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After-treatment method of crude tris-(2-isopropyl chloride) phosphate

A technology of chloroisopropyl and phosphate esters, applied in the direction of phosphorus organic compounds, etc., can solve the problems of increasing environmental protection pressure, affecting product yield, long reaction time, etc., and achieve the effect of eliminating odor

Active Publication Date: 2012-02-22
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming of this method is: 1) aqueous solution of hydroxylamine hydrochloride is incompatible with three-(2-chloroisopropyl) phosphate, therefore needs longer reaction time, and three-(2-chloroisopropyl) phosphate Will hydrolyze slowly in water, which will eventually affect the yield of the product
The addition of hydroxylamine hydrochloride will eventually enter the wastewater treatment system, thereby increasing the pressure on environmental protection
The addition of hydroxylamine hydrochloride increases production cost simultaneously
2) If you use hydroxylamine hydrochloride solution, although you can shorten the reaction time and reduce the decomposition of the product, it will further increase the pressure on environmental protection and production costs
Therefore, this method is not feasible in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Take 500 g of the crude product of tris-(2-chloroisopropyl) phosphate prepared above, put it into a 1000-liter four-neck bottle with a gas inlet tube at the bottom of the bottle, stir and heat up to 40 ° C, and use 15 minutes to evenly Introduce 20L of ozone-containing air with a concentration of 30mg / L, then add 500ml of 2% dilute hydrochloric acid, control the temperature at 55°C, stir for half an hour, and then let stand for half an hour to separate the layers and separate the acidic water layer. In the same way, wash once with 500 ml of 1% dilute alkali, wash twice with 1000 ml of deionized water, separate the water layer, and vacuum distill and dehydrate the organic layer at 70-120°C and vacuum degree of 500mmHg-1000mmHg to obtain Low-odor tris-(2-chloroisopropyl) phosphate finished product, the content of 2-methylvaleral in the chromatographic analysis product is 4.5ppm.

Embodiment 2

[0021] Example 2 Take 500 g of the crude product of tris-(2-chloroisopropyl) phosphate prepared above, put it into a 1000-liter four-neck bottle with a gas inlet tube at the bottom of the bottle, stir and heat up to 20 ° C, and use 90 minutes to evenly Introduce 50L of ozone-containing air with a concentration of 10mg / L, then add 500ml of 2% dilute hydrochloric acid, control the temperature at 55°C, stir for half an hour, and then let stand for half an hour to separate the layers and separate the acidic water layer. In the same way, wash once with 500 ml of 1% dilute alkali, wash twice with 1000 ml of deionized water, separate the water layer, and vacuum distill and dehydrate to obtain a low-odor tris-(2-chloroisopropyl) phosphate product. Chromatography The content of 2-methylvaleral in the analysis product was 3.8ppm.

Embodiment 3

[0022] Example 3 Take 500 g of the crude product of tris-(2-chloroisopropyl) phosphate prepared above, put it into a 1000-liter four-neck bottle with a gas inlet tube at the bottom of the bottle, stir and raise the temperature to 100 ° C, and use 10 minutes to evenly Introduce 30L of ozone-containing air with a concentration of 50mg / L, then add 500ml of 2% dilute hydrochloric acid, control the temperature at 55°C, stir for half an hour, and then let stand for half an hour to separate the layers and separate the acidic water layer. In the same way, wash once with 500 ml of 1% dilute alkali, wash twice with 1000 ml of deionized water, separate the water layer, and vacuum distill and dehydrate to obtain a low-odor tris-(2-chloroisopropyl) phosphate product. Chromatography The content of 2-methylvaleral in the analysis product was 1.1ppm.

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Abstract

The invention relates to an after-treatment method of crude tris-(2-isopropyl chloride) phosphate, in particular to a treatment method which can effectively remove the stinky 2-methyl-pentanal in the tris-(2-isopropyl chloride) phosphate. The method is characterized by comprising the steps of: introducing a certain amount of ozone in the crude tris-(2-isopropyl chloride) phosphate obtained by reaction; directly oxidizing the insoluble 2-methyl-pentanal generated by reaction into acidic materials such as 2- methyl-valeric acid and the like soluble in an alkaline solution; and conveniently removing the acidic materials in the subsequent washing process to ensure that the obtained tris-(2-isopropyl chloride) phosphate does not contain the 2-methyl-pentanal which stinks. The method of the invention reduces the content of the stinky 2-methyl-pentanal in the tris-(2-isopropyl chloride) phosphate from about 200-300ppm to less than 5ppm; and when the product is applied to the interior materials of automobiles or furniture and the like, the stink is eliminated, and therefore, the product is in the favor of consumers.

Description

technical field [0001] The invention belongs to the technical field of purification of fine chemical products, and in particular relates to a post-treatment method for effectively removing the malodorous substance 2-methylvaleral in the crude product of tris-(2-chloroisopropyl) phosphate. Background technique [0002] At present, the preparation method of tri-(2-chloroisopropyl) phosphate is synthesized by reacting phosphorus oxychloride and propylene oxide under Lewis acid catalysis. After the reaction of phosphorus oxychloride and propylene oxide is completed, the crude product of tris-(2-chloroisopropyl) phosphate is obtained, and the crude product is finished after acid washing, alkali washing, water washing, and distillation to remove water. Yet in the production process of tris-(2-chloroisopropyl) phosphate, the material 2-methylvaleral with foul smell is produced simultaneously, and it has good compatibility with tris-(2-chloroisopropyl) phosphate Soluble, almost ins...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09
Inventor 金译平
Owner ZHEJIANG WANSHENG
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