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Ablation-resistant phenolic cyanate prepreg and preparation method thereof

A technology of phenolic cyanate ester and prepreg, which is applied in the field of prepreg, which can solve the problems of prepreg prepared by hot melt method, high porosity of cured product, and difficulty in precise control of resin content, so as to achieve controllable curing process Good performance, high curing degree, good spreading effect

Active Publication Date: 2020-02-21
长春长光宇航复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the present invention solves the problem that the phenolic cyanate resin in the prior art is a low-viscosity liquid at room temperature, resulting in a high porosity of the cured product, which cannot be used to prepare prepregs by hot-melt method, and the resin content is difficult to accurately control. and other technical problems, providing a kind of ablation-resistant phenolic cyanate ester prepreg and its preparation method

Method used

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  • Ablation-resistant phenolic cyanate prepreg and preparation method thereof
  • Ablation-resistant phenolic cyanate prepreg and preparation method thereof
  • Ablation-resistant phenolic cyanate prepreg and preparation method thereof

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preparation example Construction

[0031] The preparation method of ablation-resistant phenolic cyanate ester prepreg of the present invention may further comprise the steps:

[0032] Step 1, synthesis of phenolic cyanate ester resin oligomer;

[0033] Step 2, modifying and prepolymerizing the phenolic cyanate resin oligomer to obtain a prepolymer;

[0034] Step 3, preparing a single-layer adhesive film with the prepolymer of step 2;

[0035] Step 4, introducing the unidirectional fiber or fiber cloth into the middle of the two single-layer adhesive films, and preparing the ablation-resistant phenolic cyanate prepreg by the hot-melt method.

[0036] In the above technical scheme, the process of step 1 is to dissolve the novolac resin and cyanogen bromide in an organic solvent, lower the temperature to below -10°C, and add the compound catalyst drop by drop under continuous stirring. The process ensures that the temperature is less than -5°C, and continues to stir for more than 2.5 hours to complete the reacti...

Embodiment 1

[0046] Step 1. Weigh 410.87g of novolac resin and 500g of cyanogen bromide, dissolve them in 2000mL of acetone, drop the temperature to -10°C in a dry ice bath, and add the compound catalyst dropwise under continuous stirring (the compound catalyst has a molar ratio of 3 : 1 mixture of triethylamine and DBU, the molar ratio of novolac resin to composite catalyst is 1:1.2), the interval between each drop is 10s, the whole dropping process ensures that the temperature is less than -5°C, continue to stir for 2.5h to make the reaction complete , using deionized water to wash repeatedly until the pH value is 6.5 to 7.0, rotary evaporation to remove water, and vacuum drying to obtain a phenolic cyanate resin oligomer.

[0047] Step 2. Weigh 500g of the phenolic cyanate ester resin oligomer prepared in step 1. After melting at 120°C, add 200ppm copper naphthenate and 0.5g cobalt acetylacetonate while stirring, pre-polymerize at 110°C for 80min, add 25g bis Phenol A-type epoxy resin E...

Embodiment 2

[0051] Step 1. Weigh 448.22g of novolac resin and 500g of cyanogen bromide, dissolve them in 1500mL of dichloromethane, drop the temperature to -15°C in a dry ice bath, and add the compound catalyst drop by drop under continuous stirring (the compound catalyst is molar ratio It is a mixture of triethylamine and DBU of 3:1, the molar ratio of novolac resin to compound catalyst is 1:1.2), the interval between each drop is 10s, the temperature of the whole dropping process is guaranteed to be less than -10°C, and the stirring is continued for 3h to make the reaction Completely, use deionized water to wash repeatedly until the pH value is 6.5 to 7.0, remove water by rotary evaporation, and dry in vacuum to obtain a phenolic cyanate resin oligomer.

[0052] Step 2. Weigh 500 g of the phenolic cyanate ester resin oligomer prepared in Step 1. After melting at 120 ° C, add 15 g of nonylphenol, 25 g of cobalt octanoate and 0.5 g of cobalt acetylacetonate while stirring, and pre-polymeri...

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Abstract

The invention discloses an ablation-resistant phenolic cyanate prepreg and a preparation method thereof, and belongs to the technical field of prepregs. The technical problems of failed hot melting process preparation of the prepreg and difficult accurate control of the resin content due to high porosity of a cured product of existing phenolic cyanate resin being a low-viscosity liquid at room temperature are solved. The preparation method comprises the following steps: firstly preparing a phenolic cyanate resin oligomer from linear phenolic resin, cyanogen bromide and a compound catalyst, modifying and pre-polymerizing the oligomer to obtain a prepolymer, preparing a single-layer adhesive film by using the prepolymer, introducing a unidirectional fiber or a fiber cloth between the two single-layer adhesive films, and carrying a hot melting process to prepare the ablation-resistant phenolic cyanate prepreg. The prepreg has a good paving performance and excellent ablation resistance, allows the room-temperature working life to be longer than 15 days, the volatile matter content to be smaller than 1% and the gelation time at 100 DEG C to be longer than 2 hours, and has a high curingdegree, a matrix resin formed after curing the prepreg has high thermal decomposition temperature and a high residual carbon ratio, and a composite material of the resin has the advantages of low porosity, excellent mechanical properties and excellent toughness.

Description

technical field [0001] The invention belongs to the technical field of prepregs, and in particular relates to an ablation-resistant phenolic cyanate prepreg and a preparation method thereof. Background technique [0002] Phenolic resin is a resin made by polycondensation of phenol and formaldehyde under catalyst conditions, neutralization and water washing. Due to the choice of catalyst, it can be divided into two types: thermosetting and thermoplastic. Phenolic resin has good acid resistance, mechanical properties and heat resistance, so it is widely used in anti-corrosion engineering, adhesives, flame retardant materials, grinding wheel manufacturing and other industries. However, phenolic resins have the following defects: one, phenolic resins contain solvents, and the volatilization of solvents can easily lead to excessive porosity of the product and cause environmental pollution; The process needs to deflate and drain under different temperature gradients, the curing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/24C08G8/28C08L61/14
CPCC08J5/24C08J2361/14
Inventor 商伟辉杨柳周玉姜昊林再文
Owner 长春长光宇航复合材料有限公司
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