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A kind of preparation method of bisphenol condensed polyphosphate with high yield

A technology for bisphenol polycondensation phosphoric acid ester and bisphenol polycondensation phosphorylation, which is applied in the field of chemical synthesis, can solve the problems of deepening the color number of products, and achieve the effect of improving yield

Active Publication Date: 2017-08-01
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of phosphorus pentachloride has problems such as easy to deepen the color number of the product

Method used

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  • A kind of preparation method of bisphenol condensed polyphosphate with high yield
  • A kind of preparation method of bisphenol condensed polyphosphate with high yield
  • A kind of preparation method of bisphenol condensed polyphosphate with high yield

Examples

Experimental program
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Effect test

Embodiment 1

[0044]1) Put 6060 kg (39.48 kilomoles) of phosphorus oxychloride into a 6300L reaction kettle equipped with bisphenol A solid twin-screw feeder, phosphorus oxychloride reflux and vacuum distillation device, and hydrogen chloride gas absorption device, and add catalyst anhydrous 20 kg of magnesium chloride, heated up to 97°C, continuously added 1575 kg (6.91 kilomoles) of bisphenol A with a twin-screw feeder, and finished adding in about 6 hours, then kept at 100-110°C for about 2 hours until the reaction was complete;

[0045] 2) Cool the above reactant to 75°C, add 20 kg of thionyl chloride, and keep it warm for 1.5 hours;

[0046] 3) Transfer the reactant in 2) to a distillation kettle equipped with phosphorus oxychloride, gradually increase the distillation temperature and vacuum degree of the reaction kettle, and remove phosphorus oxychloride. When the temperature is 130-140°C, the vacuum degree is 0.093- 0.097Mpa, complete the phosphorus oxychloride distillation process t...

Embodiment 2-4

[0050] The implementation method is as in Example 1. By adjusting the dosage of thionyl chloride in step 2), crude BDP products with different hydroxyphosphate contents are obtained, and then BDP products are obtained through post-processing.

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Abstract

The present invention relates to a preparing method of a high yield bisphenol polycondensation phosphate, through the bisphenol compounds and phosphorus oxychloride reaction to obtain bisphenol polycondylated phosphorus acetyl chloride, then thionyl chloride can be added as a hydroxyl scavenger, the hydroxyl-containing phosphorus oxychloride presented by water can be re-converted to phosphorus oxychloride, thus sharply reducing the content of hydroxyl phosphate in the crude product of polycondensated phosphate ester reaction, and then through the distillation to remove excess phosphorus oxychloride, reacts with the unit phenolic compounds, the bisphenol polycondensated phosphate ester with low hydroxyl phosphate can be obtained, which will improve the yield of the product, and the product colors of polycondensation of polycondensated phosphate ester will not be affected due to the appliance of thionyl chloride as the hydroxyl group scavenger.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of high-yield bisphenol polycondensed phosphate, and more specifically relates to the preparation of bisphenol polycondensed phosphate in the presence of a hydroxyl scavenger. Background technique [0002] The use of flame-retardant materials such as flame-retardant plastics to improve the fire safety of products is receiving more and more attention and attention in various sectors of the national economy. Various application fields of engineering plastics have put forward more and more stringent requirements on the flame retardancy of materials, especially in the electronic information industry. In recent years, the application industry of flame-retardant engineering plastics is expanding day by day. Among the five major engineering plastics, flame-retardant modification is often required to meet the needs of various users. [0003] B...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/12C08K5/523C08G79/04
CPCC07F9/12C08G79/04C08K5/523
Inventor 金译平牛丽丹沈高波吴宪水
Owner ZHEJIANG WANSHENG