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Method for preparing diphenyl ether/organic silicon double-modified phenolic resin adhesive

A technology of phenolic resin glue and diphenyl ether, applied in adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problems of easy oxidation, poor high temperature resistance, etc., and achieve increased crosslinking density The effect of large size, improved heat resistance, and broad application prospects

Inactive Publication Date: 2019-12-13
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem that the present invention mainly solves is that the phenolic hydroxyl-OH and methylene-CH on the structure of the traditional phenolic resin adhesive 2 -It is easy to oxidize, resulting in poor high temperature resistance, and a preparation method of a diphenyl ether / organic silicon double-modified phenolic resin adhesive is provided

Method used

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  • Method for preparing diphenyl ether/organic silicon double-modified phenolic resin adhesive
  • Method for preparing diphenyl ether/organic silicon double-modified phenolic resin adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 116.20g of methyltrimethoxysilane, 228.29g of bisphenol A and 3.44g of p-toluenesulfonic acid into the reaction kettle, stir until a uniform solution is formed, gradually increase the temperature, and react at 175°C±5°C to obtain alkylphenoxy base silane intermediate; after cooling down, add 62.68g of diphenyl ether and 70.61g of formaldehyde aqueous solution, react with the alkylphenoxysilane intermediate at 90°C to the end, distill under reduced pressure, and obtain a diphenyl diphenyl ether after vacuum drying Ether modified phenolic resin adhesive.

Embodiment 2

[0024] Add 41.27g of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane, 94.11g of phenol and 1.41g of phosphoric acid into the reaction kettle, stir until a homogeneous solution is formed, gradually increase the temperature, 160 ℃±5℃ to react to obtain the alkylphenoxysilane intermediate; then cool down, add 25.58g of diphenyl ether and 26.13g of paraformaldehyde, and react with the alkylphenoxysilane intermediate at 85℃ to the end, A diphenyl ether modified phenolic resin adhesive was obtained after vacuum distillation and vacuum drying.

Embodiment 3

[0026] Add 68.11g of methyltrimethoxysilane, 94.11g of phenol and 1.88g of methanesulfonic acid into the reaction kettle, stir until a uniform solution is formed, gradually increase the temperature, and react at 150°C±5°C to obtain an intermediate alkylphenoxysilane After cooling down, add 31.27g of diphenyl ether and 24.04g of paraformaldehyde, react with the intermediate of alkylphenoxysilane at 85°C to the end, distill under reduced pressure, and dry in vacuum to prepare a modified diphenyl ether phenolic resin adhesive.

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Abstract

The invention discloses a method for preparing a diphenyl ether / organic silicon double-modified phenolic resin adhesive and belongs to the technical field of adhesive preparation. The method comprisesthe following steps: firstly, under a catalysis function of an acidic catalyst, enabling a siloxane monomer and a phenol compound to react to generate an alkyl phenoxy silane intermediate; performingcooling, adding certain amounts of diphenyl ether and aldehyde compounds, enabling the compounds to react with the alkyl phenoxy silane intermediate till a final point, performing vacuum distillation, and performing vacuum drying so as to obtain the diphenyl ether / organic silicon double-modified phenolic resin adhesive. By adopting the method, a Si-O bond (460kJ / mol) with high bond energy is introduced into a phenolic resin structure, a weak section, namely a phenolic hydroxyl group -OH in the structure of the Si-O bond is partially blocked, and the thermal resistance of a resin can be improved; and in addition, diphenyl ether is introduced into the resin structure, the density of a benzene ring is indirectly increased, the cross-linking density after curing is increased, the thermal resistance of the resin can be further improved, and the resin has good insulation performance and has wide application prospects.

Description

technical field [0001] The invention discloses a preparation method of a diphenyl ether / organic silicon double-modified phenolic resin adhesive, which belongs to the technical field of adhesive preparation. Background technique [0002] Phenolic resin, also known as bakelite powder, is widely used in the fields of electronics, machinery, construction, refractory materials, and bonding because of its advantages such as simple synthesis process, low cost, and high bonding strength. 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 into the macromolecular structure of the phenolic resin to partially block the phenolic hydroxyl groups, and at the same time form a Si-O bond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C09J161/14
CPCC08G8/28C09J161/14
Inventor 袁天顺吴琼彭进宋旭东姚煜
Owner HENAN UNIVERSITY OF TECHNOLOGY
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