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P, N and Si ternary hybrid flame retardant and preparation method thereof

A flame retardant, ternary hybrid technology, applied in the field of P, N, Si ternary hybrid flame retardant and preparation, can solve the problems of cumbersome and harsh preparation process

Pending Publication Date: 2019-11-22
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of the flame retardant requires preparation conditions such as high temperature and vacuum drying, and the preparation process is cumbersome and harsh.

Method used

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  • P, N and Si ternary hybrid flame retardant and preparation method thereof
  • P, N and Si ternary hybrid flame retardant and preparation method thereof
  • P, N and Si ternary hybrid flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 1.0mol 4,4'-dihydroxybenzophenone (DHBP), dichloromethane, and 3.0mol triethylamine into a reaction vessel equipped with stirring, heating, and temperature control devices; stir for 30 minutes under nitrogen protection Add 2.0mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 2.0mol carbon tetrachloride (CCl 4 ), stirring and reacting at 25°C for 1h after the addition was completed, adding water to quench the reaction, extracting 3 times with dichloromethane, washing the organic phase 3 times with deionized water, evaporating the dichloromethane to dryness under reduced pressure to obtain a white solid, which was purified by column chromatography The product was separated and purified to obtain 4,4'-bis(diphenoxyphosphor-6-oxyl)benzophenone (DODH). Then add 1.0mol DODH, tetrahydrofuran, 1.0mol NaBH into the reaction vessel equipped with stirring, heating and temperature control devices 4 ; Stir at 25°C for 4h after the addition, evaporate the solvent...

Embodiment 2

[0035]Add 1.0mol 4,4'-dihydroxybenzophenone (DHBP), dichloromethane, and 4.6mol triethylamine into a reaction vessel equipped with stirring, heating, and temperature control devices; stir for 30 minutes under nitrogen protection Add 2.3mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 3.0mol carbon tetrachloride (CCl 4 ), stirring and reacting at 25°C for 1h after the addition was completed, adding water to quench the reaction, extracting 3 times with dichloromethane, washing the organic phase 3 times with deionized water, evaporating the dichloromethane to dryness under reduced pressure to obtain a white solid, which was purified by column chromatography The product was separated and purified to obtain 4,4'-bis(diphenoxyphosphor-6-oxyl)benzophenone (DODH). Then add 1.0mol DODH, tetrahydrofuran, 1.3mol NaBH into the reaction vessel equipped with stirring, heating and temperature control devices 4 ; Stir at 25°C for 4h after the addition, evaporate the solvent ...

Embodiment 3

[0037] Add 1.0mol 4,4'-dihydroxybenzophenone (DHBP), dichloromethane, and 3.76mol triethylamine into a reaction vessel equipped with stirring, heating, and temperature control devices; stir for 30 minutes under nitrogen protection Add 2.15mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 2.47mol carbon tetrachloride (CCl 4 ), stirring and reacting at 25°C for 1h after the addition was completed, adding water to quench the reaction, extracting 3 times with dichloromethane, washing the organic phase 3 times with deionized water, evaporating the dichloromethane to dryness under reduced pressure to obtain a white solid, which was purified by column chromatography The product was separated and purified to obtain 4,4'-bis(diphenoxyphosphor-6-oxyl)benzophenone (DODH). Then add 1.0mol DODH, tetrahydrofuran, 1.3mol NaBH into the reaction vessel equipped with stirring, heating and temperature control devices 4 ; Stir at 25°C for 4h after the addition, evaporate the solv...

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Abstract

The invention discloses a P, N and Si ternary hybrid flame retardant and a preparation method thereof, and mainly relates to the field of reactive flame retardants. The structural formula is shown inthe specification has the beneficial effects that 4, 4 '-dihydroxy benzophenone and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide are subjected to a reaction through molecular design so as to obtain 4, 4'-di (diphenoxyphosphate-6-oxy) benzophenone (DODH) to be used as raw materials; 4, 4 '-bis (diphenoxyphosphate-6-oxy) benzhydrol (DODOH) is obtained by using said raw material and using a reducing agent for reduction, and then the phosphorus-containing flame retardant and a silane coupling agent isocyanatopropyltriethoxysilane (IPTS) are mixed. Elements of phosphorus, nitrogen and silicon with flame retardant properties can be introduced into the material by adding the flame retardant into an organic polymer material, so that the material has an efficient synergistic flame retardanteffect.

Description

technical field [0001] The invention relates to the technical field of reactive flame retardants, in particular to a P, N, Si ternary hybrid flame retardant and a preparation method thereof. Background technique [0002] In the synthesis of most organic flame retardants, there will be three elements of P, N and Si. Organophosphorus compounds can improve the flame retardant level of organic polymer materials through various methods such as condensed phase reaction, gas phase reaction, and promotion of carbonization and coke formation. Silicone can generate silicon-containing compounds (such as silicon dioxide) when polymers are burned, and exerts a flame-retardant effect due to its high thermal stability and physical coverage. Organic nitrogen compounds can produce nitrogen, nitrogen oxides and other flammable and non-combustible gases when polymer materials are burned, and reduce the concentration of combustion oxygen to achieve a flame-retardant effect. [0003] Huijuan W...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5455C08L63/00
CPCC07F9/657181C08K5/5455C08L2201/02C08L63/00
Inventor 郭军红张亚斌杨保平崔锦峰田力包雪梅张秀君慕波周应萍郭永亮王露蓉王念念何婷香
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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