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Method for preparing phosphorus-silicon double-modified phenolic resin adhesive

A phenolic resin adhesive and modification technology, which is applied in the direction of adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problem of insufficient flame resistance and reaction polymerization degree of new silicon phenolic resin adhesives Difficult to control, difficult to control the reaction process, etc., to achieve the effects of enhanced resin comprehensive performance, increased flame resistance, and increased cross-linking density

Inactive Publication Date: 2019-11-15
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 silicone phenolic resin adhesives is complicated, and there are reactions such as hydrolysis and self-polymerization of silicone monomers, phenolic self-polymerization, and monomer-phenolic copolymerization, and the degree of reaction polymerization is difficult to control.
[0004] The present inventor has synthesized and prepared a novel silicon phenolic resin adhesive (SPF) by transesterification in the previous research, which solved the problem that the reaction process is difficult to control in the preparation process of the above silicon phenolic resin adhesive; yet, prepared The flame resistance of the new silicone phenolic resin adhesive is insufficient, and it is not satisfactory for a large number of applications in some fields, and its flame resistance needs to be further improved

Method used

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  • Method for preparing phosphorus-silicon double-modified phenolic resin adhesive
  • Method for preparing phosphorus-silicon double-modified phenolic resin adhesive
  • Method for preparing phosphorus-silicon double-modified phenolic resin adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 62.88g of phosphoric acid, 116.20g of methyltrimethoxysilane and 228.29g of bisphenol A into the reaction kettle, stir evenly, add 3.44g of p-toluenesulfonic acid, raise the temperature, and react at 175°C to form a compound containing phosphorus atoms or silicon atoms. After that, slowly lower the temperature, add 70.61g of formaldehyde solution, and further react with the intermediate containing phosphorus atoms or silicon atoms at a temperature of 90°C to prepare a phosphorus-silicon double-modified phenolic resin adhesive.

Embodiment 2

[0026] Add 38.79g of phosphoric acid, 68.11g of methyltrimethoxysilane and 94.11g of phenol into the reaction kettle, stir evenly, add 1.88g of methanesulfonic acid, program temperature rise, and react at 150°C to form intermediates containing phosphorus atoms or silicon atoms After that, slowly lower the temperature, add 24.04g of paraformaldehyde, and further react with intermediates containing phosphorus atoms or silicon atoms at a temperature of 85°C to prepare a phosphorus-silicon double-modified phenolic resin adhesive.

Embodiment 3

[0028] Add 25.42g of phosphoric acid, 41.27g of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 94.11g of phenol into the reaction kettle, stir evenly, add 1.41g of sulfuric acid, and heat up , react at 160°C to generate an intermediate containing phosphorus or silicon atoms; then slowly lower the temperature, add 26.13g of paraformaldehyde, and further react with the intermediate containing phosphorus or silicon atoms at a temperature of 85°C to obtain a phosphorus silicon Double modified phenolic resin adhesive.

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Abstract

The invention discloses a method for preparing a phosphorus-silicon double-modified phenolic resin adhesive. The method mainly comprises the following steps: putting phosphoric acid, a siloxane monomer and a phenolic compound into a reaction kettle, performing uniform stirring, adding an acidic catalyst, performing temperature programming, and performing a reaction at 110-200 DEG C so as to obtainan intermediate with phosphorus atoms or silicon atoms; slowly reducing the temperature, adding a certain amount of an aldehyde compound, and performing a further reaction on the aldehyde compound and the intermediate with the phosphorus atoms or the silicon atoms at 70-95 DEG C, so as to obtain the phosphorus-silicon double-modified phenolic resin adhesive. As a P-O bond (410 kJ / mol) and a Si-Obond (460 kJ / mol) with high bond energy are introduced into a phenolic resin molecule structure, a weak link phenolic hydroxyl group-OH in the structure can be partially blocked, in addition, the average functionality degree of reaction monomers is indirectly increased, the crosslinking density can be increased after the resin is cured, and the thermal resistance of the resin can be improved; andin addition, due to introduction of the phosphorus atoms P in the structure, the flame resistance of the resin can be remarkably improved, and the comprehensive properties of the resin can be improved.

Description

technical field [0001] The invention relates to the field of adhesives, in particular to a method for preparing a phosphorus-silicon double-modified phenolic resin adhesive. Background technique [0002] In the field of synthetic resin adhesives, phenolic resin is used in various fields closely related to the national economy, such as coatings, electronics, machinery, insulating materials, and molding compounds, due to its good weather resistance, water resistance, and high adhesive strength. . However, due to the easy oxidation of phenolic hydroxyl groups and methylene groups in the molecular structure of traditional phenolic resin adhesives, the heat resistance is affected, which limits its application in certain fields, especially high-temperature fields. [0003] In order to improve the thermal stability of the phenolic resin adhesive, silicon atoms are introduced into the macromolecular structure of the phenolic resin to partially block the phenolic hydroxyl groups, an...

Claims

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Application Information

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