Preparation method of amino POSS graft modified ablation-resistant phenolic resin and phenolic resin thereof

A technology of methylol phenolic resin and graft modification, applied in the field of phenolic resin and modified phenolic resin, can solve the problems of unsatisfactory ablation resistance and low modification efficiency of modified phenolic resin, and achieve the promotion of high-efficiency chemical Reaction modification, improvement of modification efficiency, excellent effect of ablation resistance

Pending Publication Date: 2020-06-05
北京玻钢院复合材料有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] The technical problem solved by the present invention is that the modification efficiency of phenolic resin by POSS is not high in the prior art, and the ablation resistance of the obtained modified phenolic resin is not ideal enough, and then a kind of amino POSS graft-modified anti-ablation is provided. Preparation method of ablation phenolic resin

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  • Preparation method of amino POSS graft modified ablation-resistant phenolic resin and phenolic resin thereof
  • Preparation method of amino POSS graft modified ablation-resistant phenolic resin and phenolic resin thereof
  • Preparation method of amino POSS graft modified ablation-resistant phenolic resin and phenolic resin thereof

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[0029] The preparation method of the ablation-resistant phenolic resin of amino POSS graft modification of the present invention, comprises the steps:

[0030] (1) get phenol and aldehyde according to the molar ratio of 1:(1.0~1.5), then add catalyst wherein, react to generate the polymer containing hydroxymethyl phenolic resin;

[0031] (2) get amino POSS, the mass ratio of described amino POSS and the described phenol in step (1) is (1~10): 100, it is dissolved in the solvent, forms amino POSS solution;

[0032] (3) Add the amino POSS solution in the step (2) to the hydroxymethyl-containing phenolic resin polymer in the step (1), and react to generate the ablation-resistant phenolic resin modified by the amino POSS grafting resin.

Embodiment 1

[0034] In the present embodiment, the preparation method of the ablation-resistant phenolic resin modified by amino POSS grafting comprises the following steps:

[0035] (1) Get phenol and formaldehyde according to the molar ratio of 1:1.2, add formaldehyde to the phenol after stirring under stirring, stir evenly, add catalyst barium hydroxide to wherein after cooling again, the quality of barium hydroxide accounts for 1 / 3 of the quality of phenol 1%, from room temperature to 80 ° C, through condensation reaction to generate a polymer containing hydroxymethyl phenolic resin;

[0036] (2) Get the cage type 8-anilino POSS, the mass ratio of the cage type 8-anilino POSS to the phenol in step (1) is 5:100, dissolve it in acetone to form an amino POSS solution ;

[0037] (3) After the condensation reaction in the step (1) is carried out for 1.5h, add the amino POSS solution described in the step (2) to the described hydroxymethyl phenolic resin polymer in the step (1), at 80 ~ Co...

Embodiment 2

[0042] In the present embodiment, the preparation method of the ablation-resistant phenolic resin modified by amino POSS grafting comprises the following steps:

[0043] (1) get methyl phenol and formaldehyde according to the mol ratio of 1:1.3, add formaldehyde in methyl phenol under stirring, stir evenly, add catalyst ammonia water to wherein after cooling again, ammonia water accounts for 0.5% of methyl phenol quality, From room temperature to 80°C, the condensation reaction produces a polymer containing hydroxymethyl phenolic resin;

[0044] (2) Get the cage type 8-anilino POSS, the mass ratio of the cage type 8-anilino POSS to the phenol in step (1) is 8:100, dissolve it in acetone to form amino POSS solution ;

[0045] (3) After the condensation reaction in the step (1) is carried out for 1h, add the amino POSS solution described in the step (2) to the described hydroxymethyl phenolic resin polymer in the step (1), at 80~95 Continue to react at a temperature of ℃ to th...

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Abstract

The invention provides a preparation method of amino POSS (polyhedral oligomeric silsesquioxane) graft modified ablation-resistant phenolic resin, which comprises the following steps: preparing phenoland aldehyde according to the molar ratio of 1:(1.0-1.5), adding a catalyst, and carrying out a reaction to generate a hydroxymethyl-containing phenolic resin polymer; preparing amino POSS, wherein the mass ratio of the amino POSS to the phenol in the step (1) is (1-10):100, and dissolving the amino POSS and the phenol in the step (1) in a solvent to form an amino POSS solution; and adding the amino POSS solution into the polymer containing hydroxymethyl phenolic resin, and carrying out a reaction until the amino POSS graft modified ablation-resistant phenolic resin is generated. The invention also provides the phenolic resin prepared by the preparation method of the amino POSS graft modified ablation-resistant phenolic resin. The preparation method is high in modification efficiency, andthe obtained modified phenolic resin is excellent in ablation resistance.

Description

technical field [0001] The invention belongs to the field of modified phenolic resins, and in particular relates to a preparation method of an amino POSS graft-modified ablation-resistant phenolic resin and the phenolic resin. Background technique [0002] Based on its good heat resistance, ablation resistance, and flame retardancy, phenolic resin is mostly used as a general-purpose matrix resin for heat-resistant and ablation-resistant materials. With the development of aerospace and national defense cutting-edge technologies, traditional phenolic resins are gradually unable to meet the needs of modern industries in terms of ablation resistance and mechanical properties. The residual carbon rate of phenolic resin is low, and it degrades seriously during the high-temperature ablation process, resulting in holes and cracks in the material. Therefore, the matrix material with a high residual carbon rate is the development direction of ablation-resistant materials, and the heat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
CPCC08G8/28
Inventor 姚亚琳刘晶王雷贾晨辉田谋锋
Owner 北京玻钢院复合材料有限公司
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