Production of modified phenolic resin with high boron content

A technology of phenolic resin and boron modification, applied in the field of materials, to achieve the effect of simple and easy preparation method and excellent thermal performance

Inactive Publication Date: 2006-08-16
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the preparation method of modified phenolic resin with high boron content at home and abroad.

Method used

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  • Production of modified phenolic resin with high boron content

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Experimental program
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Effect test

Embodiment 1

[0019] Step (1): According to the molar ratio of boric acid / phenol=1 / 3, 28.2g of phenol and 40ml of toluene solution were added into a four-necked flask equipped with a condenser, a thermometer, an electric stirrer and a thermocouple. Raise the temperature to 90°C, then add 6.2g of boric acid, and at the same time use 0.1mol / L NaOH solution to adjust the pH value of the solution in the four-necked flask. When the pH is between 6 and 8, make the solution react at a temperature range of 90°C , and vacuum dehydration at the same time, the reaction time is 3 hours, and the vacuum degree is 0.1-1KPa; when the liquid is clear and slightly orange, and no water is produced after long-term pumping, stop pumping.

[0020] Step (2) Add 10.2 g of paraformaldehyde with a molecular weight of 450, make it react at 100° C. while stirring, and dehydrate under reduced pressure. As the dehydration proceeds, the liquid in the reaction bottle gradually becomes viscous. After 3-4 hours of reaction,...

Embodiment 2

[0023] Embodiment 2: the mol ratio of the boric acid / phenol of embodiment 1 step (1) is changed into 1 / 2 by 1 / 3, by the mol ratio of boric acid / phenol=1 / 2, the phenol of 18.8g and 30ml ethanol solution Add it to a four-necked flask equipped with a condenser, a thermometer, an electric stirrer and a thermocouple. Raise the temperature to 60°C, then add 6.2g of boric acid, and at the same time adjust the pH value of the solution in the four-necked flask with 0.1mol / L potassium hydroxide solution. The reaction time is 6 hours, and the vacuum degree is 0.1-1KPa. When the liquid is clear and slightly orange, and when there is no water after long-term pumping, stop pumping.

[0024] Step (2) Add 10.2 g of paraformaldehyde with a molecular weight of 200, make it react at 80° C. while stirring, and dehydrate under reduced pressure. As the dehydration proceeds, the liquid in the reaction bottle gradually becomes viscous. After 5-6 hours of reaction, when it is yellow-green, stop the r...

Embodiment 3

[0025] Embodiment 3: the mol ratio of the boric acid / phenol of embodiment 1 step (1) is changed into 2 / 1 by 1 / 3, by the mol ratio of boric acid / phenol=2 / 1, the phenol of 9.4g and 20ml tetrahydrofuran solution Add it to a four-necked flask equipped with a condenser, a thermometer, an electric stirrer and a thermocouple. Raise the temperature to 90°C, then add 12.4g of boric acid, and at the same time use 0.1mol / L calcium carbonate solution to adjust the pH value of the solution in the four-necked flask. Reaction, vacuum decompression and dehydration at the same time, the reaction time is 4 hours, the vacuum degree is 0.1 ~ 1KPa; when the liquid is clear and slightly orange, and when there is no water after long-term pumping, stop pumping;

[0026] Step (2) Add 10.2 g of paraformaldehyde with a molecular weight of 200, make it react at 80° C. while stirring, and dehydrate under reduced pressure. As the dehydration proceeds, the liquid in the reaction bottle gradually becomes vi...

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Abstract

Production of modified phenolic resin of high-boron content is carried out by reacting boric acid with carbolic acid to generate boric acid ester by two-step method, reacting boric acid ester with paraformaldehyde to obtain final product. It is simple, controllable and quantitative, has higher boron content, excellent thermal, mechanical, friction and anti-corrosive performances. It can be used for high-temperature brake friction material, anti-corrosive materials and special thermal-insulating material.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of boron-modified phenolic resin with high boron content. technical background [0002] Phenolic resin is the first synthetic resin to realize industrial production in the world, and it has a history of nearly a hundred years so far. Due to its easy availability of raw materials, low price, simple production process and equipment, more importantly, it has excellent mechanical properties, heat resistance, ablation resistance, electrical insulation, dimensional stability, molding processability and flame retardancy , Phenolic resin has become an indispensable material in the industrial sector, and is widely used in the fields of aircraft and aviation, military equipment, automobiles and transportation, and construction. However, with the development of industry, especially the development of aerospace and other cutting-edge defense technologies, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
Inventor 邱军王国建
Owner TONGJI UNIV
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