Industrial preparation method of high-purity tris(2-butoxyethyl)phosphate

A high-purity, phosphate ester technology, applied in chemical instruments and methods, phosphorus organic compounds, compounds of group 5/15 elements of the periodic table, etc., can solve the problems of product purity yield decline, low purity, serious pollution, etc. , to achieve the effect of increased yield, simple method and improved yield

Inactive Publication Date: 2019-10-22
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] At present, about the preparation method: mainly adopt the reaction of phosphorus oxychloride and ethylene glycol monobutyl ether in the presence of Lewis catalyst under vacuum conditions, the molar ratio of phosphorus oxychloride: ethylene glycol monobutyl ether: 1:6, and use a large amount of Ethylene glycol monobutyl ether, decompression recovery ethylene glycol monobutyl ether, such as Chinese patent CN106008592A (application number is 201610331003.3, the title of invention is a kind of industrial synthesis method and device of tri(butoxyethyl) phosphate) , CN104710471A (the application number is 201510113475.6, the invention name is a kind of phosphate triester production method), the boiling point of ethylene glycol monobutyl ether is 178 ° C, it is difficult to handle it at low temperature, only the pressure is reduced to increase the temperature, and it is raised to above 150 ° C Only when the content of ethylene glycol monobutyl ether is less than 0.3% in vacuum distillation, the reaction system is acidic and the product is easy to decompose under the presence of Lewis catalyst at high temperature, and ethylene glycol monobutyl ether is easy to dehydrate and condense to cause the increase of impurities, and the product content Purity yields all drop
The purity of the CN104710471A product is 94-97%, the yield is 87-89%, the yield of the product is low, and the purity is not high
[0005] Foreign patents US3020303 and EP0091426 use traditional alkali metal oxides and alkoxy alkyl alcohols for high-temperature dehydration to obtain alkoxy alkoxides, and the resulting alkoxides react with phosphorus oxychloride to obtain products. This method consumes a lot of energy , serious pollution, basically eliminated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1. Pump 1540kg (13.03 kilomoles) of ethylene glycol monobutyl ether into the reactor, put 1Kg of catalyst magnesium chloride into the reactor, cool down to 20-25°C, turn on the vacuum, and add dropwise at a vacuum degree of 2-4KPa Phosphorus oxychloride 400kg (2.61 kilomoles, the molar ratio of phosphorus oxychloride to ethylene glycol monobutyl ether is 1:5), add dropwise in 3-5 hours, and slowly heat up to 50-80°C after dropping, Insulation reaction for 5 hours;

[0049] 2. After the gas phase detection reaction is complete, switch the vacuum (vacuum degree is 2 ~ 4KPa) to distill ethylene glycol monobutyl ether under reduced pressure. 10%) content is 6.5%, stop distillation;

[0050] Described gas-phase detection (the gas-phase detection method involved in the embodiment of the present invention or comparative example all adopts following method) step is specifically:

[0051] Gas phase analysis method: Injection temperature: 200°C, detector: 220°C Column temperature...

Embodiment 2

[0057] It is basically the same as Example 1, the molar ratio of phosphorus oxychloride: ethylene glycol monobutyl ether: 1:5, and the others remain unchanged. The product yield is 97.5%.

Embodiment 3

[0059] It is basically the same as in Example 1, the catalyst is changed to titanium tetrachloride, and the others remain unchanged. The product yield is 97%.

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Abstract

The invention relates to a preparation method of high-purity tris(2-butoxyethyl)phosphate. The method comprises the following steps: 1) reacting phosphorus oxychloride with ethylene glycol monobutyl ether under a vacuum condition under the action of a Lewis catalyst; 2) carrying out vacuum distillation after the reaction is finished to recover a large amount of ethylene glycol monobutyl ether, andstopping distillation when the content of ethylene glycol monobutyl ether in the reactant 5-10%; 3) performing neutralization by using an alkali to make the pH value be 5-8, carrying out reduced pressure distillation, and stopping distillation until the content of the ethylene glycol monobutyl ether content is less than 0.1% in order to obtain a crude product; and 4) washing the crude product with water to separate, and carrying out reduced pressure distillation on the washed product to remove water in order to obtain the high-purity tris(2-butoxyethyl)phosphate. The method provided by the invention is simple, and greatly improves the purity, the color number and the yield of the product.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to an industrial preparation method of high-purity tris(butoxyethyl)phosphate. Background technique [0002] Phosphate ester flame retardant plasticizers are multifunctional plastic additives. With the improvement of my country's fire protection regulations, the comprehensive strengthening of enforcement and the increasing attention of the people to their own safety, most of them are for the future development of phosphate ester flame retardant plasticizers. The necessary conditions are provided. Because our country has rich phosphate rock resources, it provides raw material advantages for the domestic development of phosphate esters, and there is room for the market. Therefore, vigorously developing phosphate flame retardant plasticizers and increasing their proportion in plasticizers and flame retardants is one of the development directions of the domestic plastic proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
CPCC07F9/091
Inventor 王秋伟金译平牛丽丹
Owner ZHEJIANG WANSHENG
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