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Ablative material of resin of phenolic cyanate

A technology of phenolic cyanate ester and ablation material, applied in the field of high temperature resistant ablation material, can solve the problems of low carbon content, high melt viscosity and high content of heteroatoms

Inactive Publication Date: 2005-03-30
北京玻钢院复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The phenolic novolak cyanate resin system modified by fused ring phenol used as ablative resin has been described in US Patents 4,831,086 and 4,981,994. Esterification, and since it is necessary to use higher molecular weight novolac phenolic formaldehyde as the main structure to achieve a higher carbon residue rate, this will lead to a higher melt viscosity at 100 ° C, and although the novolac cyanate has a higher The glass transition temperature and thermal decomposition temperature, but the heteroatom content is high, the carbon content is low, and it has certain limitations in materials that need to obtain a high carbon residue rate.

Method used

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  • Ablative material of resin of phenolic cyanate
  • Ablative material of resin of phenolic cyanate
  • Ablative material of resin of phenolic cyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: synthetic novolac cyanate

[0027] A 37% aqueous solution of phenol and formaldehyde and oxalic acid in a molar ratio of 1:0.9:0.005 are put into a three-necked flask equipped with a reflux condenser, reacted at 80-100°C for 3-5 hours, washed with water, and vacuumized to obtain the softening point The novolac between 40 and 60°C, the novolac is dissolved in the mixed solvent of dichloromethane and ethyl acetate, put into the four-necked bottle together with BrCN, drop triethylamine, phenolic hydroxyl group and BrCN and triethylamine The molar ratio is 1:1.05:1.10, react at -15°C to -5°C for 5 hours, separate the salt and solvent, and perform purification treatment to obtain novolac cyanate. In this example n=2~5, m=0.

[0028] 1-2: Using the same method as 1-1, change phenol to p-phenylphenol to obtain novolac cyanate. In this example n=2~5, m=0.

[0029] 1-3: Using the same method as 1-1, change phenol to o-phenylphenol to obtain novolac cyanate. In ...

Embodiment 2

[0031] Embodiment 2: Synthesis of linear fused ring phenolic cyanate

[0032] 2-1: A 37% aqueous solution of 1-naphthol and formaldehyde and oxalic acid in a molar ratio of 1:0.80:0.005 are put into a three-necked flask equipped with a reflux condenser, in the presence of a ketone solvent, at 60-100°C React for 3 to 5 hours, wash with water, and vacuumize to obtain linear condensed ring phenol novolac with a softening point between 40 and 60°C. Dissolve linear fused-ring phenolic aldehyde in dichloromethane solvent, put it into a four-necked flask together with BrCN, add triethylamine dropwise, the molar ratio of phenolic hydroxyl group to BrCN and triethylamine is 1:1.05:1.10, and store it at -15°C~ React at -5°C for 5 hours, separate the salt and solvent, and perform purification treatment to obtain linear fused ring phenol novolac cyanate. In this example n=0, m=2~5.

[0033] 2-2: Using the same method as 2-1, use 2-naphthol and polyoxymethylene as raw materials to obtain...

Embodiment 3

[0035] Embodiment 3: synthetic copolymerization type phenolic cyanate

[0036] 3-1: 37% aqueous solution of phenol, naphthol (molar ratio is 1: 1) and formaldehyde and oxalic acid according to phenol, aldehyde, acid molar ratio 1: 0.9: 0.005, drop in the three-necked flask that is equipped with reflux condenser, React at 80-100°C for 3-5 hours, wash with water, and vacuumize to obtain copolymerized phenolic formaldehyde. The copolymerized phenolic formaldehyde is dissolved in acetone solvent, put into a four-necked bottle with BrCN, and triethylamine, phenolic hydroxyl group and BrCN are added dropwise. And the molar ratio of triethylamine is 1:1.05:1.10, react at -15°C to -5°C for 5 hours, separate the salt and solvent, and perform purification treatment to obtain copolymerized phenolic cyanate. In this example n:m=1:1.

[0037] 3-2: Change the molar ratio of phenol and naphthol to 1:2, and obtain the copolymerized phenolic novolac cyanate in the same way as 3-1 with benzald...

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Abstract

The invention provides a phenolic cyanate resin ablator composed by mixture of alloied linear phenolic cyanate resin and linear fused ring phenolic cyanate resin and strengthen material which can satisfy the demand of high corbon residu ratio (>60 percent), high heat-resistance temp. (>350 deg.C), low fusant viscosity, low solidify agravity ratio and long gel time.

Description

[0001] This application is a divisional case of the patent application whose application date is July 8, 2003 and whose application number is 03146583.8. technical field [0002] The invention relates to a high-temperature-resistant ablation material suitable for injection molding. The material is formed by mixing a resin with low melt viscosity, no small molecules released during solidification, high heat-resistant temperature and carbon residue rate, and a reinforcing material. become. Background of the invention [0003] At present, the really mature ablation resin is only thermosetting phenolic resin, but because its curing system is a condensation polymerization system, a large amount of small molecular substances are released during curing, and because of its high viscosity, it must be dissolved in an inert solvent such as ethanol before it can be used. , so the ablative resin of this system is suitable for more mature molding, winding and other processes, but not suit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08L61/14
Inventor 冯青平薛忠民陈淳胡平
Owner 北京玻钢院复合材料有限公司
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