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CN-120904461-B - Self-repairing silicon resin, preparation method thereof, OCA optical cement containing self-repairing silicon resin and application of OCA optical cement

CN120904461BCN 120904461 BCN120904461 BCN 120904461BCN-120904461-B

Abstract

The invention provides self-repairing silicon resin, a preparation method thereof, OCA optical adhesive containing the self-repairing silicon resin and application thereof, wherein the molecular structure of the self-repairing silicon resin contains disulfide bonds and sulfhydryl groups, and the content of the disulfide bonds in the self-repairing silicon resin is more than 0.6mmol/g. The self-repairing silicone resin is used for preparing OCA optical cement, can improve the initial adhesion of the OCA optical cement while ensuring the high light transmittance, low yellowing and good mechanical property of the OCA optical cement, can also endow the OCA optical cement with a self-repairing function, and improves the repairing efficiency.

Inventors

  • HE NA
  • HONG LIANG
  • CAI JIEHONG
  • LI SONG
  • LIU ZHAOHUI

Assignees

  • 广东派乐玛新材料科技有限公司

Dates

Publication Date
20260508
Application Date
20250829

Claims (20)

  1. 1. The optical adhesive is characterized by comprising 15-60 parts by weight of mercapto silicone resin, 35-80 parts by weight of organosilicon modified polyurethane and 0.5-5 parts by weight of initiator; the sulfhydryl silicone resin is self-repairing silicone resin; the molecular structure of the self-repairing silicon resin contains disulfide bonds and sulfhydryl groups; the content of disulfide bonds in the self-repairing silicone resin is 0.8-1.4 mmol/g; The self-repairing silicon resin is prepared by mixing mercaptosilane, first alkylsilane, sulfur-containing silane and water for reaction to obtain the self-repairing silicon resin; The organic silicon modified polyurethane is acrylate-terminated organic silicon modified polyurethane; the preparation raw materials of the organosilicon modified polyurethane comprise hydroxy-terminated polycarbosilane, polyisocyanate, first polyol and hydroxy-containing acrylic ester.
  2. 2. The optical adhesive of claim 1, wherein the self-healing silicone resin has a number average molecular weight of 10000-30000.
  3. 3. The optical adhesive of claim 1, wherein the self-healing silicone has a polydispersity of 1.2 to 1.4.
  4. 4. The optical adhesive of claim 1, wherein the molar ratio of mercaptosilane, first alkylsilane and sulfur-containing silane is (0.6-2): 3-15): 1.
  5. 5. The optical adhesive of claim 1, wherein the mercaptosilane comprises at least one of 3-mercaptopropyl trimethoxysilane, 3-mercaptopropyl triethoxysilane, 3-mercaptopropyl tributoxysilane, mercaptopropyl dimethoxymethylsilane, 3-octanoylthiopropyl triethoxysilane.
  6. 6. The optical adhesive of claim 1, wherein the adhesive comprises a polymer, the first alkylsilane comprises methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane ethyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane at least one of methyl ethyl dimethoxy silane, methyl ethyl diethoxy silane, vinyl trimethoxy silane, vinyl triethoxy silane, methyl vinyl dimethoxy silane, or methyl vinyl diethoxy silane.
  7. 7. The optical adhesive of claim 1, wherein the sulfur-containing silane comprises bis- [3- (triethoxysilane) -propyl ] -disulfide and/or bis- [3- (triethoxysilane) -propyl ] -tetrasulfide.
  8. 8. The optical adhesive of claim 1, wherein the water is 20-70% of the total mass of mercaptosilane, first alkylsilane and sulfur-containing silane.
  9. 9. The optical adhesive of claim 1, wherein the mixed material further comprises an acid.
  10. 10. The optical adhesive of claim 9, wherein the acid is 1-5% of the water by mass.
  11. 11. The optical adhesive of claim 1, wherein the reaction is at a temperature of 40-80 ℃ for a time of 1-6 hours.
  12. 12. The optical adhesive of claim 1, wherein the post-reaction further comprises a post-treatment step.
  13. 13. The optical adhesive of claim 12, wherein the post-treatment comprises at least one of extraction, washing, and reduced pressure distillation.
  14. 14. The optical adhesive of claim 1, wherein the molar ratio of the hydroxyl-terminated polycarbosilane, the polyisocyanate, and the first polyol is 1 (1.8-3.5): 0.5-2.
  15. 15. The optical adhesive of claim 1, wherein the molar ratio of the hydroxyl-containing acrylate to the polyisocyanate is (0.2-0.8): 1.
  16. 16. The optical adhesive of claim 1, wherein the hydroxyl-terminated polycarbosilane is prepared from a second alkylsilane and a second polyol in a molar ratio of 1 (1.1-1.5).
  17. 17. The optical adhesive of claim 1, wherein the initiator comprises a macromolecular UV initiator.
  18. 18. The optical adhesive of claim 1, wherein the initiator is prepared from (1-3): (1.5-4) a small molecular initiator, a third alkylsilane and a third polyol in a molar ratio.
  19. 19. The optical adhesive of claim 18, wherein the small molecule initiator comprises a benzophenone initiator.
  20. 20. An OCA optical adhesive is characterized by comprising a light release film, an optical adhesive layer and a heavy release film which are sequentially laminated, wherein the optical adhesive layer comprises the optical adhesive as claimed in any one of claims 1-19.

Description

Self-repairing silicon resin, preparation method thereof, OCA optical cement containing self-repairing silicon resin and application of OCA optical cement Technical Field The invention belongs to the technical field of optical materials, and particularly relates to self-repairing silicon resin, a preparation method thereof, OCA optical cement containing the same and application of the OCA optical cement. Background OCA Optical adhesive (Optical CLEAR ADHESIVE) refers to a substrate-free material and a solid double-sided adhesive tape, wherein a release film is respectively adhered to the upper and lower bottom layers of the adhesive layer, and belongs to one type of pressure-sensitive adhesive. OCA optical cement is widely applied to the field of optical display, such as the bonding of display units such as display modules, glass cover plates, touch screens and the like, and has the characteristics of high light transmittance, good bonding strength and the like. Currently, OCA optical adhesives can be classified into acrylic acid ester OCA, silicone OCA, polyurethane OCA, epoxy OCA, etc. according to the type of materials used. Compared with other OCAs, the organic silicon OCA has the advantages of more excellent weather resistance, yellowing resistance, aging resistance, easy repair and the like. However, silicone OCAs currently have poor initial tack and peel strength far lower than other resins. And the initial adhesion is too low, so that the bonding element cannot be transferred immediately after bonding is completed, the production efficiency is low, and the bonding element is easy to fall off in the process of transferring the display, so that loss is caused. In addition, with market expansion of folding screens, curved screens, special-shaped screens, plastic screens and the like, the performance requirements on the bonding materials are higher and higher. However, the OCA inevitably generates mechanical damage to a certain extent in the use process, so that the OCA can cause damage to electronic products, and the application of the OCA is limited to a certain extent. Therefore, developing a silicone resin that can improve the initial adhesion and mechanical properties of OCA optical cement, and make the optical cement have a self-repairing function, and at the same time, can also ensure low haze, high light transmittance, and low yellowing of the optical cement is a problem to be solved in the art. Disclosure of Invention Aiming at the defects existing in the prior art, the invention aims to provide self-repairing silicone resin and a preparation method and application thereof. The self-repairing silicone resin is used for preparing OCA optical cement, can improve the initial adhesion of the OCA optical cement while ensuring the high light transmittance, low yellowing and good mechanical property of the OCA optical cement, can also endow the OCA optical cement with a self-repairing function, and improves the repairing efficiency. To achieve the purpose, the invention adopts the following technical scheme: In a first aspect, the invention provides self-repairing silicone resin, wherein the molecular structure of the self-repairing silicone resin contains disulfide bonds and sulfhydryl groups, and the content of the disulfide bonds in the self-repairing silicone resin is more than 0.6mmol/g. According to the invention, disulfide bonds and sulfhydryl groups are introduced into the molecular structure of the silicon resin, the content of the disulfide bonds is controlled within a specific range, so that the OCA optical adhesive can be endowed with a self-repairing function, an OCA optical adhesive with high self-repairing efficiency can be obtained, an electronic product can be effectively protected, the initial adhesion of the OCA optical adhesive can be improved, element falling and loss are avoided, the production efficiency is improved, and meanwhile, the OCA optical adhesive can be ensured to have low haze, high light transmittance, low yellowing and good mechanical property. In the present invention, the content of disulfide bonds in the self-repairing silicone resin is >0.6mmol/g, for example 0.62mmol/g、0.65mmol/g、0.68mmol/g、0.7mmol/g、0.72mmol/g、0.75mmol/g、0.78mmol/g、0.8mmol/g、0.82mmol/g、0.85mmol/g、0.88mmol/g、0.9mmol/g、0.95mmol/g、1mmol/g、1.1mmol/g、1.2mmol/g、1.3mmol/g、1.4mmol/g、1.5mmol/g、1.6mmol/g、1.7mmol/g、1.8mmol/g, more preferably 0.8 to 1.8mmol/g, still more preferably 1.0 to 1.6mmol/g. Preferably, the number average molecular weight of the self-repairing silicone resin is 10000-30000, for example, 10000, 12000, 14000, 16000, 18000, 20000, 22000, 25000, 28000 and the like can be adopted. Preferably, the polydispersity of the self-repairing silicone resin is 1.2-1.4, for example, 1.2, 1.22, 1.24, 1.26, 1.28, 1.3, 1.32, 1.34, 1.36, 1.38, etc. Preferably, the preparation raw materials of the self-repairing silicone resin comprise mercaptosilane, first alkylsilane and sulfur-containing silane. Pr