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Preparation method of low-triphenyl phosphate engineering plastic halogen-free flame retardant

A technology of low triphenyl phosphate and engineering plastics, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of high toxicity of triphenyl phosphate and easy darkening of product color and other problems, to achieve the effect of meeting industrial scale production, easy operation and high purity

Active Publication Date: 2018-01-26
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The patent CN200810063129 invented by our company traditionally uses phosphorus oxychloride to react with p-diphenol first, and then undergoes condensation reaction with phenol to obtain an oligomer. The high-temperature condensation reaction can be complete, and the high-temperature process is prone to disproportionation reaction. During the reaction preparation process Produces highly toxic triphenyl phosphate, and the process of high temperature, the color of the product tends to darken

Method used

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  • Preparation method of low-triphenyl phosphate engineering plastic halogen-free flame retardant
  • Preparation method of low-triphenyl phosphate engineering plastic halogen-free flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 78g (0.5mol) of phosphorus oxychloride and 0.1g of magnesium chloride to a four-necked flask and raise the temperature to 70-80°C, then slowly add 50g (0.55mol) of phenol dropwise for 2.5 hours. Afterwards, keep the reaction at 80-90°C for 5 hours until no hydrogen chloride is released, and the reaction is completed. After the reaction, distill phosphorus oxychloride under reduced pressure with a vacuum degree of 30-100KPa and a distillation temperature of 30-100°C. After reduced pressure distillation, the mixture is obtained Intermediate, i.e. a monosubstituted and disubstituted mixture of phosphorus oxychloride, the ratio of monosubstituted and disubstituted mixture is 4:6, the yield of the mixture intermediate is 95%, and the recovery rate of phosphorus oxychloride is 95% ( Calculated as phosphorus oxychloride);

[0025] Put the mixture intermediate into a four-necked flask, add 0.1g of magnesium chloride, first add 60g of hydroquinone, slowly raise the temperatu...

Embodiment 2

[0030]Add 160g (1mol) of phosphorus oxychloride and 1g of titanium tetrachloride into a four-necked flask for reaction, raise the temperature to 70-80°C, and slowly add 94g (1mol) of phenol dropwise. The time for adding phenol is about 2- 3 hours, after the dropwise addition, keep warm at 80-90°C for 3-5 hours, until no hydrogen chloride is released, the reaction is complete, after the reaction, distill phosphorus oxychloride under reduced pressure, the vacuum degree is 30-100KPa, and the distillation temperature is 30- At 100°C, the mixture intermediate was obtained after vacuum distillation, a mixture of monosubstituted and disubstituted phosphorus oxychloride, the ratio of the mixture was 5:5, gas phase analysis, the mixture intermediate was obtained, the yield of the intermediate was 95%, three The recovery rate of phosphorus oxychloride is 95% (calculated as phosphorus oxychloride);

[0031] Put the mixture intermediate into a four-necked flask, add 1g of titanium tetrach...

Embodiment 3

[0036] Add 1600g (1mol) of phosphorus oxychloride and 10g of aluminum trichloride into a four-necked flask for reaction, raise the temperature to 70-80°C, slowly add 1120g (1.1mol) of phenol dropwise, and the time for adding phenol is about 2 -3 hours, after the dropwise addition, keep the temperature at 80-90°C for 3-5 hours, until no hydrogen chloride is released, the reaction is complete, after the reaction, the vacuum degree of the phosphorus oxychloride distillation tower is 30-100KPa, and the distillation temperature is 30 -100°C, the mixture intermediate was obtained after vacuum distillation, a mixture of monosubstituted and disubstituted phosphorus oxychloride, the ratio of the mixture was 4:6, gas phase analysis, the mixture intermediate was obtained, and the yield of the intermediate was 95%, The recovery rate of phosphorus oxychloride is 95% (calculated as phosphorus oxychloride).

[0037] Put the mixture intermediate into a four-necked flask, add 10g of aluminum t...

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Abstract

The invention belongs to the technical field of applied engineering plastics, and in particular, relates to a preparation method of a low-triphenyl phosphate engineering plastic halogen-free flame retardant. The method comprises the steps: under the action of a Lewis catalyst, carrying out a reaction of phenol with phosphorus oxychloride, reducing the pressure and distilling out excess phosphorusoxychloride, to obtain a mixture intermediate; carrying out a condensation reaction of the mixture intermediate and p-dihydroxybenzene, carrying out a reaction of the mixed intermediate with a properamount of p-dihydroxybenzene firstly, after a part of p-dihydroxybenzene is completely reacted, carrying out high vacuum dehydrochlorination, then adding triethylamine and the remaining p-dihydroxybenzene at relatively low temperature, and carrying out a reaction, wherein increase of the content of triphenyl phosphate is greatly reduced, toxicity to human bodies is reduced, and at the same time, the purity and the yield of the product are improved; and the preparation method has the advantages of simple process operation, short production cycle, economy and environmental protection, can satisfy the requirements of industrial scale production, and is suitable for industrialized popularization and application.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, and in particular relates to a preparation method of a halogen-free flame retardant for low triphenyl phosphate engineering plastics. Background technique [0002] Halogen-free aromatic phosphate flame retardants have a large market space due to their high-efficiency and convenient flame retardant properties. With the rapid growth of the market demand for phosphate flame retardants, the production capacity will be increased, and the right to use will be formed. The scale of industrialization, meeting market demand and participating in international competition has become a top priority. [0003] The patent CN200810063129 invented by our company traditionally uses phosphorus oxychloride to react with p-diphenol first, and then undergoes condensation reaction with phenol to obtain an oligomer. The high-temperature condensation reaction can be complete, and the high-temperature proc...

Claims

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Application Information

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IPC IPC(8): C07F9/40C08K5/5333
Inventor 牛丽丹王秋伟金译艇陈建
Owner ZHEJIANG WANSHENG
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