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Silsesquioxane-modified hybrid phenolic resin, and preparation method and application thereof

A technology of silsesquioxane and phenolic resin, which is applied in the field of hybrid phenolic resin and its preparation, can solve the problems of reduced ablation resistance, reduced carbon residue rate, and reduced ablation efficiency, so as to improve ablation resistance , low chemical toxicity, increased strength and ablation resistance

Inactive Publication Date: 2018-08-14
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the literature of YueWu et al. (Polymer Bulletin, 2013, 70:3261-3277), the method of octaphenyl POSS molecule modification of thermoplastic phenolic resin was reported, and the whole reaction system used tetrahydrofuran as a solvent medium, and the obtained modified phenolic resin, The initial decomposition temperature of the modified phenolic resin is increased from 312°C of the pure resin to 385°C, but the carbon residue rate is reduced from 65% to about 58%, the ablation resistance is significantly reduced, and the ablation efficiency is reduced

Method used

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  • Silsesquioxane-modified hybrid phenolic resin, and preparation method and application thereof
  • Silsesquioxane-modified hybrid phenolic resin, and preparation method and application thereof
  • Silsesquioxane-modified hybrid phenolic resin, and preparation method and application thereof

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preparation example Construction

[0041] The embodiment of the present invention also provides a preparation method of a silsesquioxane-modified hybrid phenolic resin, which includes the following steps:

[0042] Step 1. Dissolve silsesquioxane in an alcohol solvent to obtain a silsesquioxane solution;

[0043] Step 2. Add the phenolic resin solution to the silsesquioxane solution, stir and mix to obtain a hybrid resin solution;

[0044] Step 3. Exhaust the solvent in the hybrid resin solution in a vacuum at 50-70°C, and then heat up and cure to obtain a silsesquioxane-modified hybrid phenolic resin, wherein the silsesquioxane has the following The molecular structure:

[0045]

[0046] Among them, R is isobutyl, phenyl or isooctyl, R 1 For H or

[0047] In the method for preparing a silsesquioxane-modified hybrid phenolic resin provided by the embodiment of the present invention, the POSS molecule represented by formula (1) is reacted with the phenolic resin to form a hybrid with POSS molecules as chemical crosslinki...

Embodiment 1

[0056] Weigh 10 g of trisilanol phenyl POSS molecules, dissolve them in 15 g of ethanol solvent, and stir thoroughly until completely dissolved into a transparent state to obtain a POSS solution with a concentration of 40 wt%. Weigh 120 g of an ethanol solution of barium phenolic resin with a solid content of 75%, add the POSS molecule solution to the barium phenolic solution, and mechanically stir at room temperature for 2 hours until it is uniformly mixed to obtain a hybrid resin solution. Then transfer the phenolic resin hybrid solution to a vacuum oven, evacuating at 50°C for half an hour, then raising it to 55°C for half an hour, and then raising to 60°C for about 45 minutes. Pour the hybrid resin solution from which the solvent has been drained into the mold, put it into the curing oven, and raise the temperature from room temperature to 90°C at a heating rate of 0.5°C / min, keep it for 1 hour, and then increase the temperature at 0.2°C / min The rate was increased to 120°C,...

Embodiment 2

[0058] Weigh out 5 g of trisilanol phenyl POSS molecules, dissolve them in 15 g of ethanol solvent, and stir thoroughly until completely dissolved into a transparent state to obtain a POSS solution with a concentration of 25 wt%. Weigh 136 g of an ethanol solution of a high-carbon phenolic resin with a solid content of 70%, add the POSS molecular solution to the barium phenolic solution, and mechanically stir for 2 hours at room temperature until it is uniformly mixed to obtain a hybrid resin solution. Then transfer the phenolic resin hybrid solution to a vacuum oven, evacuating at 50°C for half an hour, then raising it to 55°C for half an hour, and then raising to 60°C for about 45 minutes. Pour the hybrid resin solution from which the solvent has been drained into the mold, put it into the curing oven, and raise the temperature from room temperature to 90°C at a heating rate of 0.5°C / min, keep it for 1 hour, and then increase the temperature at 0.2°C / min The rate is increased...

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Abstract

The invention relates to a silsesquioxane-modified hybrid phenolic resin, and a preparation method and an application thereof, and belongs to the field of high-performance resin matrix composite materials. The silsesquioxane-modified hybrid phenolic resin provided by the embodiment of the invention is a hybrid phenolic resin cured product with a POSS molecule as a chemical crosslinking point, formed through reacting the POSS molecule represented by formula (1) with phenolic resin, and the addition of a POSS hybrid molecule strengthens nanoparticles, so the initial maximum decomposition temperature of the resin is improved to about 580 DEG C from 450 DEG C of pure resin, the residual weight is increased to about 65% from 58%, and the ablation resistance of the material is remarkably improved; and the POSS-modified hybrid phenolic resin provided by the invention has potential application prospects in the field of aerospacecraft resin-based advanced thermal protection materials.

Description

Technical field [0001] The invention relates to a semi-cage polyhedral silsesquioxane (POSS) molecularly modified hybrid phenolic resin and a preparation method thereof, and belongs to the field of high-performance resin-based composite materials. Background technique [0002] As the thermal environment of aerospace vehicles continues to change, the material requirements for thermal protection systems are also constantly changing. With the advent of nearby spacecraft, ablative thermal protection materials face the test of aerobic environment while facing high temperature ablation environment. The resin-based ablation and heat-proof composite material with phenolic resin as the main matrix can form a stable and strong carbon layer structure after ablation and carbonization, resist the erosion of heat flow, and increase the effect of high-temperature radiation. However, in an aerobic environment, the porous carbonized layer formed by ablation can easily be O 2 Molecular corrosion ...

Claims

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Application Information

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IPC IPC(8): C08L61/06C08L83/04C08J3/24
CPCC08J3/246C08J2361/06C08J2483/04C08L61/06C08L2312/00C08L83/04
Inventor 冯志海师建军孔磊左小彪余瑞莲严蛟
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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