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Preparation method of boron modified phenolic resin adhesive

A phenolic resin glue and the technology of the production method, which are applied in the field of polymer chemistry, can solve the problems of high corrosiveness, irritating smell, HCl gas, etc., and achieve the effects of excellent high temperature resistance, simple operation, and mild conditions

Active Publication Date: 2013-12-25
启东市天汾电动工具技术创新中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned route, there are the following problems: among them, the reaction of halosilane and boric acid is used to generate HCl gas with a pungent smell, which is highly corrosive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1: join phenyl trimethoxy silane and methyl trimethoxy silane according to the mixture that the weight fraction 1:2 makes and boric acid in diglyme, under the condition that tin protochloride exists, Gradually raise the temperature from 90°C to 200°C within 3 hours under a nitrogen atmosphere, and continue to react for 5 hours; then add resorcinol, react for 6 hours, and react for 2 hours under reduced pressure with a water pump to obtain polyborosiloxane (PBSH); organosiloxane Alkane: boric acid: the molar ratio of resorcinol is 1:1: 1, and the catalyst consumption is 1‰ of the total monomer mass;

[0026] Step 2: Take 20 parts by weight of methoxyxylene monomer, 20 parts by weight of hydroquinone and 1.5 parts by weight of 25wt% p-toluenesulfonic acid, react at 125°C for 2 hours, cool down, Add 1.5 parts by weight of 20wt% ammonia water, 12 parts by weight of styrene and 18 parts by weight of formaldehyde, and dehydrate under a vacuum of 0.6KPa to obtain a modifi...

Embodiment 2

[0029] Step 1: Add the mixture of phenyltrimethoxysilane and methyltrimethoxysilane according to the weight fraction of 1:2 and boric acid into dioxane, and in the presence of stannous chloride, in a nitrogen atmosphere Gradually raise the temperature from 90°C to 200°C within 3 hours, and continue the reaction for 5 hours; then add resorcinol, react for 6 hours, and react for 2 hours under reduced pressure by the water pump to obtain polyborosiloxane (PBSH); organosiloxane: boric acid : the molar ratio of resorcinol is 1:1:1, and the catalyst consumption is 1‰ of the total mass of the monomer;

[0030] Step 2: Take 20 parts by weight of methoxyxylene monomer, 20 parts by weight of hydroquinone and 1.5 parts by weight of 25wt% p-toluenesulfonic acid, react at 125°C for 2 hours, cool down, Add 1.5 parts by weight of 20wt% ammonia water, 12 parts by weight of styrene and 18 parts by weight of formaldehyde, and dehydrate under a vacuum of 0.6KPa to obtain a modified phenolic resi...

Embodiment 3

[0033] Step 1: Add the mixture of phenyltrimethoxysilane and methyltrimethoxysilane according to the weight fraction of 1:2 and boric acid into dioxane, and in the presence of titanium tetrachloride, in a nitrogen atmosphere Gradually raise the temperature from 90°C to 200°C within 3 hours, and continue the reaction for 5 hours; then add resorcinol, react for 6 hours, and react for 2 hours under reduced pressure by the water pump to obtain polyborosiloxane (PBSH); organosiloxane: boric acid : the molar ratio of resorcinol is 1:1:1, and the catalyst consumption is 1‰ of the total mass of the monomer;

[0034] Step 2: Take 20 parts by weight of methoxyxylene monomer, 20 parts by weight of hydroquinone and 1.5 parts by weight of 25wt% p-toluenesulfonic acid, react at 125°C for 2 hours, cool down, Add 1.5 parts by weight of 20wt% ammonia water, 12 parts by weight of styrene and 18 parts by weight of formaldehyde, and dehydrate under a vacuum of 0.6KPa to obtain a modified phenolic...

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Abstract

The invention relates to a preparation method of a boron modified phenolic resin adhesive, which comprises the following steps of 1, synthesizing polyborosiloxane (PBSH), 2, synthesizing modified phenolic resin, and 3, preparing the boron modified phenolic resin adhesive. In the boron modified phenolic resin adhesive, the method for preparing PBSH is relatively mild in condition, simple to operate, green and environment-friendly, and has no harmful gas generation; obtained PBSH is excellent in high-temperature resistance, contains a great amount of terminated hydroxy, and can improve the high-temperature resistance and the bonding strength of the phenolic resin when serving as a modifying agent; and the feasible method is provided for preparing the high-temperature-resistant phenolic resin adhesive.

Description

technical field [0001] The invention belongs to the field of macromolecular chemistry, and in particular relates to a method for preparing adhesives synthesized by using polyborosiloxane and modified phenolic resin. Background technique [0002] The price of phenolic resin is very low, the raw materials are easy to buy, and the production process and production equipment are simple. It has become one of the indispensable materials in the industrial sector and is widely used. The thermal stability and high temperature resistance of pure phenolic resin are not high enough, and a lot of research has been done on its modification to improve its heat resistance and bond strength. [0003] Polyborosiloxane (PBS) has excellent heat resistance. Some studies have used boric acid and silicone prepolymers to prepare polyborosiloxane and used it to modify phenolic resins. The carbon residue rate of the modified resins has been greatly improved, but the modified phenolic resin adhesives...

Claims

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Application Information

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IPC IPC(8): C09J161/14C09J183/14C08G8/28C08G77/56
Inventor 俞国宏
Owner 启东市天汾电动工具技术创新中心
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