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Phosphorus-nitrogen intumescent flame retardant and preparation method thereof

A technology of intumescent flame retardants and flame retardants, applied in the field of phosphorus-nitrogen-containing flame retardants and their synthesis

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention is aimed at the existing phosphorus-nitrogen flame retardants with low thermal stability, which have a great influence on the mechanical properties of materials after addition, and cannot be applied in engineering plastics Shortcomings, proposed a phosphorus nitrogen intumescent flame retardant and its synthesis method

Method used

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  • Phosphorus-nitrogen intumescent flame retardant and preparation method thereof
  • Phosphorus-nitrogen intumescent flame retardant and preparation method thereof

Examples

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Effect test

Embodiment 1

[0030] Add 83.2g of neopentyl glycol and 500mL of chloroform in a 2000mL four-necked bottle equipped with a reflux condenser, a thermometer, an agitator, and a constant pressure dropping funnel, then add 8g of anhydrous aluminum trichloride, stir fully to dissolve the raw materials, and then Put the four-necked flask into an ice-water bath, and slowly add 128.8 g of phosphorus oxychloride into the four-necked flask through a constant pressure dropping funnel under the condition of stirring at 5°C. The reaction temperature is controlled at 0-10°C. The time was 2 hours. After the phosphorus oxychloride was added dropwise, the temperature was raised to 50° C., and the reaction was carried out at this temperature for 6 hours. After the reaction was over, the solvent was recovered by distillation under reduced pressure, the residual solid was washed twice with deionized water, and dried in vacuum at 60° C. for 10 hours to obtain 137.9 g of cyclic phosphorus oxychloride, 2-chloro-2-o...

Embodiment 2

[0035]Add 83.2g of neopentyl glycol and 500mL of chloroform into a 2000mL four-necked bottle equipped with a reflux condenser, a thermometer, an agitator, and a constant pressure dropping funnel, then add 8g of anhydrous magnesium chloride, stir fully to dissolve the raw materials, and then put the four-necked Put the bottle in an ice-water bath, and slowly add 128.8g of phosphorus oxychloride into the four-necked flask through a constant pressure dropping funnel under the condition of stirring at 5°C. The reaction temperature is controlled at 0-10°C, and the dropping time is 2h. , After the phosphorus oxychloride was added dropwise, the temperature was raised to 50°C, and the reaction was carried out at this temperature for 6h. After the reaction was over, the solvent was recovered by distillation under reduced pressure, the residual solid was washed twice with deionized water, and dried in vacuum at 60° C. for 10 hours to obtain 136.9 g of cyclic phosphorus oxychloride, 2-chl...

Embodiment 3

[0040] Add 83.2g of neopentyl glycol and 500mL of chloroform into a 2000mL four-necked bottle equipped with a reflux condenser, a thermometer, a stirrer, and a constant pressure dropping funnel, then add 8g of triethylamine, stir well to dissolve the raw materials, and then put the four-necked Put the bottle into an ice-water bath, and slowly add 128.8 g of phosphorus oxychloride into the four-necked flask through a constant pressure dropping funnel under stirring at 5°C, and the reaction temperature is controlled at 0 to 10 o C, the dropping time is 2h. After the phosphorus oxychloride was added dropwise, the temperature was raised to 50°C, and the reaction was carried out at this temperature for 6h. After the reaction was over, the solvent was recovered by distillation under reduced pressure, the residual solid was washed twice with deionized water, and dried in vacuum at 60° C. for 10 hours to obtain 132.9 g of cyclic phosphorus oxychloride, 2-chloro-2-oxo-5, 5-Dimethyl-1,...

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Abstract

The invention relates to a phosphorus-nitrogen intumescent flame retardant and a preparation method thereof. The preparation method comprises the steps: mixing neopentyl glycol and a solvent, adding a catalyst, dissolving the catalyst, then, adding phosphorus oxychloride into a reaction solution under the condition of stirring at the temperature of 0-10 DEG C, reacting for 4-8 hours at the temperature of 20-50 DEG C after phosphorus oxychloride is added completely, removing the solvent through distilling after reacting ends, and washing and drying residues, so as to obtain cyclic phosphoryl chloride; adding the obtained cyclic phosphoryl chloride and an acid binding agent into a solvent, stirring to dissolve, adding diamine into a reaction solution under the condition of stirring at the temperature of 15-30 DEG C, then, reacting for 8-12 hours at the temperature of 50-110 DEG C, removing the solvent through distilling after reacting ends, and washing and drying residues, thereby obtaining the phosphorus-nitrogen intumescent flame retardant. The phosphorus-nitrogen intumescent flame retardant and the preparation method thereof have the advantages that the synthesis process is simple, the reaction time is short, the product has a melting point, the transparency is good when the flame retardant is added into materials, the flame-retardant effect is good, the influence on mechanical properties is low, and the like; and meanwhile, the disadvantage that intumescent flame retardants cannot be applied to the flame retardance of engineering plastics due to poor thermal stability is overcome.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a phosphorus-nitrogen-containing flame retardant and a synthesis method thereof. Background technique [0002] Since the 1980s, flame retardants have become one of the most important additives for polymer materials, and their usage is increasing day by day. Among many flame retardants, organophosphorus flame retardants are recognized as important varieties that can replace halogenated flame retardants because of their environmental friendliness and high efficiency. While endowing materials with good flame retardancy, compared with halogen flame retardants, it has the characteristics of less smoke generation and less formation of toxic and corrosive gases. In recent years, research on organophosphorus flame retardants has become a hot topic in the field of flame retardants. [0003] Phosphorus-containing intumescent flame retardant is a halogen-free flame retardant w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571C08K5/5399
Inventor 赵巍王晓霖李明刘名瑞薛倩
Owner CHINA PETROLEUM & CHEM CORP
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