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Preparation method of polysulfone modified silicon phenolic resin adhesive

A silicon phenolic resin and adhesive technology, applied in adhesives, adhesive additives, aldehyde/ketone condensation polymer adhesives, etc., can solve the problem of difficult control of the reaction, complicated preparation process, and poor heat resistance of the new silicon phenolic resin Improve heat resistance and oxidation resistance, improve thermal stability and mechanical properties, and achieve excellent comprehensive performance

Inactive Publication Date: 2019-11-22
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of traditional silicon phenolic resin is complex, there are reactions such as hydrolysis self-polymerization of organosilicon monomer, phenolic self-polymerization, monomer and phenolic copolymerization, etc., and the degree of reaction polymerization is difficult to control
[0004] The present inventor has synthesized and prepared novel silicon phenolic resin (SPF) by transesterification in the early stage research, has solved the problem that reaction process is difficult to control in the above silicon phenolic resin preparation process; Yet the prepared novel silicon phenolic resin is in The performance in heat resistance is still not good, and a large number of applications in the high temperature field are not satisfied, and its heat resistance needs to be further improved

Method used

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  • Preparation method of polysulfone modified silicon phenolic resin adhesive
  • Preparation method of polysulfone modified silicon phenolic resin adhesive
  • Preparation method of polysulfone modified silicon phenolic resin adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 68.11g of methyltrimethoxysilane, 94.11g of phenol and 1.88g of methanesulfonic acid into the reaction kettle, stir evenly, slowly raise the temperature, and react at 150°C to form an alkylphenoxysilane intermediate; after cooling down, add 24.04 g paraformaldehyde, slowly warming up to gel, stop reaction, add basic compound to adjust PH to neutrality, obtain silicon phenolic resin after decompression distillation, 30.11g bisphenol A type polysulfone and synthetically prepared silicon phenolic resin The polysulfone modified silicon phenolic resin adhesive was prepared by blending and modifying.

Embodiment 2

[0029] Add 116.20g of methyltrimethoxysilane, 228.29g of bisphenol A and 3.44g of p-toluenesulfonic acid into the reaction kettle, stir evenly, slowly heat up, and react at 175°C to form an alkylphenoxysilane intermediate; then cool down , add 70.61g formaldehyde aqueous solution, slowly heat up to gel, stop the reaction, add basic compound to adjust the pH to neutral, obtain silicon phenolic resin after vacuum distillation, and combine 58.42g bisphenol A polysulfone with synthetically prepared silicon phenolic resin The resin is prepared by blending and modifying to obtain the polysulfone modified silicon phenolic resin adhesive.

Embodiment 3

[0031] Add 41.27g of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane, 94.11g of phenol and 1.41g of phosphoric acid into the reaction kettle, stir evenly, raise the temperature slowly, and react at 160°C to form Alkylphenoxysilane intermediate; after cooling down, add 26.13g paraformaldehyde, slowly heat up to gel, stop the reaction, add basic compound to adjust PH to neutral, obtain silicon phenolic resin after vacuum distillation, and 22.69 g Bisphenol A polysulfone and synthetically prepared silicon phenolic resin are blended and modified to obtain the polysulfone modified silicon phenolic resin adhesive.

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Abstract

A preparation method of a polysulfone modified silicon phenolic resin adhesive belongs to the technical field of adhesive preparation, and is characterized by comprising the following steps: adding asiloxane monomer, a phenolic compound and an acidic catalyst into a reaction kettle, uniformly stirring the mixture, slowly heating the mixture, and performing a reaction at 110-200 DEG C to generatean alkylphenoxy silane intermediate; cooling the intermediate, adding a certain amount of aldehyde compound, slowly heating the mixture to form gel, stopping the reaction, adding an alkaline compoundto adjust the pH value to be neutral, performing reduced pressure distillation to obtain silicon phenolic resin, and performing blending modification on polysulfone and the synthesized silicon phenolic resin to obtain the polysulfone modified silicon phenolic resin adhesive. According to the modified resin, due to the fact that Si-O bonds with high bond energy are introduced into the structure, the heat resistance of the modified resin is greatly improved compared with that of unmodified resin, high-temperature-resistant and high-strength polysulfone is introduced into the resin structure, thethermal stability and mechanical property of the resin are further improved, and the double-modified phenolic resin has excellent comprehensive performance compared with common phenolic resin.

Description

technical field [0001] The invention belongs to the field of adhesive preparation, in particular to a preparation method of polysulfone modified silicon phenolic resin adhesive. Background technique [0002] As the earliest resin synthesized by humans, phenolic resin is usually polymerized by polycondensation of phenolic compounds and aldehyde compounds under the action of a catalyst. With its excellent mechanical properties, dimensional stability and insulation properties, it is widely used in various fields closely related to the national economy, such as automobiles, machinery, electronics, aerospace, and bonding. However, the heat resistance of traditional phenolic resins is affected due to the easy oxidation of phenolic hydroxyl groups and methylene groups in the molecular structure, which limits its application in certain fields, especially high-temperature fields. [0003] In order to improve the thermal stability of the phenolic resin, silicon atoms are introduced i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J161/14C09J11/08C08G8/28
CPCC08G8/28C09J11/08C09J161/14C08L81/06
Inventor 袁天顺吴琼姚煜邹文俊彭进简亚溜
Owner HENAN UNIVERSITY OF TECHNOLOGY