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Preparation method of phosphorus oxime-containing flame retardant

A flame retardant and solvent technology, applied in the field of organic chemistry and polymer material synthesis, can solve the problems of insufficient improvement of flame retardancy and heat resistance, easy hydrolysis, etc., to achieve safe escape and fire fighting time, flame retardant Performance Hydrolysis resistance, loss reduction effect

Inactive Publication Date: 2018-11-30
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the complex synthetic method of the flame retardant limits the application of the flame retardant
In addition, it was found that the flame retardant did not sufficiently improve the flame retardancy and heat resistance, and was easily hydrolyzed

Method used

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  • Preparation method of phosphorus oxime-containing flame retardant
  • Preparation method of phosphorus oxime-containing flame retardant
  • Preparation method of phosphorus oxime-containing flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 30 parts of 4,4'-dihydroxybenzophenone, 350 parts of xylene, and 12.5 parts of triethylamine into a reaction vessel equipped with a mechanical stirring and temperature control device. Blow nitrogen, stir for 30 minutes, add 82.5 parts of diphenyl chlorophosphate, and stir at 20-30°C for 1 hour after the addition, the system turns from cloudy to clear, add water to quench the reaction, evaporate the solvent under reduced pressure, and extract 3 times with dichloromethane, The organic phase was washed 3 times with deionized water, dichloromethane was evaporated to dryness under reduced pressure to obtain a colorless liquid, and the product was separated and purified by column chromatography (petroleum ether: ethyl acetate=5:1, V / V) to obtain a white solid DHPP .

Embodiment 2

[0035] Add 132 parts of DHPP, 180 parts of ethanol, 20.4 parts of hydroxylamine hydrochloride and 39.6 parts of sodium acetate trihydrate into a reaction vessel equipped with a mechanical stirring and temperature control device. After the addition was complete, stir at 20-30°C for 4 h; evaporate the solvent to dryness under reduced pressure, then extract 3 times with dichloromethane, wash the organic phase 3 times with deionized water, evaporate the dichloromethane to dryness under reduced pressure, and use column chromatography (PE:EA =4:1, V / V) separation and purification to obtain DHPP-NOH.

Embodiment 3

[0037] Add 253.6 parts of DHPP-NOH, 220 parts of toluene, 7.2 parts of triethylamine, and 26.4 parts of p-phenylene diisocyanate into a reaction vessel equipped with a reflux device, a temperature control device, and a mechanical stirring device, and stir at 110°C for 6 hours under reflux; The solvent was dried, the system was extracted 3 times with dichloromethane, and the organic phase was washed 3 times with deionized water. Dichloromethane was evaporated to dryness under reduced pressure. DHPP-NOH-NCO was obtained by separation and purification by column chromatography (petroleum ether: ethyl acetate = 3:1, V / V).

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Abstract

Provided is a preparation method of a phosphorus oxime-containing flame retardant. 4,4'-dihydroxybenzophenone (DHBP) is adopted as a raw material to synthesize a new organic monomer 4,4'-diphenyl diphosphate benzophenone oxime (DHPP-NOH), and the DHPP-NOH has a formula of, in percent by mass, 33.0-41.0% of DHPP, 5.1-6.4% of hydroxylamine hydrochloride, 9.9-12.4% of sodium acetate trihydrate and 45.0-55.0% of a solvent; and then a new organic monomer 1,4-bis[(4,4'-diphenyl diphosphate benzophenone oximido)formyl]aniline (DHPP-NOH-NCO) is further synthesized from the DHPP-NOH. The preparation method has a simple process, and the prepared phosphorus oxime-containing flame retardant has good flame retardancy and hydrolysis resistance.

Description

technical field [0001] The invention relates to a preparation method and technology of a phosphorus-containing oxime flame retardant, and belongs to the technical field of organic chemistry and polymer material synthesis. Background technique [0002] Polymers as material class are generally flammable. Due to its flammability, flame retardants need to be added in many applications. In general, halogenated compounds have been widely used in the field of polymer flame retardancy. It is generally believed that when these products are ignited, halogenated compound products can continue to flame Free radical gas phase reactions occur in , which makes halogenated flame retardants very useful additives in different types of polymers. However, in the past decade or so, due to human concerns about the ecological environment, halogenated flame retardants have received widespread attention. At this time, the flame retardant industry is facing pressure to switch to flame retardants th...

Claims

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Application Information

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IPC IPC(8): C07F9/12C08K5/523
CPCC07F9/12C08K5/523
Inventor 田力李响杨保平崔锦峰郭军红包雪梅张秀君慕波郭永亮刘国天张亚斌王露蓉
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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