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Zirconium-modified phenolic resin and preparation method thereof

A phenolic resin and modification technology, applied in the field of zirconium-modified phenolic resin and its preparation, can solve the problems of low thermo-oxidative stability and carbon residue rate of cured products, difficult to meet higher requirements for ablation resistance, etc. Significant economic and social benefits, low cost, good heat resistance effect

Active Publication Date: 2013-06-26
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when used as the matrix of ablation-resistant resin-based composites or converted into matrix carbon of C / C composites, traditional PF has a large amount of low-molecular volatiles generated during the curing process, thermal oxygen stability of the cured product, and carbon residues. It is difficult to meet the higher requirements of ablation resistance as an aerospace material.

Method used

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  • Zirconium-modified phenolic resin and preparation method thereof
  • Zirconium-modified phenolic resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0016] 1) Feed according to the mass fraction of phenol and formaldehyde as 24 parts and 10 parts respectively, and add 2.5g of sodium hydroxide solution with a mass fraction of 40% as a catalyst, heat up to 70°C while stirring, and react for 1h;

[0017] 2) According to the parts by mass: 40 parts of ethanol, 20 parts of acetylacetone, 20 parts of zirconium oxychloride, 1 part of hydrogen peroxide to configure zirconium oxychloride solution;

[0018] 3) Adjust the temperature of the constant temperature water bath to 95°C, add the prepared zirconium oxychloride solution dropwise, and control the pH value of the solution to 8-9;

[0019] 4) After the temperature reaches 95°C, keep warm for 2 hours, then discharge;

[0020] 5) Put the product obtained in the previous step into a vacuum drying oven at 50°C for 5 hours to obtain a zirconium-modified phenolic resin.

Embodiment 2

[0022] 1) Feed according to the mass fraction of phenol and formaldehyde as 24 parts and 10 parts respectively, and add 2 g of sodium hydroxide solution with a mass fraction of 40% as a catalyst, heat up to 70°C while stirring, and react for 1 hour;

[0023] 2) According to the parts by mass: 40 parts of ethanol, 20 parts of acetylacetone, 10 parts of zirconium oxychloride, and 1 part of hydrogen peroxide are used to configure zirconium oxychloride solution;

[0024] 3) Adjust the temperature of the constant temperature water bath to 85°C, add the prepared zirconium oxychloride solution dropwise, and control the pH value of the solution to 8-9;

[0025] 4) After the temperature reaches 85°C, keep warm for 2 hours, then discharge;

[0026] 5) Put the product obtained in the previous step into a vacuum drying oven at 50°C for 5 hours to obtain a zirconium-modified phenolic resin.

Embodiment 3

[0028] 1) Feed 24 parts and 10 parts by mass of phenol and formaldehyde respectively, and add 1.5g of sodium hydroxide solution with a mass fraction of 40% as a catalyst, heat up to 70°C while stirring, and react for 1h;

[0029] 2) According to the parts by mass: 40 parts of ethanol, 20 parts of acetylacetone, 15 parts of zirconium oxychloride, 1 part of hydrogen peroxide to prepare zirconium oxychloride solution;

[0030] 3) Adjust the temperature of the constant temperature water bath to 85°C, add the prepared zirconium oxychloride solution dropwise, and control the pH value of the solution to 8-9;

[0031] 4) After the temperature reaches 85°C, keep warm for 2.5 hours, then discharge;

[0032] 5) Put the product obtained in the previous step into a vacuum drying oven at 50°C for 5 hours to obtain a zirconium-modified phenolic resin.

[0033] The high temperature resistance of the zirconium modified phenolic resin prepared by the invention is better than that of common phe...

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Abstract

The invention relates to a zirconium-modified phenolic resin and a preparation method thereof. The zirconium-modified phenolic resin is technically characterized by being prepared from the following raw materials in parts by weight: 20-50 parts of phenol, 9-20 parts of formaldehyde, 2-10 parts of sodium hydroxide, 20-40 parts of ethanol, 10-20 parts of acetylacetone, 5-20 parts of zirconium oxychloride, and 0.5-2 parts of hydrogen peroxide. The preparation method comprises the following steps of: charging raw materials, refluxing, stirring, dropwise adding zirconium oxychloride ethanol solution, adjusting the pH value, discharging, and removing the solvent to obtain the zirconium-modified phenolic resin. The preparation method is simple, the cost is low, the content of zirconium is controllable, the prepared zirconium-modified phenolic resin has higher carbon yield, as well as good heat resistance, ablation resistance and mechanical property, is wide in application range, and has obvious economic and social benefits.

Description

technical field [0001] The invention belongs to the field of modified polymers, and in particular relates to a zirconium-modified phenolic resin and a preparation method thereof. Background technique [0002] Generally, the polymer formed by polycondensation of phenols and aldehydes under the action of a catalyst is called phenolic resin (PF). As one of the three major thermosetting resins, PF has been widely used due to its advantages of low price, heat resistance, ablation resistance, flame retardancy, less smoke, and good workmanship, and is still used as the main material for resin-based ablation-resistant materials. Base resin. However, when used as the matrix of ablation-resistant resin-based composites or converted into matrix carbon of C / C composites, traditional PF has a large amount of low-molecular volatiles generated during the curing process, thermal oxygen stability of the cured product, and carbon residues. However, it is difficult to meet the higher require...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
Inventor 李克智刘长青张守阳张雨雷李贺军
Owner NORTHWESTERN POLYTECHNICAL UNIV
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