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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  • 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 fun

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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

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Example Embodiment

[0021] Example 1

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

Example Embodiment

[0028] Example 2

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

Example Embodiment

[0031] Example 3

[0032] The first step: 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 25g potassium carbonate, 17.6g p-hydroxybenzaldehyde and 250mL refined ethyl acetate. Under the protection of argon, stir at room temperature 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 100mL refined ethyl acetate In the ester, it was slowly added dropwise to the above reaction system for 1 hour; after 0.5 hours, the temperature was raised to 80°C, refluxed and stirred for 24 hours, and the reaction was completed. Filter, concentrate the filtrate, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; filter again, repeatedly wash the product with deionized water 3 times; finally recrystallize twice with ethyl acetate, an...

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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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