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Phosphorus-containing flame retardant and preparation method

A flame retardant and solvent technology, applied in the field of phosphorus-containing flame retardants and preparation, can solve problems such as complicated preparation, and achieve the effect of strengthening the flame retardant effect and enriching the flame retardant methods.

Pending Publication Date: 2019-11-05
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The flame retardant contains a composite structure of multiple DOPO cyclic phosphates, which has the advantage of high phosphorus content, but has the disadvantage of cumbersome preparation

Method used

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  • Phosphorus-containing flame retardant and preparation method
  • Phosphorus-containing flame retardant and preparation method
  • Phosphorus-containing flame retardant and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 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

[0031] 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

[0033] 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, 1.15mol 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 sol...

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Abstract

The invention discloses a phosphorus-containing flame retardant and a preparation method and mainly relates to the field of reactive flame retardants. The structural formula of the flame retardant isshown in the description, and the phosphorus-containing flame retardant has the advantages that 4,4'-dihydroxy benzophenone and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide are firstly adopted for a one-step reaction through molecular design to obtain 4,4'-bis(diphenyl phosphorus oxide-6-oxy)benzophenone, and 4,4'-bis(diphenyl phosphorus oxide-6-oxy)benzhydrol is reduced by using 4,4'-bis(diphenyl phosphorus oxide-6-oxy)benzophenone as a raw material and a reducing agent. Because 4,4'-bis(diphenyl phosphorus oxide-6-oxy)benzhydrol is high in phosphorus content, 4,4'-bis(diphenyl phosphorus oxide-6-oxy)benzhydrol can be directly added into an organic polymer material, element phosphorus with the flame retardance can be induced into the material, and then the material has a high-efficiency flame retardance effect. Prepared 4,4'-bis(diphenoxyphosphorus-6-oxy)benzhydrol can be used as a flame retardant intermediate and is combined with other flame retardant segments through secondarydevelopment, the flame retardance modes of 4,4'-bis(diphenoxyphosphorus-6-oxy)benzhydrol are enriched, and the flame retardance effect of 4,4'-bis(diphenoxyphosphorus-6-oxy)benzhydrol on organic polymer materials is enhanced.

Description

technical field [0001] The invention relates to the technical field of reactive flame retardants, in particular to a phosphorus-containing flame retardant and a preparation method thereof. Background technique [0002] The wide use of organic polymer materials has greatly facilitated people's clothing, food, housing and transportation. However, most polymer materials are flammable, and are extremely flammable during use, seriously endangering people's personal and property safety, and the use of polymer materials is also greatly restricted. In the early stage of flame retardant treatment of organic polymer materials, a large amount of halogen-containing flame retardants were often added. Through the process of using halogen-containing flame retardants in recent years, it has been found that halogen-containing flame retardants adopt a gas-phase flame-retardant mechanism when they play a flame-retardant role. Halogen in the air often exists in the form of toxic gases, which w...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5357C08L63/00
CPCC07F9/657181C08K5/5357C08L63/00C08L2201/02
Inventor 田力张亚斌杨晶雯崔锦峰郭军红包雪梅张秀君慕波周应萍郭永亮何婷香王露蓉王念念
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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