Preparation method of boron modified phenolic resin

A technology of phenolic resin and boron modification, applied in the field of phenolic resin preparation, can solve the problems of difficult production control and large-scale industrial production, achieve excellent thermal oxidation resistance, facilitate large-scale industrial production, and have mild reaction conditions Effect

Active Publication Date: 2010-08-18
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent 200610024515.0 provides a method for preparing a modified phenolic resin with high boron content, but the resin prepared in this invention is a thermosetting resin, which is difficult to control in production. Improper control will solidify in the reactor, and it is difficult to realize large-scale industrial production

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  • Preparation method of boron modified phenolic resin
  • Preparation method of boron modified phenolic resin

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preparation example Construction

[0021] A preparation method of boron modified phenolic resin, comprising the following steps:

[0022] (1), add phenol and aldehyde that molar ratio is 1.0:0.1~1.0 in the reactor, stir reflux reaction in acidic environment for 5 hours~6 hours;

[0023] (2), the reaction product of step (1) carries out normal pressure distillation dehydration, to water content less than 10% by weight;

[0024] (3) Add a boron-containing hydroxy compound to the dehydrated product in step (2) for esterification; the amount of the boron-containing hydroxy compound is at most 20% by weight of the phenol.

[0025] The preparation method of above-mentioned boron-modified phenolic resin, at first adopts traditional synthetic method to prepare phenolic resin, just limits the condition of reaction under acidic environment, promptly adds acidic solution in reactor, thereby makes the phenolic resin that synthetically obtains be Linear structure, that is, thermoplastic phenolic resin. The thermoplastic p...

Embodiment 1

[0029] Put 500g of phenol, 301g of 37% formaldehyde solution, and 5g of oxalic acid into a 1000ml reaction vessel equipped with a thermometer, a stirring device, and a reflux condenser, heat up to 80°C to 85°C for 1 hour, and then heat up to 90°C to 95°C, keep the temperature for 1 hour, finally raise the temperature to 100°C, reflux for 3 hours, end the reaction and carry out atmospheric distillation dehydration, atmospheric distillation dehydration to 150°C ~ 160°C, when the moisture content in the resin is detected to be 2.3%, stop the atmospheric pressure Distillation, adding 50g of boric acid, esterification reaction for 30 minutes, then under the conditions of 150℃~160℃, pressure 8000Pa, vacuum distillation dehydration, dephenolization, when the detected moisture content is 4.3%, stop vacuum distillation, release the material to cool , to obtain 530g of boron-modified phenolic resin A.

Embodiment 2

[0031] Put 445g of phenol and 4.45g of sulfuric acid with a content of 20% into a 1000ml reaction vessel equipped with a thermometer, a stirring device, and a reflux condenser, heat up to 80°C to 90°C, start adding formaldehyde dropwise, finish adding in 90 minutes, and then Heat up to 100°C, reflux for 3 hours, add barium hydroxide to neutralize, end the reaction and carry out atmospheric distillation dehydration, atmospheric distillation dehydration to 160°C ~ 170°C, when the moisture content is 1.2%, stop atmospheric distillation, add Boric acid 66g, esterification reaction for 40 minutes, then dehydration and dephenolization by vacuum distillation under the conditions of 160°C-170°C and pressure 5000Pa, when the detected moisture content is 3.7%, stop the vacuum distillation, release the material to cool, and obtain 408g boron Modified phenolic resin B.

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Abstract

The invention discloses a preparation method of boron modified phenolic resin, which comprises the following steps that: (1) phenol and formaldehyde in the molar ratio of 1.0:0.1 to 1.0 is added into a reactor, to be stirred under acid environment and reflux for 5 to 6 hours; (2) a reaction product prepared in step (1) is distilled and hydrated at normal pressure, until the water content is less than 10 weight percent; (3) the produce dehydrated in step (2) is added with a compound which contains boron hydroxyl, to have esterification; and the input of the compound which contains boron hydroxyl is 20 weight percent of that of the phenol at most. The synthesis method provided by the invention is simple and feasible, the prepared resin has stable performance and is beneficial to large-scaleindustrial production, and the prepared boron modified phenolic resin has excellent thermal oxidation and ablation resistant performance, and can be widely applied to high-temperature brake materials, ablation resistant materials, heat insulation materials and other fields.

Description

technical field [0001] The invention relates to a preparation method of phenolic resin, in particular to a preparation method of boron modified phenolic resin. Background technique [0002] Phenolic resin, due to its excellent mechanical properties, heat resistance, ablation resistance, electrical insulation, dimensional stability, molding processability and flame retardancy, its raw materials are readily available, low in price, and its production process and equipment are simple. , has become an indispensable material in the industrial sector. However, with the development of industry, especially the development of aerospace and other cutting-edge defense technologies, traditional unmodified phenolic resins still have disadvantages such as high brittleness, poor toughness and low heat resistance, which limits the application of high-performance materials. develop. In order to meet the development needs of the automobile industry, aerospace and national defense industry, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
Inventor 唐路林刘卫刘翠华李枝芳
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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