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Continuous production method for triethyl phosphite

A triethyl phosphite, continuous process technology, applied in chemical instruments and methods, compounds of elements in Group 5/15 of the periodic table, organic chemistry, etc., can solve the trouble of salt treatment, secondary pollution, and high production energy consumption problem, to achieve no toxic and harmful solvent residues, reduce labor intensity, and reduce production costs.

Inactive Publication Date: 2016-04-20
JIANGSU SUYUANHUIPU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1724546A uses benzene as a solvent, and in the presence of triethylamine, phosphorus trichloride and absolute ethanol are used as raw materials to synthesize and separate triethyl phosphite, which solves the problem of low production yield and low product purity. problem, but it needs to go through processes such as alkaline washing, salt drying, etc., the operation is cumbersome and the production efficiency is low
[0003] Chinese patent CN101624400A introduces a production method of triethyl phosphite, using pure benzene as a solvent and using triethylamine for continuous production, which has the advantages of large production capacity and stable product quality, but due to the use of highly toxic benzene as a solvent, and Both benzene and triethylamine need to be distilled out, which is potentially harmful to the environment and the health of on-site operators, and the production energy consumption is high. At the same time, a salt drying tower is required for drying. The treatment of the salt after absorbing water is cumbersome, resulting in Secondary pollution, not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. a method for continuous production of triethyl phosphite, is characterized in that: comprise the following steps:

[0022] (1) dimethylaniline and o-dichlorobenzene are transported to the continuous reactor with a pump, and ethanol, phosphorus trichloride, and ammonia are passed into simultaneously, the reaction temperature is 30° C., and the pH value is 5 to 7. After the reaction is completed, the The reaction product is directly sent to the continuous distillation tower for vacuum distillation, and the vacuum degree is controlled to -0.085~-0.095Mpa to obtain the crude product of triethyl phosphite;

[0023] (2) The remaining material from the distillation in step (1) is pumped to the continuous water washing tower. After washing with hot water at 95°C, the water layer flows out from the top to the crystallization kettle, and the organic layer is sent to the distillation dehydration tower for distillation and dehydration; the crystallization kettle After cooling to...

Embodiment 2

[0029] 1. a method for continuous production of triethyl phosphite, is characterized in that: comprise the following steps:

[0030] (1) dimethylaniline and o-dichlorobenzene are transported to the continuous reactor with a pump, and ethanol, phosphorus trichloride, and ammonia are passed into simultaneously, the reaction temperature is 20° C., and the pH value is 5 to 8. After the reaction is completed, the The reaction product is directly sent to the continuous distillation tower for vacuum distillation, and the vacuum degree is controlled to -0.085~-0.095Mpa to obtain the crude product of triethyl phosphite;

[0031] (2) The remaining material from the distillation in step (1) is transported to the continuous water washing tower through a pump. After washing with hot water at 60°C, the water layer flows out from the top to the crystallization tank, and the organic layer is transported to the distillation dehydration tower for distillation and dehydration; After cooling to 2...

Embodiment 3

[0037] 1. a method for continuous production of triethyl phosphite, is characterized in that: comprise the following steps:

[0038] (1) dimethylaniline and o-dichlorobenzene are transported to the continuous reactor with a pump, and ethanol, phosphorus trichloride, and ammonia gas are passed into the continuous reactor at the same time. The reaction temperature is 10 ° C, and the pH value is 6 to 9. After the reaction is completed, the The reaction product is directly sent to the continuous distillation tower for vacuum distillation, and the vacuum degree is controlled to -0.085~-0.095Mpa to obtain the crude product of triethyl phosphite;

[0039] (2) The remaining material from the distillation in step (1) is pumped to the continuous water washing tower. After washing with hot water at 40°C, the water layer flows out from the top to the crystallization kettle, and the organic layer is sent to the distillation dehydration tower for distillation and dehydration; the crystalliza...

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PUM

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Abstract

The invention discloses a continuous production method for triethyl phosphite. The method comprises the steps that absolute ethyl alcohol and phosphorus trichloride are taken as reaction raw materials, dimethylaniline and o-dichlorobenzene are taken as reaction solvent, ammonia is introduced while reacting is performed, and after reacting is finished, a product is directly delivered into a continuous distillation column to be processed through reduced pressure distillation to obtain crude triethyl phosphite; the rest materials are delivered into a washing column to be washed by adding hot water and then layered, an organic layer is delivered into a distillation column to be processed through distillation dewatering to be recycled by serving as solvent, a water layer is delivered into a cooling kettle to be cooled, ammonium chloride solids are crystallized out, and mother liquor is continuously used for washing the rest materials of distillation. After the obtained triethyl phosphite is rectified through a rectifying column, the purity is 99.5%-99.9%, and the obtained ammonium chloride can serve as an ammonium fertilizer raw material. The continuous production method has the advantages that a decomposition reaction can be prevented from occurring in the process that the triethyl phosphite participates washing, dewatering can be achieved only by simply distilling the mother liquor, a salt column does not need to be introduced for dewatering, generation of secondary solid waste can be avoided, pollution to the environment is greatly reduced, the labor intensity is low, and the production cost is low.

Description

technical field [0001] The invention relates to a method for preparing chemical substances, in particular to a method for producing triethyl phosphite with the advantages of high yield, stable quality, low energy consumption and low pollution. technical background [0002] Triethyl phosphite, also known as triethyl phosphite; triethyl phosphite (triethoxyphosphine), is mainly used as pesticide and pharmaceutical intermediates, used to prepare OB series fluorescent whitening agents, AE active esters, Glufosinate intermediates, various flame retardants, etc. Chinese patent CN1724546A uses benzene as a solvent, and in the presence of triethylamine, phosphorus trichloride and absolute ethanol are used as raw materials to synthesize and separate triethyl phosphite, which solves the problem of low production yield and low product purity. problem, but it needs to go through processes such as alkaline water washing and salt drying, the operation is cumbersome and the production eff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 潘银祥余根青
Owner JIANGSU SUYUANHUIPU CHEM
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