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Flame-retardant co-curing agent, preparation method thereof, intrinsic high-thermal-conductivity/flame-retardant liquid crystal epoxy resin material and preparation method of epoxy resin material

A technology of co-curing agent and epoxy resin, applied in the field of intrinsic high thermal conductivity/flame retardant liquid crystal epoxy resin material and its preparation, flame retardant co-curing agent and its preparation, can solve the problem of poor compatibility and thermal stability Problems such as poor quality and high price

Active Publication Date: 2021-08-13
RES & DEV INST OF NORTHWESTERN POLYTECHNICAL UNIV IN SHENZHEN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In addition, different types of flame retardant co-curing agents have different flame retardant properties: P series flame retardant co-curing agents have low smoke and low toxicity, but have the problems of high volatility and poor thermal stability; Si-based flame retardant co-curing agents The agent has the advantages of low burning rate, low release, anti-dripping, low smoke, and low CO generation, but when it is used alone, it often has poor compatibility with the matrix and the price is high

Method used

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  • Flame-retardant co-curing agent, preparation method thereof, intrinsic high-thermal-conductivity/flame-retardant liquid crystal epoxy resin material and preparation method of epoxy resin material
  • Flame-retardant co-curing agent, preparation method thereof, intrinsic high-thermal-conductivity/flame-retardant liquid crystal epoxy resin material and preparation method of epoxy resin material
  • Flame-retardant co-curing agent, preparation method thereof, intrinsic high-thermal-conductivity/flame-retardant liquid crystal epoxy resin material and preparation method of epoxy resin material

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preparation example Construction

[0036] The present invention also provides a preparation method of the flame retardant co-curing agent described in the above technical solution, comprising the following steps:

[0037] mixing p-hydroxybenzaldehyde, amino-terminated polysilsesquioxane and an organic solvent to perform a first substitution reaction to obtain a first substitution reaction feed liquid;

[0038] The first substitution reaction liquid and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide are mixed for a second substitution reaction to obtain the flame retardant co-curing agent.

[0039] In the present invention, unless otherwise specified, the raw materials used in the present invention are preferably commercially available products.

[0040] The invention mixes p-hydroxybenzaldehyde, amino-terminated polysilsesquioxane and an organic solvent to perform a first substitution reaction to obtain a first substitution reaction feed liquid.

[0041] In the present invention, the molar ratio of p-hydro...

Embodiment 1

[0073] 0.1 mol of p-hydroxybenzaldehyde (PHBA) and 0.1 mol of amino-terminated polysilsesquioxane (NH 2 -POSS) was dissolved in a mixed solution of THF and EtOH with a volume ratio of 1:1, and the first substitution reaction was carried out at 80°C for 12 hours; then 0.1mol of 9,10-dihydro-9-oxa was added to the above reaction system -10-phosphaphenanthrene-10-oxide (DOPO), proceed to the second substitution reaction at 80°C for 12h; remove dissolved THF and EtOH by rotary evaporation, and wash the solid residue with distilled water and EtOH; finally at 60°C Dry overnight in a vacuum oven to obtain a flame retardant co-curing agent (DOPO-POSS).

[0074] The flame retardant co-curing agent (DOPO-POSS) that present embodiment prepares 1 H NMR picture as figure 1 shown. from figure 1 It can be seen that: NH 2 The characteristic peaks of protons on the -POSS molecule appear at 2.6ppm, 1.8ppm, 1.3ppm, 1.0ppm and 0.6ppm, and the multiplets at 4.2ppm and 3.8ppm are from -NH-CH- ...

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Abstract

The invention relates to the technical field of epoxy resin materials, and especially relates to a flame-retardant co-curing agent, a preparation method thereof, an intrinsic high-thermal-conductivity / flame-retardant liquid crystal epoxy resin material and a preparation method of the epoxy resin material. The flame-retardant co-curing agent provided by the invention has a structure as shown in a formula I. Metaphosphoric acid generated by decomposition of the flame-retardant co-curing agent at high temperature is a strong dehydrating agent, and can promote rapid dehydration and carbonization of the surface of discotic liquid crystal epoxy resin to form a P-containing carbon layer; the Si element is oxidized into SiO2 which tends to migrate towards the surface of the discotic liquid crystal epoxy resin due to low surface energy, so that a Si-containing protective layer is formed, a P-containing carbon layer is protected from oxidative degradation, the strength and density of the carbon layer can be increased, a high-efficiency compact heat insulation layer for isolating heat and air is formed, and further combustion of the intrinsic high-thermal-conductivity / flame-retardant liquid crystal epoxy resin material is stopped or slowed down.

Description

technical field [0001] The invention relates to the technical field of epoxy resin materials, in particular to a flame retardant co-curing agent and a preparation method thereof, an intrinsic type high thermal conductivity / flame retardant liquid crystal epoxy resin material and a preparation method thereof. Background technique [0002] Pure epoxy resin is easy to burn, and it will produce more dense smoke and higher heat release during combustion, which limits its application. The excellent flame retardant effect of epoxy resin can be endowed by introducing flame retardant components. However, the additive flame retardant epoxy resin composite has the problem of poor compatibility between the flame retardant component and the epoxy resin matrix, and the poor dispersion of the flame retardant component in the epoxy resin matrix, which affects the mechanical properties of the epoxy resin composite. ; And after curing, the flame retardant component is easy to escape from the ...

Claims

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Application Information

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IPC IPC(8): C08G77/395C08G77/38C08G59/62C08G59/56
CPCC08G77/045C08G77/395C08G77/38C08G59/621C08G59/56
Inventor 顾军渭钟洨阮坤鹏郭永强
Owner RES & DEV INST OF NORTHWESTERN POLYTECHNICAL UNIV IN SHENZHEN