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A kind of preparation method of silicon-containing thiazole dopo type flame retardant

A flame retardant, silicon thiazole technology, applied in the field of preparation of silicon-containing thiazole DOPO flame retardant, can solve the problems of Tg value decrease, limited application range, thermal stability and mechanical properties decrease, etc., to achieve enhanced compatibility , good flame retardant effect, the effect of overcoming the deterioration of thermal stability

Active Publication Date: 2020-06-09
XIAMEN WAEXIM RUBBER CO LTD
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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 silicon-containing thiazole dopo type flame retardant
  • A kind of preparation method of silicon-containing thiazole dopo type flame retardant
  • A kind of preparation method of silicon-containing thiazole dopo type flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 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.

[0031] 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

[0036] 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.

[0037] 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

[0039] 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.

[0040] 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 silylthiazole-containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) type flame retardant. The silylthiazole-containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) type flame retardant is prepared from 2-aminobenzothiazole, dicholorvinylsilane, and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, with triethylamine serving as an acid binding agent, AIBN (azodiisobutyronitrile) as an initiator and THF (tetrahydrofuran) and toluene as solvents. Modified epoxy resin is prepared with the silylthiazole-containing DOPO type flame retardant and bisphenol A type epoxy resin. The silylthiazole-containing DOPO type flame retardant herein has phosphorus, nitrogen and silicon, can provide phosphorus-nitrogen-silicon synergyto retard flaming, and has good flame retardancy after being applied to the modified epoxy resin. The silylthiazole-containing DOPO type flame retardant contains a plurality of heteroaromatic rings, high-bonding-energy Si-N bonds and -NH that may react with epoxy groups, and the problem that the addition of part of flame retardants brings down the mechanical performance and thermal stability of epoxy resin is solved.

Description

technical field [0001] The invention belongs to the field of flame retardant materials, in particular to a preparation method of silicon-containing 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, and no pollution, and have attracted ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/548C07F9/6574C08L63/00
CPCC07F9/657172C08K5/548C08L2201/02C08L2201/08C08L63/00
Inventor 陈明锋李珊珊李治农苏丽评刘灿培
Owner XIAMEN WAEXIM RUBBER CO LTD
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