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P-N collaborative type flame-retardant compound and preparation method thereof

A compound, P-N technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of restricting the development of the flame retardant material industry, starting late, etc. The effect of simple control and preparation method

Active Publication Date: 2010-03-10
河南森远科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in terms of the development of organic phosphorus flame retardants, my country started late, and has not yet introduced similar organic flame retardants with outstanding performance, which directly limits the industrial development of related flame retardant materials. The research and development of fuel has urgent practical significance and long-term strategic significance to our country

Method used

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  • P-N collaborative type flame-retardant compound and preparation method thereof
  • P-N collaborative type flame-retardant compound and preparation method thereof
  • P-N collaborative type flame-retardant compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 250ml three-neck flask equipped with a stirrer and a water separator, after nitrogen protection, add 0.1mol carboxyethylphenylphosphinic acid and 0.1mol ethylenediamine, and add 150ml o-dichlorobenzene, stir, slowly Raise the temperature of the reaction system to 135°C, maintain the temperature for 3 hours, continue to raise the temperature to 160°C for 3 hours, remove the reaction water, and then cool the mixed reaction system to solidify, grind and wash the solid with acetone, suction filter, and filter the residue through The target P-N synergistic flame retardant compound is formed by vacuum drying, the yield rate is 95%, the melting temperature of the product is 190±10°C, and the decomposition temperature is 230±5°C. Its process route is:

[0032]

Embodiment 2

[0034] In a 250ml three-neck flask equipped with a stirrer and a water separator, after nitrogen protection, add 0.1mol carboxyethylphenylphosphinic acid and 0.1mol ethylenediamine, and add 150ml high boiling point solvent oil, stir, slowly Raise the temperature of the reaction system to 140°C, maintain the temperature for 4 hours, then continue to raise the temperature to 155°C for 4 hours to remove the reaction water, then cool the mixed reaction system to solidify, grind and wash the solid with ether, filter with suction, and filter the residue through The target P-N synergistic flame retardant compound was formed by vacuum drying, the yield rate was 94%, the melting temperature of the product was 190±10°C, and the decomposition temperature was 230±5°C.

Embodiment 3

[0036] In a 250ml three-necked flask equipped with a stirrer and a water separator, after nitrogen protection, add 0.1mol carboxyethylphenylphosphinic acid and 0.1mol ethylenediamine, add 150ml xylene, stir, and slowly raise the temperature Reflux at 140°C for 8 hours to remove the reaction water, then cool and solidify the mixed reaction system, grind and wash the solid with ethyl acetate, filter with suction, and vacuum-dry the filter cake to form the target P-N synergistic flame retardant compound. The yield is 93%, the melting temperature of the product is 190±10°C, and the decomposition temperature is 230±5°C.

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Abstract

The invention relates to a P-N collaborative type flame-retardant compound and a preparation method thereof. The flame-retardant compound comprises a structural unit as the below formula, wherein, n is not less than 1 and R represents aromatic radical or straight-chain or branched-chain hydrocarbyl containing 1-8 C atoms. The method comprises the following steps: leading carboxyl ethyl(phenyl)phosphinic acid and a compound containing active amine to be directly reacted under the heating condition and the nitrogen protection condition or be reacted in an organic solvent, then cooling a reaction system, carrying out purification treatment, drying and then forming a target product. The compound has the advantages of stable physical and chemical performances, high flame-retardant performance, safety, environmental protection, good compatibility with polymer base materials, diverse technologies, and simple and easy preparation, thereby being applicable to manufactures with various scales for production. The compound can be widely used in polyesters and polyamides, as well as epoxy resin, glass fiber reinforced resin, paints (water-soluble and oil-soluble) and the like.

Description

technical field [0001] The invention relates to a flame retardant compound and a preparation method thereof, in particular to a P-N synergistic flame retardant compound based on carboxyethylphenylphosphinic acid and a preparation method thereof. Background technique [0002] As the world's environmental protection requirements for flame retardants are getting higher and higher, halogenated flame retardants are facing tremendous pressure, and intumescent phosphorus-nitrogen flame retardants that are environmentally friendly and less polluting are favored by people, especially phosphorus-nitrogen synergistic Flame retardant compounds, the reason is that such flame retardant compounds themselves have the three elements of acid source, carbon source, and gas source flame retardant mechanism, and because they contain C-P bonds, they have high chemical stability, water resistance, solvent resistance, and flame retardant Due to its high flammability, low smoke, and low toxicity, it...

Claims

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Application Information

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IPC IPC(8): C07F9/36C08G69/42C09K21/12C09K21/14
Inventor 王彦林王冬军蒋泽军
Owner 河南森远科技有限公司
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