High-stability release agent, preparation method thereof, release liquid and release film

Abstract

The invention discloses a high-stability release agent, a preparation method thereof, a release liquid and a release film. The high-stability release agent is prepared from the following raw material components in parts by weight: 5-20 parts of dihydroxyl-terminated long-chain-chain organic silicone oil, 1-4 parts of benzoate and 0.05-0.2 part of a solid acid catalyst. The preparation raw materials of the dihydroxyl-terminated long-chain branch organic silicone oil comprise the following components in parts by weight: 0.5-2 parts of dimethoxyalkylsilane; 10 to 100 parts of hydroxyl-terminated silicone oil; 0.1 to 0.4 part of a solid acid catalyst; and 0.8 to 2.5 parts of vinyl dimethoxy silane. According to the high-stability release agent disclosed by the invention, low-polarity long-chain siloxane is introduced into a silicone oil main chain, so that the isolation effect of an interface layer can be improved; a benzyl ester hard chain segment is connected to a silicone oil chain, so that the body structural strength can be improved, and the self-adsorption phenomenon is prevented.

Description

Technical Field

[0001] The present invention relates to the field of release materials, and particularly to a high-stability release agent, a preparation method thereof, a release liquid and a release film. Background Art

[0002] Release materials are functional materials with excellent isolation performance. By virtue of their extremely low surface tension and good flatness on the surface, they can effectively reduce the adsorption and wettability of adhesive materials to the film surface and maintain a good unwinding and peeling effect. Therefore, when producing and preparing adhesive materials, the adhesive materials can be first coated and adhered to the release film, and the release film is used to protect the adhesive layer. After the release film is peeled off, various applications can be carried out on the adhesive materials. Therefore, release films are extremely widely used in industrial production.

[0003] 3. OCA optical adhesive is an adhesive commonly used for bonding optical and electronic components. In devices such as display screens, OCA optical adhesives are widely used for bonding liquid crystal screens and touch screens. In 2023, the demand for China's OCA optical adhesive industry was 48.572 million square meters, and the market scale was 8.409 billion yuan, showing strong market demand and growth potential. With the popularization of consumer electronic products such as smart phones and tablet computers, as well as the rapid development of industries such as medical devices and automobiles, the demand for OCA optical adhesives continues to grow. China is the largest and most important production and consumption market for OCA optical adhesives in the world. OCA optical adhesives have the advantages of being colorless and transparent, having high adhesion, high wettability, high transmittance, low haze, and good yellowing resistance. As a release film that plays a protective and isolating role in the OCA production process, it plays a crucial role in the production quality of OCA products. Due to the characteristics of low modulus and high viscosity of the OCA adhesive film, it is necessary to ensure that when peeling off from the release film, a very low peeling force is maintained to prevent damage to the main body structure of the OCA adhesive film. However, currently, the peeling force of the release films on the market has an obvious climbing phenomenon after standing for a period of time after being adhered to the OCA release film, resulting in abnormal peeling during the use of OCA, greatly shortening the inventory time of the OCA adhesive film. CN202411062594.9 discloses a preparation method of a release film with good high-temperature heat insulation performance, but the disadvantage is that fluorine-containing substances are used therein, and fluorine elements may involve carcinogenic risks in 3C electronic products and are not suitable for the use of OCA adhesive films. CN115322426A discloses a preparation method of a release film with good wear resistance, but the polyurethane therein is a physical blending filler, which will reduce the flatness of the surface layer of the release film and increase the surface energy of the release layer, resulting in the disadvantage of high peeling force.

[0004] The basic structure of the release film is a PET base film layer + a release layer. The release layer provides the release and isolation effect, and the PET base film provides the supporting role. The current mainstream release agent in the market is linear organosilicon oil. Through cross-linking and curing between molecular chains, a network-structured silicone release layer is formed. The extremely low surface tension of the silicone polymer is used to provide the isolation effect. The thickness and surface tension of the release layer determine the wetting and adsorption performance of the release layer on the adhesive material. However, due to the low modulus of the silicone coating, when the coating is thick, it will produce a reverse wetting and adsorption effect on the attached material, and at this time, the isolation effect cannot be reflected. When the coating is too thin, the coverage of the release layer on the PET base film and the wetting and isolation performance on the adhesive layer decrease, and a good isolation effect cannot be achieved, making it difficult to meet the application requirements of low release force and high isolation stability.

[0005] The existing main methods to reduce the peeling force of the release film and improve the isolation stability are as follows: ① Increase the thickness of the silicone release layer to make the release agent fully cover the PET base film, and at the same time add a large amount of silicon particle fillers internally to prevent the adsorption phenomenon of the release layer. However, this method will introduce more silicon particle fillers, making the surface layer of the release film rougher, and after the thickness reaches saturated coverage, increasing the thickness further will not have a corresponding increase. ② Add non-reactive light peeling additives to the silicone release layer. Since such substances do not have a chemical bonding force with the main body of the release agent, after addition, over time, they are extremely likely to migrate to the surface of the release layer, resulting in a significant decrease in the residue of the release film and fluctuations in the peeling force, thereby affecting the stability of use. Summary of the Invention

[0006] The technical problem to be solved by the present invention is to provide a high-stability release agent, its preparation method, release liquid and release film in view of the above-mentioned deficiencies in the prior art. The present invention can maintain an extremely low climbing over time while providing a low peeling force, effectively solving the above problems.

[0007] To achieve the above object, the technical solution adopted by the present invention is: In the first aspect of the present invention, a high-stability release agent is provided, which includes the following raw material components by weight: 5-20 parts of long-chain branched organosilicon oil with double hydroxyl ends, 1-4 parts of benzoate, and 0.05-0.2 parts of solid acid catalyst;

[0008] Among them, the preparation raw materials of the long-chain branched organosilicon oil with double hydroxyl ends include by weight:

[0009] 0.5-2 of dimethoxyalkylsilane;

[0010] 10-100 parts of hydroxyl-terminated silicone oil;

[0011] 0.1-0.4 of solid acid catalyst;

[0012] 0.8 - 2.5 parts of vinyl dimethoxysilane.

[0013] Preferably, the dimethoxyalkylsilane is one or more of: octadecyl dimethoxysilane, diisopropyl dimethoxysilane, hexadecyl dimethoxysilane, dodecyl dimethoxysilane.

[0014] Preferably, the vinyl dimethoxysilane is one or more of: vinyl ethyl dimethoxysilane, vinyl propyl dimethoxysilane, vinyl butyl dimethoxysilane, vinyl methyl sil (diol) diacetate.

[0015] Preferably, the benzoate is one or more of: methyl benzoate, ethyl benzoate, butyl benzoate.

[0016] Preferably, the number average molecular weight of the hydroxyl-terminated silicone oil is: 4000 - 20000 g / mol.

[0017] Preferably, the long-chain branched organosilicone oil terminated with dihydroxy groups is prepared by the following method:

[0018] Mix the dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, react under heating, then add vinyl methyl dimethoxysilane and react. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst, and dehydrate the obtained product under negative pressure and heating to obtain the long-chain branched organosilicone oil terminated with dihydroxy groups.

[0019] Preferably, the long-chain branched organosilicone oil terminated with dihydroxy groups is prepared by the following method:

[0020] Mix the dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, heat up to 50 - 70 °C, react at a constant temperature for 2 - 8 h, then add vinyl methyl dimethoxysilane and react at a constant temperature for 2 - 8 h. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst, and dehydrate the obtained product under a negative pressure of -0.03 mpa to -0.1 mpa and at 70 - 90 °C for 1 - 4 h to obtain the long-chain branched organosilicone oil terminated with dihydroxy groups.

[0021] In the second aspect of the present invention, a preparation method of the high-stability release agent as described above is provided, including the following steps:

[0022] Mix the long-chain branched organosilicone oil terminated with dihydroxy groups, benzoate, and solid acid catalyst evenly, heat up to 80 °C, react in a negative pressure environment of -0.03 mpa to -0.1 mpa for 6 h, filter by suction to separate and remove the solid acid catalyst, and obtain the high-stability release agent.

[0023] In a third aspect of the present invention, there is provided a release liquid obtained by uniformly mixing the following raw materials by weight:

[0024] 100 parts of the high-stability release agent as described above;

[0025] 0.8 - 2.5 parts of hydrogen-containing silicone oil;

[0026] 0.3 - 1.2 parts of anchoring agent;

[0027] 0.05 - 0.2 parts of Karstedt's platinum catalyst;

[0028] 12 - 50 parts of solvent;

[0029] In a fourth aspect of the present invention, there is provided a release film prepared by the following method: The release liquid as described above is uniformly coated on a substrate and dried to obtain the release film.

[0030] The beneficial effects of the present invention are:

[0031] The present invention provides a high-stability release agent, a release liquid, and a release film. The high-stability release agent of the present invention introduces a low-polarity long-chain siloxane into the silicone oil main chain, which can improve the isolation effect of the interface layer; a benzyl ester hard segment is incorporated into the silicone oil chain, which can improve the strength of the bulk structure and prevent self-adsorption.

[0032] A large number of long-chain linear organosilicon polymers are incorporated into the side chains of the linear organosilicon polymer in the high-stability release agent of the present invention. The prepared long-branched organosilicon polymer as a release agent can provide an extremely low surface tension.

[0033] The high-stability release agent of the present invention uses the design of introducing benzyl ester groups into the molecular chain, which can enhance the modulus of the release layer itself, improve the hardness of the release layer, and prevent the reverse adsorption problem caused by the coating thickness. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is the preparation reaction principle of long-branched organosilicon oil capped with dihydroxy groups and long-branched benzoate organosilicon release agent. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0035] The following further describes the present invention in detail with reference to embodiments, so that those skilled in the art can implement it according to the description in the specification.

[0036] It should be understood that the terms such as "having", "comprising", and "including" used herein do not exclude the presence or addition of one or more other elements or their combinations.

[0037] Unless otherwise specified, the test methods used in the following examples are all conventional methods. Unless otherwise specified, the materials and reagents used in the following examples can all be obtained through commercial channels. For those not specifying specific conditions in the following examples, they are carried out according to conventional conditions or the conditions recommended by the manufacturer. For those reagents or instruments without indicating the manufacturer, they are all conventional products that can be obtained through commercial purchase.

[0038] The present invention provides a high-stability release agent, which comprises the following raw material components by weight: 5-20 parts of a long-chain branched organosilicon oil capped with dihydroxy groups, 1-4 parts of benzoate, and 0.05-0.2 part of a solid acid catalyst;

[0039] Among them, the raw materials for preparing the long-chain branched organosilicon oil capped with dihydroxy groups include by weight:

[0040] 0.5-2 of dimethoxyalkylsilane;

[0041] 10-100 parts of a hydroxyl-terminated silicone oil;

[0042] 0.1-0.4 of a solid acid catalyst;

[0043] 0.8-2.5 parts of vinyl dimethoxysilane.

[0044] In a preferred embodiment, the dimethoxyalkylsilane is one or more of octadecyl dimethoxysilane, diisopropyl dimethoxysilane, hexadecyl dimethoxysilane, and dodecyl dimethoxysilane.

[0045] In a preferred embodiment, the vinyl dimethoxysilane is one or more of vinyl ethyl dimethoxysilane, vinyl propyl dimethoxysilane, vinyl butyl dimethoxysilane, and vinyl methyl silanediol diacetate.

[0046] In a preferred embodiment, the benzoate is one or more of methyl benzoate, ethyl benzoate, and butyl benzoate.

[0047] In a preferred embodiment, the number-average molecular weight (Mn) of the hydroxyl-terminated silicone oil is: 4000-20000 g / mol. For example, the number-average molecular weight is 20000 g / mol, 16000 g / mol, 12000 g / mol, 10000 g / mol, 8000 g / mol, 6000 g / mol, 4000 g / mol, etc.

[0048] In a preferred embodiment, the long-chain branched organosilicon oil capped with dihydroxy groups is prepared by the following method:

[0049] Mix dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, react under heating, then add vinylmethyldimethoxysilane and react. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst. The obtained product is dehydrated under negative pressure and heating to obtain long-chain branched organosilicone oil terminated with dihydroxy groups.

[0050] In a preferred embodiment, the long-chain branched organosilicone oil terminated with dihydroxy groups is prepared by the following method:

[0051] Mix dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, slowly raise the temperature to 50 - 70 °C, react at a constant temperature for 2 - 8 h, then add vinylmethyldimethoxysilane and react at a constant temperature for 2 - 8 h. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst. The obtained product is dehydrated under a negative pressure of -0.03 mpa to -0.1 mpa and at 70 - 90 °C for 1 - 4 h to obtain long-chain branched organosilicone oil terminated with dihydroxy groups.

[0052] In a preferred embodiment, the long-chain branched organosilicone oil terminated with dihydroxy groups is prepared by the following method:

[0053] Mix dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, slowly raise the temperature to 60 °C, react at a constant temperature for 4 h, then add vinylmethyldimethoxysilane and react at a constant temperature for 4 h. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst. The obtained product is dehydrated under a negative pressure of -0.03 mpa to -0.1 mpa and at 80 °C for 2 h to obtain long-chain branched organosilicone oil terminated with dihydroxy groups.

[0054] The present invention also provides a preparation method of a high-stability release agent as above, including the following steps:

[0055] Mix the long-chain branched organosilicone oil terminated with dihydroxy groups, benzoate, and solid acid catalyst evenly, slowly raise the temperature to 80 °C, and react for 6 h in a negative pressure environment of -0.03 mpa to -0.1 mpa. Filter by suction to separate and remove the solid acid catalyst to obtain a long-chain branched benzoate organosilicone release agent, that is, a high-stability release agent.

[0056] The preparation route of the long-chain branched benzoate organosilicone release agent in the present invention is as follows:

[0057] (1) Select dimethoxyalkylsilane, hydroxyl-terminated silicone oil, vinylalkyldimethoxysilane, etc. to react to obtain long-chain branched organosilicone oil terminated with dihydroxy groups (denoted as A);

[0058] (2) Perform transesterification reaction between the long-chain branched organosilicone oil terminated with dihydroxy groups and benzoate to obtain a long-chain branched benzoate organosilicone release agent (i.e., a high-stability release agent);

[0059] The preparation reaction principle of the dihydroxy-terminated long-chain branched organosilicone oil and the reaction principle of further preparing the long-chain branched benzoate organosilicone release agent are as follows Figure 1 shown (where the catalyst is a solid acid catalyst).

[0060] The present invention also provides a release liquid, which is obtained by uniformly mixing the following raw materials by weight:

[0061] 100 parts of the high-stability release agent as described above;

[0062] 0.8 - 2.5 parts of hydrogen-containing silicone oil;

[0063] 0.3 - 1.2 parts of anchoring agent;

[0064] 0.05 - 0.2 parts of Karstedt's platinum catalyst;

[0065] 12 - 50 parts of solvent.

[0066] In a preferred embodiment, the solvent is ethyl acetate.

[0067] The present invention also provides a release film, which is prepared by the following method: The release liquid as described above is uniformly coated on a substrate and dried to obtain the release film.

[0068] The above is the general concept of the present invention. The following provides detailed examples and comparative examples on this basis to further illustrate the present invention.

[0069] In the following examples and comparative examples, the sources of the main raw materials involved are as follows:

[0070] The solid acid catalyst is T-62MP DRY, purchased from Clean Science & Technology (Beijing) Co., Ltd.;

[0071] The hydrogen-containing silicone oil is MY 203, purchased from Anhui Mingyi Silicon Industry Co., Ltd.;

[0072] The anchoring agent is HF86 from Wacker Chemie AG of Germany;

[0073] The Karstedt's platinum catalyst is PC-611, purchased from Shanghai Neutron Star Technology Co., Ltd.;

[0074] Octadecyl dimethoxysilane (Hangzhou Jessica Chemical Co., Ltd.), hexadecyl dimethoxysilane (Hunan Binghang New Materials Co., Ltd.), octamethylcyclotetrasiloxane (Jiangxi BlueStar Silicone Co., Ltd.), vinyl methyl dimethoxysilane (Nanjing Nengde New Materials Technology Co., Ltd.), methyl benzoate (Shandong Yinglang Chemical Co., Ltd.);

[0075] The solvent is ethyl acetate (Aladdin Chemical Reagent);

[0076] PET film (Jiangsu Stdick New Materials Technology Co., Ltd.).

[0077] Example 1

[0078] A high-stability release agent, the preparation method of which comprises the following steps:

[0079] S1. Preparation of dihydroxy-terminated long-chain branched silicone oil:

[0080] By weight, 1 part of dimethoxyoctadecylsilane, 10 parts of terminal hydroxyl silicone oil (Mn=8000), and 0.2 parts of solid acid catalyst were fully mixed, and the temperature was slowly raised to 60°C, and the reaction was carried out at a constant temperature for 4 hours, and then 2 parts of vinylmethyldimethoxysilane were added, and the reaction was carried out at a constant temperature for 4 hours. After the reaction was completed, the obtained silicone oil was placed in a suction filter for suction filtration, and the solid acid catalyst was separated from the silicone oil product. Then, the separated silicone oil was dehydrated at a negative pressure of -0.03 MPa to -0.1 MPa and 80°C for 2 hours to finally obtain a dihydroxy-terminated long-chain branched organic silicone oil;

[0081] S2. By weight, 10 parts of the prepared dihydroxy-terminated long-chain branched silicone oil, 2 parts of methyl benzoate and 0.1 parts of a solid acid catalyst are fully mixed, the temperature is slowly raised to 80°C, and the reaction is maintained in a negative pressure environment of -0.03 MPa to -0.1 MPa for 6 hours, and then the prepared silicone oil is placed in a suction filter for filtration, the solid acid catalyst is separated from the finished silicone oil, and a long-chain branched benzoate silicone release agent, i.e., a high-stability release agent, is obtained.

[0082] Example 2

[0083] A high-stability release agent, the preparation method of which comprises the following steps:

[0084] S1. Preparation of dihydroxy-terminated long-chain branched silicone oil:

[0085] By weight, 1 part of dimethoxyoctadecylsilane, 10 parts of terminal hydroxyl silicone oil (Mn=10000), and 0.2 parts of solid acid catalyst are fully mixed, and then the temperature is slowly raised to 60°C, and the reaction is carried out at a constant temperature for 4 hours, and then 2 parts of vinylmethyldimethoxysilane are continuously added, and the reaction is carried out at a constant temperature for 4 hours. After the reaction is completed, the obtained silicone oil is placed in a suction filter for suction filtration, and the solid acid catalyst is separated from the silicone oil product, and then the separated silicone oil is dehydrated at a negative pressure of -0.03 MPa to -0.1 MPa and 80°C for 2 hours to finally obtain a dihydroxy-terminated long-chain branched organic silicone oil;

[0086] S2. By weight, 10 parts of the prepared dihydroxy-terminated long-chain branched silicone oil, 2 parts of methyl benzoate and 0.1 parts of a solid acid catalyst are fully mixed, the temperature is slowly raised to 80°C, and the reaction is maintained in a negative pressure environment of -0.03 MPa to -0.1 MPa for 6 hours, and then the prepared silicone oil is placed in a suction filter for filtration, the solid acid catalyst is separated from the finished silicone oil, and a long-chain branched benzoate silicone release agent, i.e., a high-stability release agent, is obtained.

[0087] Example 3

[0088] A high-stability release agent, the preparation method of which comprises the following steps:

[0089] S1. Preparation of dihydroxy-terminated long-chain branched silicone oil:

[0090] By weight, 1 part of dodecylmethyldimethoxysilane, 10 parts of terminal hydroxyl silicone oil (Mn=10000), and 0.2 parts of solid acid catalyst are fully mixed, and then the temperature is slowly raised to 60°C, and the reaction is carried out at a constant temperature for 4 hours, and then 2 parts of vinylmethyldimethoxysilane are continuously added, and the reaction is carried out at a constant temperature for 4 hours. After the reaction is completed, the prepared silicone oil is placed in a suction filter for suction filtration, and the solid acid catalyst is separated from the finished silicone oil. Then, the separated silicone oil is dehydrated at a negative pressure of -0.03 MPa to -0.1 MPa and 80°C for 2 hours to finally obtain a dihydroxy-terminated long-chain branched organic silicone oil;

[0091] S2. By weight, 10 parts of the prepared dihydroxy-terminated long-chain branched silicone oil, 2 parts of methyl benzoate and 0.1 parts of a solid acid catalyst are fully mixed, the temperature is slowly raised to 80°C, and the reaction is maintained in a negative pressure environment of -0.03 MPa to -0.1 MPa for 6 hours, and then the prepared silicone oil is placed in a suction filter for filtration, the solid acid catalyst is separated from the finished silicone oil, and a long-chain branched benzoate silicone release agent, i.e., a high-stability release agent, is obtained.

[0092] Example 4

[0093] A high-stability release agent, the preparation method of which comprises the following steps:

[0094] S1. Preparation of dihydroxy-terminated long-chain branched silicone oil:

[0095] By weight, 1 part of diisopropyl dimethoxysilane, 10 parts of hydroxyl-terminated silicone oil (Mn = 10000), and 0.2 part of solid acid catalyst were fully mixed, then slowly heated to 60 °C and reacted at a constant temperature for 4 h. Then, 2 parts of vinyl methyl silanediol diacetate were added, and the reaction was carried out in a negative pressure environment of -0.03 mpa to -0.1 mpa for 6 h. After the reaction, the prepared silicone oil was placed in a suction filter for suction filtration to separate the solid acid catalyst from the silicone oil product. Then, the separated silicone oil was dehydrated at -0.03 mpa to -0.1 mpa and 80 °C for 2 h, and finally, a long-chain branched organosilicone oil with double hydroxyl ends was prepared.

[0096] S2. By weight, 10 parts of the prepared long-chain branched organosilicone oil with double hydroxyl ends, 2 parts of methyl benzoate, and 0.1 part of solid acid catalyst were fully mixed, slowly heated to 80 °C, and reacted in a negative pressure environment of -0.03 mpa to -0.1 mpa for 6 h. Then, the prepared silicone oil was placed in a suction filter for suction filtration to separate the solid acid catalyst from the silicone oil product, and a long-chain branched benzoate organosilicon release agent, namely a high-stability release agent, was prepared.

[0097] Preparation of the release film: In 100 parts of the long-chain branched benzoate organosilicon release agent prepared in the above four examples, 1 part of hydrogen-containing silicone oil, 0.6 part of anchoring agent, 0.1 part of Karstedt platinum catalyst, and 25 parts of ethyl acetate were added, mixed evenly, and uniformly coated onto a PET substrate through a coater. After baking in an oven at 150 °C for 1 min, a silicone release film with uniform and stable peel force was obtained, and the coating thickness was 0.5 μm. The prepared release films were respectively denoted as Examples 1-4.

[0098] Example 5

[0099] In 100 parts of the long-chain branched benzoate organosilicon release agent (prepared in Example 1), 1 part of hydrogen-containing silicone oil, 0.6 part of anchoring agent, 0.1 part of Karstedt platinum catalyst, and 25 parts of ethyl acetate were added, mixed evenly, and uniformly coated onto a PET substrate through a coater. After baking in an oven at 150 °C for 1 min, a silicone release film with uniform and stable peel force was obtained, and the coating thickness was 1 μm.

[0100] Example 6

[0101] In 100 parts of the long-chain branched benzoate organosilicon release agent (prepared in Example 4), 1 part of hydrogen-containing silicone oil, 0.6 part of anchoring agent, Karstedt platinum catalyst, ethyl acetate were fully mixed with the hydrogen-containing silicone oil, and uniformly coated onto a PET substrate through a coater. After baking in an oven at 150 °C for 1 min, a silicone release film with uniform and stable peel force was obtained, and the coating thickness was 1 μm.

[0102] Comparative Example 1

[0103] 100 parts of Wacker's commercially available release agent were evenly coated onto a PET substrate through a coater, and after baking in an oven at 150 °C for 1 min, a silicone release film with uniform and stable peel strength was obtained, and the coating thickness was 0.5 μm.

[0104] Comparative Example 2

[0105] 100 parts of Wacker's commercially available release agent were evenly coated onto a PET substrate through a coater, and after baking in an oven at 150 °C for 1 min, a silicone release film with uniform and stable peel strength was obtained, and the coating thickness was 1 μm.

[0106] The following performance tests were carried out on the release films prepared in the examples and comparative examples:

[0107] Peel strength test, method: FINAT10; surface free energy test, method: water contact angle tester (OWRK method); coating modulus test, method: nanoindentation instrument (200 nm).

[0108] The test results are shown in Table 1 below:

[0109] Table 1

[0110]

[0111]

[0112] Through the comparison of the 180° peel strength and peel strength climbing rate of Example 1 with Comparative Example 1 and Comparative Example 2, it can be seen that by introducing low-polarity long-chain siloxane branches in this solution, the peel strength is significantly lower than that of commercially available products, and the high-temperature stability is significantly better than that of commercially available products. Through the comparative analysis of the test results of the coating modulus and self-adsorption phenomenon of Comparative Example 2 and Example 5, it can be seen that by introducing benzyl ester segments in the present invention, the modulus of the release coating is significantly higher than that of commercially available products. After increasing the coating thickness to 1 μm, there is no self-adsorption phenomenon in Example 5 while there is a self-adsorption phenomenon in the commercially available product (Comparative Example 2).

[0113] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and embodiments. It can be fully applied to various fields suitable for the present invention. For those familiar with the field, additional modifications can be easily made. Therefore, without departing from the general concept defined by the claims and the equivalent scope, the present invention is not limited to specific details.

Claims

1. A high-stability release agent, characterized in that, It includes the following raw material components by weight parts: 5-20 parts of dihydroxy-terminated long-chain branched organosilicone oil, 1-4 parts of benzoate, and 0.05-0.2 part of solid acid catalyst; Among them, the preparation raw materials of the dihydroxy-terminated long-chain branched organosilicone oil include by weight parts: 0.5-2 of dimethoxyalkylsilane; 10-100 parts of hydroxyl-terminated silicone oil; 0.1-0.4 of solid acid catalyst; 0.8-2.5 parts of vinyl dimethoxysilane.

2. The high-stability release agent according to claim 1, wherein The dimethoxyalkylsilane is one or more of octadecyl dimethoxysilane, diisopropyl dimethoxysilane, hexadecyl dimethoxysilane, and dodecyl dimethoxysilane.

3. The high-stability release agent according to claim 1, wherein The vinyl dimethoxysilane is one or more of vinyl ethyl dimethoxysilane, vinyl propyl dimethoxysilane, vinyl butyl dimethoxysilane, and vinyl methyl silanediol diacetate.

4. The high-stability release agent according to claim 1, characterized in that, The benzoate is one or more of methyl benzoate, ethyl benzoate, and butyl benzoate.

5. The high-stability release agent according to claim 1, wherein The number-average molecular weight of the hydroxyl-terminated silicone oil is 4000-20000 g / mol.

6. The high-stability release agent according to claim 1, wherein, The dihydroxy-terminated long-chain branched organosilicone oil is prepared by the following method: Mix the dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, react under heating, then add vinyl methyl dimethoxysilane and react. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst, and dehydrate the obtained product under negative pressure and heating to obtain the dihydroxy-terminated long-chain branched organosilicone oil.

7. The high-stability release agent according to claim 6, characterized in that, The dihydroxy-terminated long-chain branched organosilicone oil is prepared by the following method: Mix the dimethoxyalkylsilane, hydroxyl-terminated silicone oil, and solid acid catalyst evenly, heat up to 50-70 °C, carry out a constant-temperature reaction for 2-8 h, then add vinyl methyl dimethoxysilane and carry out a constant-temperature reaction for 2-8 h. After the reaction is completed, filter by suction to separate and remove the solid acid catalyst, and dehydrate the obtained product under a negative pressure of -0.03 mpa to -0.1 mpa and at 70-90 °C for 1-4 h to obtain the dihydroxy-terminated long-chain branched organosilicone oil.

8. A preparation method of a high-stability release agent according to any one of claims 1-7, characterized in that, It includes the following steps: Mix the dihydroxy-terminated long-chain branched organosilicone oil, benzoate, and solid acid catalyst evenly, heat up to 80 °C, and react in a negative pressure environment of -0.03 mpa to -0.1 mpa for 6 h. Filter by suction to separate and remove the solid acid catalyst to obtain the high-stability release agent.

9. A release liquid, characterized in that, It is obtained by uniformly mixing the following raw materials by weight parts: 100 parts of the high-stability release agent described in any one of claims 1-7; 0.8-2.5 parts of hydrogen-containing silicone oil; 0.3-1.2 parts of anchoring agent; 0.05-0.2 part of Karstedt platinum catalyst; 12-50 parts of solvent.

10. A release film, characterized in that, It is prepared by the following method: uniformly coat the release liquid described in claim 9 on a substrate and dry it to obtain the release film.

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