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Method for preparing triethyl phosphite

A technology of triethyl phosphite and absolute ethanol, which is applied in the chemical industry, can solve the problems of long production cycle, high discharge of "three wastes" and difficult wastewater treatment, so as to improve the purity and conversion rate, avoid the problem of wastewater discharge, Conducive to the effect of environmental protection

Active Publication Date: 2016-08-10
LIAONING INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are two main methods to produce triethyl phosphite in China using phosphorus trichloride and absolute ethanol as raw materials. One is to use benzene as solvent and N,N-xylaniline as acid binding agent to synthesize Triethyl phosphate, and then pass through ammonia gas to analyze the acid-binding agent; the reacted mixture is washed, layered, dried and dehydrated, and distilled to obtain pure triethyl phosphite. This method has a small production capacity and a short production cycle. Long, large material consumption, unstable product quality, high cost, high discharge of "three wastes", especially waste water is not easy to treat, which is not conducive to environmental protection
The other is to use pure benzene as a solvent and N,N-xylaniline as an acid-binding agent to synthesize triethyl phosphite, and then add soda ash to resolve the acid-binding agent; the reacted mixture is washed, layered, and dried Dehydration, distillation and other processes are used to obtain pure triethyl phosphite. This method has a large production capacity and stable product quality, but the same by-product discharge is large, the "three wastes" are difficult to treat, the waste water has high salt content, high production costs, and is not conducive to environmental protection

Method used

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  • Method for preparing triethyl phosphite

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Experimental program
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Effect test

Embodiment 1

[0019] A kind of preparation method of triethyl phosphite proposed by the present invention comprises the following steps,

[0020] S1: Add 46g of absolute ethanol, 100ml of toluene, 6.5g of di-n-butylamine to a 500ml reactor equipped with electric stirring, thermometer, constant pressure dropping funnel, acid absorption system, vacuum system and condenser, and start the stirring device , mix the materials evenly, use an ice-water bath to lower the temperature of the system to 20°C, and observe the temperature displayed on the thermometer all the time, and control the reaction temperature between 15-20°C by adding ice cubes to the ice-water bath, and rotate The plunger of the constant pressure dropping funnel adjusts the dropping speed, so that 45g of phosphorus trichloride solution in the constant pressure dropping funnel is slowly added dropwise to the reactor. After 1 hour of dropping, the temperature of the reaction system is raised to 50°C by a heater in 30 minutes. ;

...

Embodiment 2

[0024] A kind of preparation method of triethyl phosphite proposed by the present invention comprises the following steps,

[0025] S1: In a 500ml reactor equipped with electric stirring, thermometer, constant pressure dropping funnel, acid absorption system, vacuum system and condenser, add absolute ethanol 46g, toluene 100ml, triethylamine 5g, open the stirring device, make Mix the materials evenly, use an ice-water bath to lower the temperature of the system to 20°C, and observe the temperature displayed on the thermometer all the time, and control the reaction temperature between 15-20°C by adding ice cubes to the ice-water bath, and rotate at a constant pressure The plunger of the dropping funnel adjusts the dropping speed so that 45g of phosphorus trichloride solution in the constant pressure dropping funnel is slowly added dropwise to the reactor, and the dropping is completed within 1 hour, and the temperature of the reaction system is raised to 50°C within 30 minutes; ...

Embodiment 3

[0029] A kind of preparation method of triethyl phosphite proposed by the present invention comprises the following steps,

[0030] S1: In a 500ml reactor equipped with electric stirring, thermometer, constant pressure dropping funnel, acid absorption system, vacuum system and condenser, add 46g of absolute ethanol, 100ml of toluene, 8g of di-n-butylamine, start the stirring device, Mix the materials evenly, use an ice-water bath to lower the system temperature to 20°C, and observe the temperature displayed on the thermometer all the time, and control the reaction temperature between 15 and 20°C by adding ice cubes to the ice-water bath, and rotate it constantly Press the plunger of the dropping funnel to adjust the dropping speed, so that 45g of phosphorus trichloride solution in the constant pressure dropping funnel is slowly added dropwise to the reactor, after 0.6h the dropping is completed, and the temperature of the reaction system is raised to 50°C within 30min;

[0031...

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PUM

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Abstract

The invention discloses a method for preparing triethyl phosphate .The method comprises the following steps that phosphorus trichloride and absolute ethyl alcohol are adopted as raw materials, methylbenzene is adopted as a solvent, a synthetic reaction is carried out under the action of an acid absorbent, the product is subjected to filtering and vacuum distillation, and refined triethyl phosphate is obtained .Compared with the prior art, 90% or above of a byproduct hydrogen chloride can be removed under the micro-negative pressure condition, the product conversion rate is high, the quality is stable, the quantity of adopted acid absorbent can be reduced, cost can be reduced, recycled hydrogen chloride can be used for other fields, environmental pollution is reduced, and effective resources are reasonably reused; the method for preparing triethyl phosphate is simple, operate is convenient, productivity is high, and the obtained product is high in purity and yield.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of triethyl phosphite. Background technique [0002] Triethyl phosphite is a colorless and transparent liquid chemical substance with the molecular formula C 6 h 15 o 3 P, is a class of organophosphorus reagents widely used in pesticides, plastics, pharmaceuticals and other fields. Because it can interact with the oxygen in the air or the organic hydroperoxide generated by the automatic oxidation of plastics, it can play a role in maintaining the stability of plastics, and can also be used as an auxiliary anti-aging agent. It can be used in conjunction with various main anti-aging agents to produce good The synergistic effect is mainly used in soft products such as agricultural film and artificial leather. At the same time, triethyl phosphite is also an important intermediate for the synthesis of pesticides and medicines. In the dye industry, it is used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 李双奇孙国军孙浩妍
Owner LIAONING INST OF SCI & TECH
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