Hybridization structured polysiloxane flame retardant and preparation method thereof

A technology of polysiloxane and hybrid structure, which is applied in the field of polysiloxane flame retardants and their preparation, can solve the problems of limited flame retardant effect and limited flame retardant elements of flame retardants, and achieve improved compatibility, Good flame retardant effect, good thermal stability effect

Active Publication Date: 2017-05-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the production method of the invention is simple and efficient, and the reaction by-products can be recovered, the flame retardant elements in the flame retardant are limited, and there are only three flame retardant elements, N, P, and C, and the flame retardant effect is limited.

Method used

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  • Hybridization structured polysiloxane flame retardant and preparation method thereof
  • Hybridization structured polysiloxane flame retardant and preparation method thereof
  • Hybridization structured polysiloxane flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 6 parts of poly(methylhydrogensiloxane-dimethylsiloxane copolymer), 6*10 -5 Parts of Karstdet catalyst and 70 parts of isopropanol were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere, and the temperature was raised to 60°C and then stirred at a constant temperature for 30 minutes; after the temperature was raised to 100°C, the 10 parts CH in a press funnel 2 =CH-NH-Si-(OCH 2 CH 3 ) 3 , 30 parts of allyl glycidyl ether and 30 parts of isopropanol were added dropwise in a four-necked flask, and the constant temperature was reacted for 24 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain a flame retardant intermediate I; The flame retardant intermediate I obtained in the step, 50 parts of phosphorus-containing active substance diphenylphosphine oxide, 0.18 parts of triethanolamine and 100 parts of isopropanol are added to a four-necked flask,...

Embodiment 2

[0061] Mix 5 parts of poly(methylhydrogensiloxane-dimethylsiloxane copolymer), 8*10 -5 Speier catalyst and 50 parts of benzene were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere. After the temperature was raised to 80°C, it was stirred at a constant temperature for 10 minutes; after the temperature was raised to 95°C, the 10 copies of CH 2 =CH-COO(CH 2 ) 3 -(H 3 C)Si-(OCH 3 ) 3, 50 parts of allyl glycidyl ether, and 50 parts of benzene solution were added dropwise in a four-necked flask, and reacted at a constant temperature for 18 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain a flame retardant intermediate I; the previous step Obtained flame retardant intermediate I, 20 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and phosphorous acid (the molar ratio of the two is 1:1), 0.2 parts Triphenylphosphine and 100 parts of benzen...

Embodiment 3

[0063] 9 parts of 1,3,5,7-tetramethylcyclotetrasiloxane, 5*10 -5 Add the Karstdet catalyst and 50 parts of toluene solvent into a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere. After heating up to 70°C, stir at a constant temperature for 25 minutes; 15 copies of CH 2 =CH-Si-(OCH 3 ) 3 , 40 parts of allyl glycidyl ether, and 40 parts of toluene solution were added dropwise in a four-necked flask, and the constant temperature was reacted for 10 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain the flame retardant intermediate I; the previous step The obtained flame retardant intermediate I, 50 parts of diphenylphosphine oxide, 0.125 parts of triphenylphosphine and 80 parts of toluene were added to a four-necked flask, equipped with a reflux condenser, a thermometer and a magnetic stirrer, and nitrogen gas was introduced, and the temperature was raised to 100 ...

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Abstract

The invention discloses a hybridization structured polysiloxane flame retardant and a preparation method thereof. The hybridization structured polysiloxane flame retardant is prepared by enabling hydrogen-containing silicone oil, allyl glycidyl ether, vinyl silane substances, phosphorus-containing active substances and a silane coupling agent to react with one another under the action of a catalyst. The flame retardant comprises a great amount of organic groups such as benzene rings, a relatively long -Si-O-Si-main chain and a hybridization structure, has hydrophobicity, is relatively high in thermal stability, comprises a great number of elements such as carbon, nitrogen, phosphorus and silicon, can be used as a carbon source and a gas source in an intumescent system, meanwhile has a synergistic flame retardant effect of multiple flame-retardant elements, is good in carbonization property and high in flame-retardant efficiency, the contact angle of the composition is up to 95 DEG C, the compatibility of the composition and a high polymer can be improved, and processing requirements of the high polymer can be met.

Description

technical field [0001] The invention relates to a polysiloxane flame retardant containing a hybrid structure and a preparation method thereof, belonging to the technical field of flame retardant preparation. Background technique [0002] In contemporary life, the polymer material industry is developing rapidly, and polymer materials are more and more widely used in various industries, which makes people not only require them to have excellent performance, but also require them to be safe and environmentally friendly. Most polymer materials are extremely flammable, and will release flammable gases and toxic fumes when burned, which can easily cause fires and cause harm to people and the environment. Therefore, in order to reduce fire hazards and damage caused by fire, flame retardancy has become one of the important performance requirements of material properties, and people's demand for halogen-free and environmentally friendly flame retardants is increasing. [0003] In re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/395C08G77/12C08L83/05
CPCC08G77/12C08G77/38C08G77/395C08L83/04C08L2201/02
Inventor 晏泓赵智垒郭丽娜宋秀安卜颖宏张乃恩
Owner TAIYUAN UNIV OF TECH
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