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CN-122011395-A - Method for synthesizing UV (ultraviolet) light-cured trapezoidal polysiloxane resin by self-catalysis, UV light-cured trapezoidal polysiloxane polyacrylic resin and application thereof

CN122011395ACN 122011395 ACN122011395 ACN 122011395ACN-122011395-A

Abstract

The invention belongs to a photocuring organic silicon resin material, and discloses a method for synthesizing a UV photocuring trapezoidal tertiary amine polysiloxane resin by self-catalysis, the UV photocuring trapezoidal tertiary amine polysiloxane polyacrylic resin and application thereof. The method for synthesizing the UV light-cured trapezoidal tertiary amine polysiloxane resin by self-catalysis comprises the following steps of uniformly mixing an aminosilane coupling agent containing tertiary amine groups, a phenylsilane coupling agent, an acryloyloxy silane coupling agent and an organic solvent, adding water, adding a blocking agent after a period of reaction, and removing the solvent in the product after the reaction is finished to obtain the UV light-cured trapezoidal tertiary amine polysiloxane resin. And mixing the obtained UV light-cured trapezoidal tertiary amine polysiloxane resin with polyacrylate to obtain the UV light-cured trapezoidal tertiary amine polysiloxane polyacrylate resin. The invention provides a simple method for preparing trapezoidal polysiloxane resin, which does not need to add a catalyst, does not need to carry out operations such as washing, filtering and the like, and has wide application prospect.

Inventors

  • LIN SHUDONG
  • LIU HUI
  • HUANG YUEWEN
  • LI XIAOBIN

Assignees

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

Dates

Publication Date
20260512
Application Date
20260226

Claims (10)

  1. 1. A method for autocatalytically synthesizing a UV light-cured trapezoidal tertiary amine polysiloxane resin, which is characterized by comprising the following steps: Uniformly mixing an aminosilane coupling agent containing tertiary amine groups, a phenylsilane coupling agent, an acryloyloxy silane coupling agent and an organic solvent, adding water, reacting for a period of time, adding a blocking agent, and removing the solvent in the product after the reaction is finished to obtain the UV light-cured trapezoidal tertiary amine polysiloxane resin.
  2. 2. The method for autocatalytically synthesizing a UV photocured trapezoidal tertiary amine polysiloxane resin according to claim 1, wherein the tertiary amine group-containing aminosilane coupling agent is at least one of (N, N-dimethyl-3-aminopropyl) trimethoxysilane, (N, N-diethyl-3-aminopropyl) trimethoxysilane, (N, N-dimethyl-3-aminopropyl) triethoxysilane; the phenylsilane coupling agent is at least one of phenyltrimethoxysilane and phenyltriethoxysilane; The acryloyloxy silane coupling agent is at least one of 3- (methacryloyloxy) propyl trimethoxy silane, 3- (methacryloyloxy) propyl triethoxy silane and 3-acryloyloxy propyl trimethoxy silane; the organic solvent is at least one of dichloromethane and tetrahydrofuran; the end capping agent is at least one of trimethylethoxysilane and methoxytrimethylsilane.
  3. 3. The method for autocatalytically synthesizing the UV light-cured trapezoidal tertiary amine polysiloxane resin according to claim 1, wherein the molar ratio of the aminosilane coupling agent, the phenylsilane coupling agent, the acryloyloxy silane coupling agent and the end capping agent containing tertiary amine groups is 0.5-1:1:1:0.5-1; the molar ratio of the phenylsilane coupling agent to the water is 1:5-9; the dosage ratio of the solvent to the silane coupling agent is 15~50 g:0.1~0.5 mol; the reaction temperature is 30-40 ℃ and the reaction time is 48-96 hours; the adding time of the end capping agent is 1/3-1/2 of the reaction time.
  4. 4. A UV light-curable trapezoidal tertiary amine polysiloxane resin prepared by the method of any one of claims 1-3.
  5. 5. A method of making a UV light-curable trapezoidal tertiary amine polysiloxane polyacrylate resin using the UV light-curable trapezoidal polysiloxane resin of claim 4, comprising the steps of: and mixing the UV light-cured trapezoidal tertiary amine polysiloxane resin with polyacrylate to obtain the UV light-cured trapezoidal tertiary amine polysiloxane polyacrylate resin.
  6. 6. The method for preparing a UV light-curable trapezoidal tertiary amine polysiloxane polyacrylate according to claim 5, wherein the polyacrylate is at least one of trimethylolpropane triacrylate, pentaerythritol tetraacrylate, pentaerythritol triacrylate; the mass ratio of the polyacrylate to the UV light-cured trapezoidal tertiary amine polysiloxane resin is 0.5-2:0.5-4.
  7. 7. A UV light-curable trapezoidal tertiary amine polysiloxane polyacrylate resin prepared by the method of claim 5 or 6.
  8. 8. Use of a UV light-curable trapezoidal tertiary amine polysiloxane polyacrylate resin as claimed in claim 7 in the preparation of a paint, coating material, film forming composition or protective coating.
  9. 9. The use according to claim 8, wherein the paint, coating material, film-forming composition or protective coating comprises the components of a ladder tertiary amine polysiloxane polyacrylate, a photoinitiator and an organic solvent; Wherein the dosage of the photoinitiator is 7-10wt% of the mass of the trapezoidal tertiary amine polysiloxane polyacrylate resin.
  10. 10. The use according to claim 9, wherein the initiator is a hydrogen abstraction type photoinitiator; The organic solvent is at least one of butyl acetate, propyl acetate and ethyl acetate; the mass ratio of the organic solvent to the photoinitiator is 2-3:0.7-1.

Description

Method for synthesizing UV (ultraviolet) light-cured trapezoidal polysiloxane resin by self-catalysis, UV light-cured trapezoidal polysiloxane polyacrylic resin and application thereof Technical Field The invention belongs to the field of photo-curing advanced organic silicon materials, and particularly relates to a method for synthesizing UV photo-curing trapezoidal polysiloxane resin by self-catalysis, the UV photo-curing trapezoidal polysiloxane polyacrylic resin and application thereof. Background The light-cured advanced organosilicon material has the advantages of high molecular polymer, environmental protection and the like, does not need to be cured in a complex and complicated mode such as heat curing, moisture curing and the like other materials, can be rapidly crosslinked and cured only under ultraviolet radiation, and has the advantages of high efficiency, environmental protection and the like. As such, advanced silicone materials continue to be one of the development hotspots in various development directions. Among them, the polysiloxane resin material is one of the main development directions of advanced photo-curing organosilicon materials, and the polysiloxane resin is a multi-polymer taking Si-O-Si as a framework. The polymer has the performances of thermal stability, hydrophobicity, chemical inertness, processability and the like, so that the polymer can be widely applied to the fields of coating, construction, textile and the like. Is the most studied photo-curing organic silicon material at present. In the polysiloxane resin, the trapezoidal polysiloxane has a double-chain Si-O-Si structure, so that the trapezoidal polysiloxane has higher thermal stability and mechanical property than the common polysiloxane resin, and the double-chain structure means that more functional groups can be linked to a main chain, so that different silane coupling agent types can be better replaced according to actual requirements, and different properties are given to the resin. However, the synthesis of trapezoidal polysiloxane resins generally requires the addition of a catalyst to effect the reaction, and the addition of hydrochloric acid or potassium carbonate to provide acidic or basic conditions to catalyze the reaction, which presents a problem of catalyst removal after the reaction. Liu Guojun et al use anhydrous potassium carbonate as a catalyst to synthesize an epoxycyclohexyl trapezoidal polysiloxane, but the subsequent removal of anhydrous potassium carbonate requires multiple water washes and filtration, resulting in more product loss and low yield. And multiple times of filtration can generate a lot of waste water and waste materials, which is not beneficial to environmental protection and cost saving. Jin Ziyi Lang et al in Japan synthesized an amino ladder polysiloxane resin using hydrochloric acid as the catalyst, but subsequently required freeze drying to remove the catalyst. It is a difficult problem to separate the product from the catalyst while synthesizing the trapezium polysiloxane efficiently. Disclosure of Invention To overcome the disadvantages and shortcomings of the prior art, a primary object of the present invention is to provide a method for autocatalytically synthesizing a UV light curable trapezoidal polysiloxane resin. It is a further object of the present invention to provide a UV light curable trapezoidal tertiary amine polysiloxane resin. The invention also aims to provide a preparation method of the UV light-cured trapezoidal tertiary amine polysiloxane polyacrylate resin. It is still another object of the present invention to provide a UV light curable trapezoidal tertiary amine polysiloxane polyacrylate resin. It is still another object of the present invention to provide the use of a UV light cured trapezoidal tertiary amine polysiloxane polyacrylate resin. The aim of the invention is achieved by the following technical scheme: a method for synthesizing UV light curing trapezoidal tertiary amine polysiloxane resin by self-catalysis comprises the following steps: Uniformly mixing an aminosilane coupling agent containing tertiary amine groups, a phenylsilane coupling agent, an acryloyloxy silane coupling agent and an organic solvent, adding water, reacting for a period of time, adding a blocking agent, and removing the solvent in the product after the reaction is finished to obtain the UV light-cured trapezoidal tertiary amine polysiloxane resin. Preferably, the amino silane coupling agent containing tertiary amine groups is at least one of (N, N-dimethyl-3-aminopropyl) trimethoxysilane, (N, N-diethyl-3-aminopropyl) trimethoxysilane and (N, N-dimethyl-3-aminopropyl) triethoxysilane; the phenylsilane coupling agent is at least one of phenyltrimethoxysilane and phenyltriethoxysilane; The acryloyloxy silane coupling agent is at least one of 3- (methacryloyloxy) propyl trimethoxy silane, 3- (methacryloyloxy) propyl triethoxy silane and 3-acryloyloxy propyl trimethoxy sila