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Method for preparing organic phosphorous flame retardant with hydroquinone phosphate as framework

A technology of hydroquinone phosphate and quinone phosphate, which is applied in the field of preparation of organophosphorus flame retardants, can solve the problems of synthetic process description, unsuitability for industrial production, high cost, etc., and achieve environmental friendliness and high product quality. High purity, convenient transportation and storage

Inactive Publication Date: 2012-08-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

That is to say, the flame retardant effect of the flame retardant synthesized by using hydroquinone as raw material is better than that of the flame retardant synthesized by using resorcinol as raw material. However, this article is limited to the introduction of the two flame retardants. The research on characterization and flame retardant mechanism does not describe the synthesis process, and the raw material 2,6-dimethylphenol used is expensive and not suitable for industrial production

Method used

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  • Method for preparing organic phosphorous flame retardant with hydroquinone phosphate as framework
  • Method for preparing organic phosphorous flame retardant with hydroquinone phosphate as framework
  • Method for preparing organic phosphorous flame retardant with hydroquinone phosphate as framework

Examples

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Effect test

Embodiment 1

[0036] The first step is the synthesis of hydroquinone phosphate intermediate (1): add 27.5g (0.25mol) hydroquinone into a four-necked flask equipped with stirring, condensing device, temperature probe and protective gas interface, and the temperature is controlled at 80°C , add 116ml (1.25mol) phosphorus oxychloride (POCl 3 ), adding 1.0g (0.0075mol) of aluminum trichloride as a catalyst, reacting at this temperature for 3h, and absorbing the hydrogen chloride gas produced by dilute lye. Distill unreacted POCl under reduced pressure 3 , to obtain 83.9 g (0.245 mol) of hydroquinone phosphate intermediate (1), with a yield of 98%.

[0037]The second step of product synthesis: Take 112g (1.19mol) of phenol and add it to the same type of flask as above, add 1.0g (0.0075mol) of aluminum trichloride as a catalyst, control the reaction temperature at 100°C, and add hydroquinone phosphate in 3 times The intermediate (1) was added into the reaction flask and reacted for 6-8 hours. ...

Embodiment 2

[0041] The first step is the synthesis of hydroquinone phosphate intermediate (1): Add 27.5g (0.25mol) hydroquinone into a four-necked flask with stirring, condensing device, temperature probe and protective gas connection, and control the temperature at 100°C , add 93ml (1.03mol) phosphorus oxychloride (POCl 3 ), adding 1.0g (0.0075mol) of aluminum trichloride as a catalyst, reacting at this temperature for 2h, and absorbing the hydrogen chloride gas produced by dilute lye. Distill unreacted POCl under reduced pressure 3 , to obtain 84.1 g (0.245 mol) of hydroquinone phosphate intermediate (1), with a yield of 98%.

[0042] The second step of product synthesis: Take 42g (0.56mol) of tert-butanol and add it to the above-mentioned four-necked flask of the same type, add 1.0g (0.0038mol) of tin tetrachloride as a catalyst, control the reaction temperature at 80°C, and divide the p-benzene Add the diphenol phosphate intermediate (1) into the reaction flask, and react for 6 hour...

Embodiment 3

[0046] The first step is the synthesis of hydroquinone phosphate intermediate (1): add 27.5g (0.25mol) hydroquinone into a four-necked flask equipped with stirring, condensing device, temperature probe and protective gas interface, and the temperature is controlled at 60°C , add 116ml (1.25mol) phosphorus oxychloride (POCl 3 ), adding 1.5g (0.011mol) of aluminum trichloride as a catalyst, reacting at this temperature for 4h, and absorbing the hydrogen chloride gas produced by dilute lye. Distill unreacted POCl under reduced pressure 3 , to obtain 83.5 g (0.243 mol) of hydroquinone phosphate intermediate (1), with a yield of 97%.

[0047] The second step of product synthesis: Take 60g (0.60mol) of cyclohexanol and add it to the above-mentioned four-necked flask of the same type, add 1.0g (0.0075mol) of aluminum trichloride as a catalyst, control the reaction temperature at 100°C, and add p-benzene Diphenol phosphate intermediate (1) was added to the reaction flask, and reacte...

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Abstract

The invention discloses a method for preparing organic phosphorous flame retardant with hydroquinone phosphate as framework. The method is characterized by adding catalyst with hydroquinone with the molar weight ranging from 0.1% to 5% into phosphorous oxychloride with the excessive molar weight ranging from 1% to 300%, realizing catalytic reaction for 0.5 to 5 hours at the temperature ranging from 10 DEG C to 150 DEG C, decompressing and drying for 0.5 to 5 hours after the reaction is completed, and removing unreacted phosphorous oxychlorid to obtain hydroquinone phosphate intermediate; and adding hydroquinone phosphate intermediate catalyst with the molar weight ranging from 0.1 to 5% into the hydroquinone phosphate intermediate and hydroxyl-containing compound with the excessive molar weight ranging from 0% to 100%, realizing catalytic reaction for 0.1 to 24 hours at the temperature ranging from 30 DEG C to 300 DEG C, washing by the aid of 0.05-5% of oxalate liquor, 0.05-5% of sodium hydroxide liquor and distilled water at the temperature ranging from 25 DEG C to 100 DEG C by three times respectively, then crystallizing by the aid of cold water, decompressing and drying to obtain the organic phosphorous flame retardant with the hydroquinone phosphate.

Description

technical field [0001] The invention relates to a preparation method of an organophosphorus flame retardant with hydroquinone phosphate as a skeleton, and belongs to the field of organophosphorus flame retardants. Background technique [0002] The treatment method to improve the flame retardancy of polymers is to add various flame retardant materials to them. Common flame retardant materials include inorganic metal oxides and organic compounds. [0003] The problem with the application of inorganic flame retardants is that the particle size is mostly at the micron level, which has poor compatibility with polymers, and the addition of a large number of micron-sized flame retardants will have a greater impact on the mechanical properties of the polymer; Combustion agents have high requirements on the synthesis process, and the surface of the nano-powder must be modified in order to be better dispersed in the polymer material, so as to achieve a flame-retardant effect that has...

Claims

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Application Information

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IPC IPC(8): C07F9/12C07F9/58C07F9/6568C07F9/6521C08K5/523C08K5/529C08L55/02C08L67/02C08L23/12C08L23/06C08L69/00C08L75/04
Inventor 杨林付全军王辛龙张志业钟本和
Owner SICHUAN UNIV
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