CN-121975128-A - Heavy stripping regulator for organosilicon release film, and preparation method and application thereof

CN121975128ACN 121975128 ACN121975128 ACN 121975128ACN-121975128-A

Abstract

The invention belongs to the technical field of organosilicon release agents, and discloses a heavy stripping regulator for an organosilicon release film, and a preparation method and application thereof. The regulator is prepared by condensing branched polysiloxane oligomer and hydroxyl-containing alkane monomer or polymer with the mass ratio of 0.4-2.5:1 under the catalysis of toluene and alkali at 60-120 ℃ for 2-8 hours, and then neutralizing with acid, filtering, drying and distilling under reduced pressure to obtain the product. The branched polysiloxane oligomer is prepared by pre-dissolving trifunctional silane and isopropanol, then dropwise adding water, condensing oxalic acid, washing and vacuum drying at 40-60 ℃. The regulator is used for solvent-free organic silicon release agent and is prepared into release paper through coating and curing, the change amplitude of the stripping force is less than or equal to 25% under the aging condition of 70 ℃, the residual adhesion rate is more than or equal to 90%, the stripping force is increased along with the increase of the addition amount, and the silicon transfer is small, so that the release paper is suitable for heavy stripping scenes of high-viscosity surface materials.

Inventors

SHI JUN
WANG CHAOLIN
ZHANG GUOHAO
TU YUANYUAN
WANG HANGZHOU
HUANG YOUCHENG
JIANG SHUMIN
ZHOU YU
Qi Longbo
TANG YANTING

Assignees

中科院广州化学有限公司
国科广化(南雄)新材料研究院有限公司
国科广化精细化工孵化器(南雄)有限公司
国科广化韶关新材料研究院

Dates

Publication Date: 20260505
Application Date: 20260206

Claims (9)

1. The heavy peeling regulator for the organic silicon release film is characterized by having a structure shown in the following formula 1, wherein R is H-(O-CH 2 -CH 2 -)O-、HO-CH 2 -CH(OH)-CH 2 -O-、HO-(CHOH-CH 2 -O-) 2 -(CHOH) 2 - CH 2 -O-、R 1 COO-(CH 2 -CH(OH)-CH 2 -O-) 2 -CH 2 -CH(OH)-CH 2 -O- or- (O-CH 2 -CH 2 -) n -O-,R 1 ) is isostearyl; ; formula 1.
2. The method for preparing the heavy release regulator for the organosilicon release film, which is disclosed in claim 1, is characterized by comprising the following operation steps of reacting hydroxyl-containing alkane monomers or polymers thereof with branched polysiloxane oligomers under the condition of base catalysis to prepare the heavy release regulator for the organosilicon release film.
3. The method for preparing a heavy release modifier for a silicone release film according to claim 1, wherein the branched polysiloxane oligomer has a structure as shown in formula 2: ; 2, 2 The branched polysiloxane oligomer is prepared by the following method: (1) Mixing a trifunctional silane monomer and isopropanol in a mass ratio of 1:1, and uniformly stirring at room temperature to obtain a solution a; (2) Mixing deionized water and oxalic acid solution in a mass ratio of 3:2, and uniformly stirring to obtain a solution b; (3) Dropwise adding the solution b obtained in the step (2) into the solution a obtained in the step (1), wherein the mass ratio of the solution a to the solution b is 4:1, stirring is kept at room temperature and in a sealing state, and stirring is continued for 2-8 hours at 60-80 ℃ after the dropwise adding is finished, so that a clear and transparent solution is obtained; (4) Washing the clear and transparent solution obtained in the step (3) with deionized water for multiple times, collecting the lower viscous product, and vacuum drying the viscous product at 60 ℃ for 2 hours to obtain the branched polysiloxane oligomer.
4. The method of preparing a heavy release modifier for a silicone release film according to claim 3, wherein the trifunctional silane monomer in the step (1) is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, and 3-glycidoxypropyl triethoxysilane.
5. The method for preparing a heavy release modifier for a silicone release film according to claim 2, wherein the hydroxyl-containing alkane monomer or the polymer thereof is one or more of glycerol, sorbitol, isomalt, polyglycerin-3-diisostearate, polyethylene glycol and polyethylene oxide.
6. The preparation method of the heavy peeling regulator for the organic silicon release film is characterized by comprising the following steps of mixing hydroxyl-containing alkane monomers or polymers thereof with branched polysiloxane oligomer according to a mass ratio of 1:0.4-2.5, adding toluene and an alkaline catalyst, reacting for 6 hours at 80 ℃, neutralizing the obtained reaction mixture to be neutral at 60 ℃ by weak acid, filtering, drying for 2 hours by using anhydrous sodium sulfate, and filtering again to obtain the heavy peeling regulator for the organic silicon release film.
7. The method for preparing a heavy peeling regulator for an organosilicon release film according to claim 6, wherein the alkaline catalyst is one of potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide, ammonia water, butanediamine and sodium methoxide, and the dosage of the alkaline catalyst is 100 ppm-1000 ppm.
8. The method of claim 6, wherein the toluene is used in an amount of 20 to 40% of the sum of the amounts of the hydroxyalkane monomers or polymers thereof and the branched polysiloxane oligomer.
9. The application of the heavy release modifier for the organic silicon release film in preparing release paper is characterized by comprising the following steps of dissolving vinyl silicone oil and hydrogen-containing silicone oil with ethyl acetate, adding an inhibitor, stirring for 30 minutes, adding the heavy release modifier for the organic silicon release film, uniformly stirring, adding a catalyst, stirring for 15 minutes to obtain the release agent, coating and curing to obtain the release paper, wherein the dosage of the heavy release modifier for the organic silicon release film is 5-30% of the total mass of the release agent.

Description

Heavy stripping regulator for organosilicon release film, and preparation method and application thereof Technical Field The invention belongs to the technical field of organosilicon release agents, and particularly relates to a heavy stripping regulator for an organosilicon release film, and a preparation method and application thereof. Background The parting agent is a key auxiliary agent capable of forming a separation film on the surface of a mold, and has the core function of ensuring that molded products such as plastics, rubber, composite materials and the like are smoothly separated from the mold, and simultaneously ensuring the surface smoothness of the products and the integrity of the mold. The application field of the organosilicon release agent is directly determined by the stripping force and the stability of the organosilicon release agent. In the current market, the research of the regulator aiming at light and medium stripping force scenes is mature, but the research of the heavy stripping force regulator aiming at special application scenes still has obvious gaps. Particularly in heavy peeling scenes such as electronic component manufacturing, high-viscosity adhesive tape compounding and the like which need to bear a high-viscosity surface material, if the peeling strength of the organosilicon release agent is lower than the bonding threshold value of the surface material and the base material, the surface material can fall off under the action of slight peeling operation or external vibration. The dropping can not only greatly increase the production reworking rate and increase the enterprise cost due to the re-lamination or direct scrapping of the surface material, but also pollute the clean production environment due to the scraps generated by the dropping, and can directly lower the product yield of the subsequent process for the electronic industry with extremely high precision requirement. Therefore, developing a special heavy stripping force regulator becomes a key path for solving the technical problems of the organosilicon release agent such as silicon transfer, small stripping force, easy stripping of the surface material and the like. Disclosure of Invention In view of the above-mentioned drawbacks and shortcomings of the prior art, a primary object of the present invention is to provide a heavy release modifier for silicone release films. The invention further aims to provide a preparation method of the heavy peeling regulator for the organic silicon release film. It is still another object of the present invention to provide an application of the heavy release modifier for silicone release films. The aim of the invention is achieved by the following technical scheme: A heavy peeling regulator for an organosilicon release film, which has a structure shown in the following formula 1, wherein R is H-(O-CH2-CH2-)O-、HO-CH2-CH(OH)-CH2-O-、HO-(CHOH-CH2-O-)2-(CHOH)2- CH2-O-、R1COO-(CH2-CH(OH)-CH2-O-)2-CH2-CH(OH)-CH2-O- or- (O-CH 2-CH2-)n-O-,R1) is isostearyl; formula 1. The preparation method of the heavy stripping regulator for the organosilicon release film comprises the following operation steps of reacting hydroxyl-containing alkane monomers or polymers thereof with branched polysiloxane oligomer under the condition of base catalysis to obtain the heavy stripping regulator for the organosilicon release film. The branched polysiloxane oligomer has a structure as shown in formula 2: 2, 2 The branched polysiloxane oligomer is prepared by the following method: (1) Mixing a trifunctional silane monomer and isopropanol in a mass ratio of 1:1, and uniformly stirring at room temperature to obtain a solution a; (2) Mixing deionized water and oxalic acid solution in a mass ratio of 3:2, and uniformly stirring to obtain a solution b; (3) Dropwise adding the solution b obtained in the step (2) into the solution a obtained in the step (1), wherein the mass ratio of the solution a to the solution b is 4:1, stirring is kept at room temperature and in a sealing state, and stirring is continued for 2-8 hours at 60-80 ℃ after the dropwise adding is finished, so that a clear and transparent solution is obtained; (4) Washing the clear and transparent solution obtained in the step (3) with deionized water for multiple times, collecting a lower viscous product, and vacuum drying the viscous product at 40-60 ℃ for 2 hours to obtain the branched polysiloxane oligomer. The trifunctional silane monomer of step (1) is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, and 3-glycidoxypropyl triethoxysilane. The hydroxyl-containing alkane monomer or polymer thereof is one or more of glycerol, sorbitol, isomalt, polyglycerol-3-diisostearate, polyethylene glycol and polyethylene oxide. The preparation method of the heavy stripping regulator for the organosilicon release film comprises the following operation steps of mixing hydroxyl-containing alkane monomer