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Cyclophosphaxene compound as flame-proof material and synthetic method thereof

A cyclophosphazene compound technology, applied in the field of cyclophosphazene compounds and their synthesis, can solve the problems of harsh synthesis conditions, less curing methods, unstable performance, etc., achieve short curing time, avoid separation and purification methods, and flame retardant effect obvious effect

Inactive Publication Date: 2007-08-08
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Japanese patent JP70-95426 19701028 once reported a phosphazene compound with an unsaturated bond as an end group. This kind of compound has the characteristics of curable, flame retardant and heat resistant after curing, but there are harsh synthesis conditions, Unstable performance, few curing methods, long curing time and other disadvantages

Method used

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  • Cyclophosphaxene compound as flame-proof material and synthetic method thereof
  • Cyclophosphaxene compound as flame-proof material and synthetic method thereof
  • Cyclophosphaxene compound as flame-proof material and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add THF 350ml, N 3 P 3 Cl 6 10g, HO-C 6 h 4 -p-CHO 25g, dry K 2 CO 3 35g, heated under reflux and stirred for 48h. The solvent was distilled off, the remaining solid was washed 3 times with distilled water, recrystallized from ethyl acetate, and dried to obtain N 3 P3 (OC 6 h 4 -p-CHO) 6 18.50g, yield 75%;

[0030] Add 600ml volume ratio THF:CH to the three-necked flask 3 OH is 1:1 mixed solvent, 10g N 3 P 3 (OC 6 h 4 -p-CHO) 6 , After dissolving, add 4g NaBH 4 , Stir at room temperature for 17h. The solvent was distilled off, recrystallized from ethanol, and dried to obtain N 3 P 3 (OC 6 h 4 -p-CH 2 Oh) 6 7g, yield 70%;

[0031] Add N to the three-neck flask 3 P 3 (OC 6 h 4 -p-CH 2 Oh) 6 -5g, 40% HBr solution 25ml, concentrated H 2 SO 4 5ml, stirred at reflux for 6h, filtered to take the solid, washed the solid with plenty of water, and dried.

[0032] Recrystallize with acetone:petroleum ether mixed solvent with a volume ratio of ...

Embodiment 2

[0035] Add 150ml THF and 7.50g PhOH to the three-necked flask, after dissolving, add 2.00gNaH, stir at room temperature for 4h, then add dropwise 80ml of 5gN 3 P 3 Cl 6 THF solution, continue to stir at room temperature for 24h after the addition is complete, add dropwise 30ml of 2.5g HOC dissolved in the mixture 6 h 4 -p-CHO and 1gNaH THF solution, reflux and stir for 20h. Filtrate, get the filtrate, distill the filtrate under reduced pressure and concentrate, dry to obtain N 3 P 3 (OPh) 5 (OC 6 h 4 CHO) 6.97g, yield 70%;

[0036] Add 60ml THF:CH to a 100ml flask 3 Mixed solvent with OH volume ratio of 9:1, 6g N 3 P 3 (OPh) 5 (OC 6 h 4 CHO), add 0.5g NaBH after dissolving 4 , stirred at room temperature for 24h. Add this mixture dropwise to dilute hydrochloric acid, collect the precipitated white solid, wash with ethanol until neutral, recrystallize from ethanol, and dry to obtain white needle-like crystals N 3 P 3 (OPh) 5 (OC 6 h 4 CH 2 OH) 4.81g, yield...

Embodiment 3

[0039] Add THF 350ml, N 3 P 3 Cl 6 10g, HO-C 6 h 4 -p-CHO 25g, dry K 2 CO 3 35g, heated under reflux and stirred for 48h. The solvent was distilled off, the remaining solid was washed 3 times with distilled water, recrystallized from ethyl acetate, and dried to obtain N 3 P 3 (OC 6 h 4 -p-CHO) 6 18.50g, yield 75%;

[0040] Add 600ml volume ratio THF:CH to the three-necked flask 3 OH is 1:1 mixed solvent, 10g N 3 P 3 (OC 6 h 4 -p-CHO) 6 , After dissolving, add 4g NaBH 4 , Stir at room temperature for 17h. The solvent was distilled off, recrystallized from ethanol, and dried to obtain N 3 P 3 (OC 6 h 4 -p-CH 2 Oh) 6 7g, yield 70%;

[0041] Add N into the three-neck flask 3 P 3 (OC 6 h 4 -p-CH 2 Oh) 6 5g, 25ml of 40% HBr solution, concentrated H 2 SO 4 5ml, stirred under reflux for 6h, filtered to take the solid, washed the solid with a large amount of distilled water, and dried. Recrystallize with acetone:petroleum ether mixed solvent with ...

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PUM

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Abstract

The invention discloses a cyclophosphazene compound and synthesizing method as photographic flame-proof material, which comprises the following parts: cyclophosphazene, p-hydroxybenzoic acid, potassium acrylate, potassium methyl acrylate, acryloyl chloride or methyl acryloyl chloride.

Description

technical field [0001] The invention relates to a cyclophosphazene compound as a flame-retardant material and a synthesis method thereof. technical background [0002] Phosphorus and nitrogen compounds have been extensively researched and applied as flame retardants with environmental protection functions. In the molecule of cyclophosphazene compound, the phosphorus atom contains two substitutable active chlorine atoms, and various derivatives can be obtained through various substitution reactions. Phosphazene derivatives have higher phosphorus and nitrogen content, which determines Whether it is used as a flame-retardant functional material or a flame-retardant additive for various materials, it has good flame retardancy and heat resistance. Developed countries have been researching and developing phosphazene compound flame retardants in recent decades, but at present, such flame retardants are mainly additive, and less reactive. Additive flame retardants need to solve a ...

Claims

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Application Information

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IPC IPC(8): C07F9/6593C09K21/12
Inventor 刘承美洪育林邱进俊包瑞赵晨
Owner HUAZHONG UNIV OF SCI & TECH
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