A kind of preparation method of epoxy resin based on silicon thiazole dopo type flame retardant modification

An epoxy resin and flame retardant technology, which is applied in the field of epoxy resin preparation based on silicon thiazole DOPO type flame retardant modification, can solve the problems of limited application scope, reduced thermal stability and mechanical properties, and decreased Tg value. , to achieve the effect of improving compatibility, good flame retardant effect and good flame retardant performance

Active Publication Date: 2020-07-31
上海道宜半导体材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its Tg value has decreased, and the tensile strength and impact strength have decreased by 1.56% and 1.07% compared with pure EP. The decrease in thermal stability and mechanical properties limits the application range of this type of material.

Method used

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  • A kind of preparation method of epoxy resin based on silicon thiazole dopo type flame retardant modification
  • A kind of preparation method of epoxy resin based on silicon thiazole dopo type flame retardant modification
  • A kind of preparation method of epoxy resin based on silicon thiazole dopo type flame retardant modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Under the protection of high-purity nitrogen, 2-aminobenzothiazole (40mmol) and triethylamine (6ml) were added to a three-necked flask, and dichloromethylvinylsilane (20mmol) and tetrahydrofuran were added dropwise through a constant pressure dropping funnel (40ml) of the mixed solution, the temperature of the whole system is controlled at 30 ° C, after the dropwise addition is completed, the reaction is continued at this temperature for 5 h, after the reaction is completed, it is left to settle, and the hydrochloride of triethylamine is removed by suction filtration, and the filtrate is collected and used Wash with anhydrous ether, remove the solvent by rotary evaporation, and dry in vacuum to obtain vinyldiaminobenzothiazole.

[0038] Under high-purity nitrogen protection, the mixture of DOPO (16.5mmol), vinyl diaminobenzothiazole (15mmol) and toluene (30ml) is added in the 150ml three-necked flask that magnetic stirrer and reflux condenser tube are housed, be warming ...

Embodiment 2

[0043] The silicon-containing thiazole DOPO type flame retardant synthesized in Example 1 (mass fraction is 2.5%) is used as a flame retardant modifier, and 4,4-diaminodiphenylmethane (mass fraction is 17.1%) is used as a curing agent to prepare a modified E44 epoxy resin material.

[0044] Weigh silicon-containing thiazole DOPO flame retardant (3.11g) and slowly add it into E44 epoxy resin (100g), stir at 100°C for 20min to obtain a homogeneous mixture. Then the obtained epoxy resin and 4,4-diaminodiphenylmethane (21.30 g) were stirred at 100° C. for 5 min until the curing agent was completely dissolved. Finally, the epoxy resin mixture was poured into the mold for heating and curing. The curing program was 100°C for 120 minutes and 150°C for 120 minutes to prepare a modified epoxy resin material with a flame retardant content of 2.5%.

Embodiment 3

[0046] The silicon-containing thiazole DOPO type flame retardant synthesized in Example 1 (mass fraction is 5%) is used as a flame retardant modifier, and 4,4-diaminodiphenylmethane (mass fraction is 16.3%) is used as a curing agent to prepare a modified E44 epoxy resin material.

[0047] Weigh silicon-containing thiazole DOPO flame retardant (6.36g) and slowly add to E44 epoxy resin (100g), stir at 100°C for 20min to obtain a homogeneous mixture. Then the obtained epoxy resin and 4,4-diaminodiphenylmethane (20.75 g) were stirred at 100° C. for 10 min until the curing agent was completely dissolved. Finally, the epoxy resin mixture was poured into the mold for heating and curing. The curing program was 100°C for 120 minutes and 150°C for 150 minutes to prepare a modified epoxy resin material with a flame retardant content of 5%.

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Abstract

The invention provides a preparation method of modified epoxy resin based on a silicon thiazole DOPO flame retardant. The method includes the steps: stirring the silicon-containing DOPO fire retardantand bisphenol A-type epoxy resin to homogenized mixing liquid, and mixing and dissolving the homogenized mixing liquid and curing agents; pouring mixed liquid into a mold, and performing heating andcuring in a sectioned manner. According to the silicon-containing DOPO flame retardant, 2-aminobenzothiazole, vinyl dichloride silane and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide serve as araw material, triethylamine serves as an acid-binding agent, azodiisobutyronitrile (AIBN) serves as an initiator, and tetrahydrofuran (THF) and methylbenzene serve as a solvent. The prepared flame-retardant modified epoxy resin has excellent flame resistance, mechanical property and heat stability, reaction conditions are easily controlled, yield is high, and the epoxy resin had wide applicationprospects in the fields of aerospace, home decoration buildings, microelectronic packaging, accessories and the like.

Description

technical field [0001] The invention belongs to the field of flame retardant modified epoxy resin materials, in particular to a method for preparing epoxy resin modified based on silicon thiazole DOPO type flame retardant. [0002] technical background [0003] Epoxy resin has excellent water resistance, solvent resistance and chemical corrosion resistance, and has good mechanical properties and dielectric properties. It can be used as a resin matrix for high-performance composite materials, in aerospace, home improvement construction, and microelectronic packaging materials. , jewelry and other fields have broad application prospects. But the main disadvantage of epoxy resin is flammability, which limits its effective application in many fields. Therefore, research on the flame retardant modification of epoxy resin is an important way to improve its application field. [0004] Organophosphorus flame retardants have the advantages of low smoke, high efficiency, low toxicity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C08K5/5445
CPCC08G59/5033C08K5/5477
Inventor 陈明锋李珊珊李治农苏丽评刘灿培
Owner 上海道宜半导体材料有限公司
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