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Hydroxyl-containing liquid phosphor-nitrogen fire retardant and preparation method thereof

A flame retardant, diethyl phosphate methylolphenoxy technology, applied in the field of flame retardant, can solve problems such as limited application, and achieve the effects of strong practicability, high content of phosphorus elements, and simple and easy-to-operate preparation process

Inactive Publication Date: 2015-09-02
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above patents, the obtained products are all solid products, and some of them have no reactive functional groups, so they can only be used as additive flame retardants, which limits their wide application

Method used

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  • Hydroxyl-containing liquid phosphor-nitrogen fire retardant and preparation method thereof
  • Hydroxyl-containing liquid phosphor-nitrogen fire retardant and preparation method thereof
  • Hydroxyl-containing liquid phosphor-nitrogen fire retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] In a 500mL dry four-necked flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel, and a condensing reflux device, add 30g of potassium carbonate, 17.6g of p-hydroxybenzaldehyde and 200mL of refined tetrahydrofuran in sequence, and under nitrogen protection, Stir for 1 h to dissolve it; then weigh 8.35 g of hexachlorocyclotriphosphazene (the molar ratio of hexachlorocyclotriphosphazene to p-hydroxybenzaldehyde is 1:6) and dissolve it in 100 mL of refined tetrahydrofuran, and slowly add it dropwise to In the above reaction system, the dropwise addition time is 1 h; after 0.5 h, the temperature is raised to 65° C., refluxed and stirred for 48 h, and the reaction ends. Filtrate, concentrate the filtrate, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; filter again, wash the product repeatedly with deionized water for 3 times; finally recrystallize twice with ethyl acetate, and vacuum dry ...

Embodiment 2

[0029] In a 500mL dry four-necked flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel, and a condensing reflux device, add 30g of potassium carbonate, 17.6g of p-hydroxybenzaldehyde, and 250mL of refined tetrahydrofuran in sequence. Stir for 1 h to dissolve it; then weigh 6.3 hexachlorocyclotriphosphazene (the molar ratio of hexachlorocyclotriphosphazene to p-hydroxybenzaldehyde is 1:8) and dissolve it in 100 mL of refined tetrahydrofuran, and slowly add it dropwise to In the above reaction system, the dropwise addition time is 1h; after 0.5h, the temperature is raised to 65°C, refluxed and stirred for 36h, and the reaction ends. Filtrate, concentrate the filtrate, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; filter again, wash the product repeatedly with deionized water for 3 times; finally recrystallize twice with ethyl acetate, and vacuum dry at 50°C for 12 hours to obtain white Pow...

Embodiment 3

[0032] The first step: in the 500mL dry four-necked flask that mechanical stirrer, thermometer, constant pressure dropping funnel and condensation reflux device are housed, add potassium carbonate 25g, 17.6g p-Hydroxybenzaldehyde and 250mL refining ethyl acetate successively, Stir at room temperature under argon protection for 1 h to dissolve; then weigh 8.35 hexachlorocyclotriphosphazene (the molar ratio of hexachlorocyclotriphosphazene to p-hydroxybenzaldehyde is 1:6) and dissolve it in 100 mL of refined ethyl acetate In the ester, it was slowly added dropwise to the above reaction system, and the dropwise addition time was 1h; after 0.5h, the temperature was raised to 80°C, refluxed and stirred for 24h, and the reaction was completed. Filtrate, concentrate the filtrate, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; filter again, wash the product repeatedly with deionized water for 3 times; finally recrystallize twice with et...

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Abstract

The invention relates to a hydroxyl-containing liquid phosphor-nitrogen fire retardant and a preparation method thereof, and belongs to the technical field of flame retardation. The preparation method comprises that hexachlorocyclotriphosphazene, p-hydroxybenzaldehyde and an acid binding agent are added into an organic solvent and undergo a heating reflux reaction, the reaction product is subjected to aftertreatment to form white solid powder hexa(4-formylphenoxy)cyclotriphosphazene, the hexa(4-formylphenoxy)cyclotriphosphazene, diethyl phosphite and triethylamine undergo a heating reflux reaction in an organic solvent, and the reaction product is subjected to reduced pressure distillation so that the organic solvent, diethyl phosphite and the catalyst are removed and a hexa(4-diethyl phosphate hydroxymethylphenoxy)cyclotriphosphazene fire retardant is obtained.

Description

technical field [0001] The invention relates to a synthetic method of a novel hydroxyl-containing liquid phosphorus nitrogen flame retardant hexa(4-diethyl phosphate hydroxymethylphenoxy)cyclotriphosphazene, in particular to a reactive flame retardant containing nitrogen and phosphorus The invention relates to a preparation method of a synergistic flame retardant element compound, which belongs to the field of flame retardant technology. Background technique [0002] Cyclotriphosphazene derivative flame retardants have developed rapidly in recent years as environmentally friendly and highly efficient phosphorus-nitrogen flame retardant products. Hexachlorocyclotriphosphazene is a cyclic phosphazene compound, which also contains phosphorus and nitrogen elements. It has high thermal stability and flame retardancy. It and its derivatives have been widely used in polymer materials. application. Patent 201010501935.X discloses the preparation method of hexaphenoxycyclotriphosph...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C07F9/6593C08G18/66C08G18/32C08G101/00
Inventor 李锦春胡文田张鑫
Owner CHANGZHOU UNIV
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