Recovery method of rectification residual liquid of dimethyl phosphite

A technology of dimethyl phosphite and a recovery method, which is applied in the field of recovery of dimethyl phosphite rectification raffinate, can solve the problems of low production efficiency, large floor area, high investment in production equipment, etc., and achieves improved purity, high temperature and the effect of time reduction

Inactive Publication Date: 2016-07-13
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitation of equipment materials and other factors, most of them adopt batch method, which seriously restricts the enlargement and optimization of production equipment. Facto...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for recovering dimethyl phosphite rectification raffinate, its preparation process is as follows:

[0031] First, methanol and phosphorus trichloride are sprayed slowly into the esterification reaction kettle in the form of mist at the same time. The molar ratio of the injected amount is methanol:phosphorus trichloride=3:1, and the reaction is exothermic. By controlling the injected amount of methanol To control the reaction temperature between 48°C, the solid in the esterification reactor after the reaction is completed is the crude product of dimethyl phosphite;

[0032] Then add an appropriate amount of ammonia to the crude dimethyl phosphite in the neutralization tank for neutralization, the addition of ammonia should be slow, and stop when the pH value of the material in the neutralization tank is 6.5, and the material in the neutralization tank is phosphorous acid A mixture of dimethyl esters and ammonium chloride;

[0033] Then the material in the neutr...

Embodiment 2

[0041] A method for recovering dimethyl phosphite rectification raffinate, its preparation process is as follows:

[0042] First, methanol and phosphorus trichloride are sprayed slowly into the esterification reaction kettle in the form of mist at the same time. The molar ratio of the injected amount is methanol:phosphorus trichloride=3:1, and the reaction is exothermic. By controlling the injected amount of methanol To control the reaction temperature between 49°C, the solid in the esterification reactor after the reaction is completed is the crude product of dimethyl phosphite;

[0043] Add an appropriate amount of ammonia to the crude product of dimethyl phosphite in the neutralization tank for neutralization, the addition of ammonia should be slow, and stop when the pH value of the material in the neutralization tank is 6.8, and the material in the neutralization tank is phosphorous acid A mixture of dimethyl esters and ammonium chloride;

[0044] Then the material in the...

Embodiment 3

[0052] A method for recovering dimethyl phosphite rectification raffinate, its preparation process is as follows:

[0053]First, methanol and phosphorus trichloride are sprayed slowly into the esterification reaction kettle in the form of mist at the same time. The molar ratio of the injected amount is methanol:phosphorus trichloride=3:1, and the reaction is exothermic. By controlling the injected amount of methanol To control the reaction temperature between 50°C, the solid in the esterification reactor after the reaction is completed is the crude product of dimethyl phosphite;

[0054] Then add an appropriate amount of ammonia to the crude dimethyl phosphite in the neutralization tank for neutralization, the addition of ammonia should be slow, and stop when the pH value of the material in the neutralization tank is 7.2, and the material in the neutralization tank is phosphorous acid A mixture of dimethyl esters and ammonium chloride;

[0055] Then the material in the neutra...

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PUM

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Abstract

The invention provides a recovery method of a rectification residual liquid of dimethyl phosphite. The preparation process comprises steps as follows: methanol and phosphorus trichloride are sprayed to an esterification reaction kettle slowly; a proper amount of ammonia is added to crude dimethyl phosphite in a neutralization tank slowly for neutralization; materials in the neutralization tank are sent to a rectifying tower to be rectified, dimethyl phosphite is completely distilled off, and a rectification residual liquid of dimethyl phosphite is left; the rectification residual liquid of dimethyl phosphite is transferred to a reaction kettle; the rectification residual liquid is subjected to activated carbon decoloration; the decolored liquid is filtered; a proper amount of hydrochloric acid is dropwise added to the filtered liquid, the mixture is sufficiently stirred until acidolysis is sufficient; tail gas generated in the acidolysis process is sent to a chloromethane recovery pipeline in a workshop; after acidolysis is finished, a phosphorous acid water solution in the kettle is concentrated and crystalized. Clean production is realized, discharge of three wastes is reduced, the recovery rate of byproducts is increased, and the production cost is reduced.

Description

technical field [0001] The invention relates to the field of fine chemical production, in particular to a method for recovering dimethyl phosphite rectification raffinate. Background technique [0002] Glyphosate is a herbicide commercialized by Monsanto Company in the United States in 1974. Because of its high efficiency, low toxicity, low residue, broad spectrum, and good environmental compatibility, glyphosate has become the most widely used herbicide in the world. Broad range of herbicides. The production of glyphosate in my country started in the 1980s, mostly using the alkyl ester synthesis process with glycine, dimethyl phosphite, and paraformaldehyde as the main raw materials. This method has stable process and high yield, so it develops very rapidly. The method includes a multi-step reaction process of synthesis, hydrolysis and crystallization. Due to the limitation of equipment materials and other factors, most of them use batch method, which seriously restricts...

Claims

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Application Information

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IPC IPC(8): C07F9/142C07C17/16C07C19/03C01B25/163
CPCC07F9/142C01B25/163C07C17/16
Inventor 刘心龙段利莹杨华左照庆
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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