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A kind of preparation method of modified silicon phenolic resin adhesive

A silicon phenolic resin and adhesive technology, which is applied in the directions of adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problems of difficult control of the reaction process, product application restrictions, complex preparation process, etc. To achieve the effect of simple steps, improved comprehensive performance, and improved heat resistance

Active Publication Date: 2021-09-03
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 inventor of the present application has synthesized and prepared a novel silicon phenolic resin (SPF) by transesterification in the previous research, which has solved the problem that the reaction process is difficult to control in the above silicon phenolic resin preparation process; however, the prepared novel silicon phenolic resin Some properties of the resin, such as toughness, wear resistance and water resistance are not good, and the application of products, especially in the high-tech field, is limited. It is urgent to further improve its comprehensive performance in order to industrialize production

Method used

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  • A kind of preparation method of modified silicon phenolic resin adhesive
  • A kind of preparation method of modified silicon phenolic resin adhesive
  • A kind of preparation method of modified silicon phenolic resin adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 9.41 g of nylon, 41.27 g of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane, 94.11 g of phenol and 1.41 g of phosphoric acid into the reactor, stir evenly, and slowly heat up. React at 160°C to generate intermediates containing amide groups or silicon atoms; then slowly lower the temperature, add 26.13 g of paraformaldehyde, and further react with intermediates containing amide groups or silicon atoms at a temperature of 85°C to prepare A modified silicone phenolic resin adhesive based on blocked phenolic hydroxyl groups.

Embodiment 2

[0029] Add 15.56 g of epoxy resin, 116.20 g of methyltrimethoxysilane, 228.29 g of bisphenol A and 3.44 g of p-toluenesulfonic acid into the reaction kettle, stir evenly, slowly raise the temperature, and react at 165 ° C to form or intermediates of silicon atoms; then slowly lower the temperature, add 70.61 g of formaldehyde solution, and further react with intermediates containing epoxy groups or silicon atoms at a temperature of 90 ° C to prepare a modified silicon based on blocking phenolic hydroxyl groups Phenolic resin adhesive.

Embodiment 3

[0031] Add 36.17 g of bismaleimide, 68.11 g of methyltrimethoxysilane, 94.11 g of phenol and 1.88 g of methanesulfonic acid into the reaction kettle, stir evenly, slowly raise the temperature, and react at 158 ​​° C to form a group or silicon atom intermediate; then slowly lower the temperature, add 24.04 g of paraformaldehyde, through its further reaction with the intermediate containing imide ring group or silicon atom at a temperature of 85 ℃, to prepare a blockade-based Phenolic hydroxyl modified silicone phenolic resin adhesive.

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Abstract

A preparation method of a modified silicon phenolic resin adhesive, characterized in that: the method comprises the following steps: first adding a phenolic hydroxyl blocking agent, a siloxane monomer, a phenolic compound and an acidic catalyst into a reaction kettle, Stir evenly, slowly heat up, and react at 110~200°C to form intermediates containing blocker groups or silicon atoms; then slowly cool down, add a certain amount of aldehyde compounds, and pass through the intermediate containing blocker groups or silicon atoms The body is further reacted at a temperature of 70~95°C to prepare a modified silicon phenolic resin adhesive based on blocking phenolic hydroxyl groups; among them: four raw materials: phenolic hydroxyl blocking agent, siloxane monomer, phenolic compound and acidic catalyst The mass ratio of the compound is 0.05~0.80:0.1~1.0:1:0.05%~4%; the molar ratio of aldehyde compounds and phenolic compounds is 0.5~1.0:1.

Description

technical field [0001] The invention relates to the technical field of adhesive preparation, in particular to a preparation method of a modified silicon phenolic resin adhesive. Background technique [0002] Phenolic resin (PF) is the earliest synthetic resin. Its raw materials are cheap, the synthesis process is simple, and it has excellent mechanical properties, dimensional stability, flame retardancy and electrical insulation. It is widely used in chemical industry, construction, machinery, aerospace , Bonding and other fields have been widely used. 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 were introduced into the macromolecular structure of the phenolic resin to partial...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J161/14C08G8/28
CPCC08G8/28C09J161/14
Inventor 彭进袁天顺张琳琪邹文俊夏绍灵简亚溜吴琼
Owner HENAN UNIVERSITY OF TECHNOLOGY
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