tape is respectively attached to a clean PE film without a release agent, a common release film, and the release film prepared in Example 2, and the release force test tape is cut into 25 mm × 200 mm strips, and a standard rolling roller is used to roll back and forth three times, and the test is performed after standing for 20 minutes. The test method of GB-2792-1998 adhesive tape peeling strength is adopted, and the test is performed using an electronic universal tester, and the peeling speed is set to 300 mm / min.

[0059] The experimental results show that the peeling force of the clean PE film without release agent is relatively large, which is 3.45N, while the peeling force of the ordinary release film is reduced to 8.98×10 -3 N, while the peeling force of the release film prepared in Example 2 was reduced to 2.23×10 -3 N, better release performance.

[0060] Silicon residual adhesion rate test: In the release film of organic silicone material, the silicon residual adhesion rate is an important parameter for measuring the performance of the coating. In this embodiment, the FINAT test method is used to detect the amount of ordinary release film and the release film in Example 2 transferred from the PE film substrate after the above peeling force test. The tape in the above peeling test is re-adhered to a clean PE film substrate for a 180° peeling test, and compared with the unused tape, the residual adhesion rate of the ordinary release film is 75.3%, while the residual adhesion rate of the release film prepared in Example 2 is 88.3%. This is because the release film prepared in the present invention contains more fluorine, the surface energy of the coating is reduced, the residual adhesion rate is increased, and the release performance is better.

[0061] The effect of the number of peeling times on the water contact angle of the coating was tested. The specific method was as follows: a release force test tape was attached to a common release film and the release film prepared in Example 2, respectively, and the release film was cut into 25 mm × 200 mm strips. A standard rolling roller was used to roll the release force test tape back and forth three times, and then the release force test tape was peeled off. Then, water was dripped onto the peeled release film, and the water contact angle after peeling was measured. Five different positions were taken, each position was measured once, and the average value of the five times was calculated. Then, the above steps were repeated, and the two release films were peeled off multiple times. The water contact angle was measured after each peeling. The experimental results are shown in Table 2.

[0062]

[0063] According to the data in Table 2, it can be seen that under the same number of peeling times, the water contact angle of the release film of the present invention is greater than that of the ordinary release film, and the water contact angle of the ordinary release film has been reduced to 100° after peeling 10 times, while the water contact angle of the release film prepared by the present invention is reduced to 100° after peeling 14 times. With the increase of the number of peeling times, the water contact angles of the ordinary release film and the release film of the present invention both show a downward trend. This is because as the coating is peeled off, the surface integrity and surface fluorine content of the coating continue to decrease, and more defects make the coating more easily transferred by the tape, so the water contact angle shows a downward trend; however, for the release film prepared by the present invention, the amplitude of the decrease in the water contact angle is not very large with the increase in the number of peeling times before peeling 10 times. After peeling 10 times, the amplitude of the decrease in the water contact angle begins to increase with the increase in the number of peeling times, while the amplitude of the decrease in the water contact angle of the ordinary release film is relatively large with the increase in the number of peeling times.

[0064] This is because epoxy groups are introduced into the main agent of the release agent used in the present invention. During the curing process, the epoxy groups react with the curing agent to generate a cured product with a three-dimensional cross-linked structure, which has better adhesion to the PET film substrate.

[0065] By introducing benzene rings on the side chains, the mechanical stability of the release agent is improved and the residual adhesion rate is reduced. The fluorinated styrene ether side chains in the main agent of the release agent make the release film have better hydrophobic and oleophobic properties and improve the stability of the release film. In addition, through the π-π interaction of the benzene ring, the arrangement of the fluorinated chain segments is more orderly and the adhesion to the PE film surface is more uniform.

[0066] The specific implementation of the present invention described above does not constitute a limitation on the protection scope of the present invention. Any other corresponding changes and modifications made based on the technical concept of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A method for preparing a silicone release film, characterized in that: The following steps are involved: S1. Preparation of the main release agent; Fluorinated styrene ether was prepared from trifluoropropanol, sodium hydride and pentafluorostyrene under nitrogen protection. The fluorinated styrene ether is used as a modified monomer and reacted with tetramethyltetrahydrocyclotetrasiloxane by hydrosilylation to prepare fluorinated cyclosiloxane; The fluorinated cyclosiloxane and octamethylcyclotetrasiloxane are used as polymerization monomers, tetramethyldihydrodisiloxane is used as a capping agent, and trifluoromethanesulfonic acid is used as a catalyst, and the polymerization reaction is carried out at 75° C. for 8 hours to obtain a hydrogen-terminated fluorinated polysiloxane; Using allyl glycidyl ether as a modified monomer, reacting with the hydrogen-terminated fluorinated polysiloxane through hydrosilylation to prepare an epoxy-terminated fluorinated polysiloxane; S2. Preparation of release agent; The terminal epoxy-containing fluorinated polysiloxane is used as a main agent of a release agent, and is mixed with a curing agent and an acid catalyst to form a release agent, wherein the mass ratio of the terminal epoxy-containing fluorinated polysiloxane, the curing agent, and the acid catalyst is 8:1.5-1.8:0.8-1; S3, preparation of release film; A PE film is used as a substrate, and the surface of the substrate is cleaned with deionized water and ethanol. After drying, the PE film is subjected to ultraviolet irradiation, and then the release agent is diluted with a diluent to a solution with a mass fraction of 5%, and the diluted release agent is coated on the PE substrate, baked at 80°C for 2 minutes, and then cured at 60°C for 36 hours. The release agent is cured on the PE film to obtain a release film, wherein the thickness of the cured film of the release agent is 1.5~3μm.

2. The method for preparing a silicone release film according to claim 1, characterized in that: In step S1, the preparation method of the fluorinated styrene ether is specifically as follows: dissolving sodium hydride in a three-necked flask containing tetrahydrofuran, slowly dropping trifluoropropanol into the three-necked flask under nitrogen protection, reacting at room temperature for 1 hour, then cooling to 0°C, adding a tetrahydrofuran solution containing pentafluorostyrene into the three-necked flask, continuing to react at 0°C for 1 hour, then heating under reflux at 70°C for 19 hours, after the reaction is completed, cooling the reaction solution to room temperature, then quenching with ice water, washing with saturated brine, and then extracting with anhydrous ether three times, combining the organic phases, adding anhydrous sodium sulfate thereto to dry and remove the organic solvent, and finally purifying the residue by silica gel column chromatography to obtain the fluorinated styrene ether; The molar ratio of the trifluoropropanol to the pentafluorostyrene is 1.1:

1.

3. The method for preparing a silicone release film according to claim 1, characterized in that: In step S1, the preparation method of the fluorinated cyclosiloxane is specifically as follows: taking the fluorinated styrene ether into a dry three-necked flask, adding tetramethyltetrahydrocyclotetrasiloxane, 5 mL of solvent 1,3-bis(trifluoromethyl)benzene and 1 mL of platinum catalyst, placing the three-necked flask in an oil bath, heating to 80° C., reacting for 12 hours, and after the reaction is completed, distilling off the solvent to obtain the fluorinated cyclosiloxane; The molar ratio of the fluorine-containing styrene ether to the tetramethyltetrahydrocyclotetrasiloxane is 5:

1.

4. The method for preparing a silicone release film according to claim 1, characterized in that: In step S1, the preparation method of the terminal hydrogen-containing fluorine-containing polysiloxane is specifically as follows: the fluorine-containing cyclosiloxane, octamethylcyclotetrasiloxane and tetramethyldihydrodisiloxane are placed in a dry three-necked flask, the system is sealed and filled with nitrogen, the three-necked flask is placed in an oil bath under nitrogen protection, the temperature is raised to 75°C, stirred for 30 minutes, the system temperature is kept constant, and then the catalyst trifluoromethanesulfonic acid is added, and the reaction is continued for 8 hours. After the reaction is completed, it is cooled to room temperature, and then n-heptane is added to neutralize the trifluoromethanesulfonic acid in the system, and then filtered and distilled to remove the solvent, and the pressure is reduced at 180°C for 30 minutes to obtain the terminal hydrogen-containing fluorine-containing polysiloxane.

5. The method for preparing a silicone release film according to claim 1, characterized in that: In step S1, the preparation method of the terminal epoxy fluorinated polysiloxane is specifically as follows: taking the terminal hydrogen fluorinated polysiloxane in a dry three-necked flask, adding allyl glycidyl ether, 5ppm Karstedt catalyst and 5mL 1,3-bis(trifluoromethyl)benzene thereto, and then placing the three-necked flask in an oil bath, heating to 80°C, reacting for 10h, and distilling at 116°C after the reaction to obtain the terminal epoxy fluorinated polysiloxane, wherein the molar ratio of the terminal hydrogen fluorinated polysiloxane to the allyl glycidyl ether is 1:1.

1.

6. The method for preparing an organosilicon release film according to claim 4, characterized in that: The molar ratio of the fluorinated cyclosiloxane to the octamethylcyclotetrasiloxane is 7:3, the amount of the catalyst trifluoromethanesulfonic acid added is 5% of the total molar amount of the fluorinated cyclosiloxane and the octamethylcyclotetrasiloxane, and the amount of the tetramethyldihydrodisiloxane added is 2% of the total molar amount of the fluorinated cyclosiloxane and the octamethylcyclotetrasiloxane.

7. The method for preparing a silicone release film according to claim 1, characterized in that: In step S2, the acid catalyst is benzoic acid or phenol, and the curing agent is ethylamine or n-butylamine.

8. The method for preparing an organosilicon release film according to claim 1, characterized in that: In step S3, the diluent is n-heptane.

9. A release film prepared by the method for preparing an organosilicon release film according to any one of claims 1 to 8.

Citation Information

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