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Synthesis process of glyphosate intermediate dimethyl phosphite

A technology for the synthesis of dimethyl phosphite and a synthesis process, which is applied in the field of synthesis technology of glyphosate intermediate dimethyl phosphite, can solve the problems of difficult metering control, frequent operations, high labor intensity, etc., and achieves improved efficiency. Conversion rate, avoid acid hydrolysis side reaction, shorten the effect of reaction time

Inactive Publication Date: 2017-12-22
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] At present, the industrial production of dimethyl phosphite has been using the batch method of single-pot reaction and single-pot rectification. The reaction materials are fed through the high-level tank, and the measurement control is difficult, and the reaction needs to be controlled below 55°C. , frequent operations, high labor intensity, long production cycle and low equipment capacity
At the same time, the heat of reaction needs to be removed by freezing during the reaction process, and the material needs to be heated during deacidification, so the energy utilization rate in the production process is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 64Kg of methanol is measured by the methanol metering tank and enters the esterification reaction kettle, and 106Kg of phosphorus dichloride enters the esterification reaction kettle after passing through the metering tank. Still, the gas generated by the esterification reaction returns to the esterification kettle through the first and second condensers of the esterification, and the feed liquid in the deacidification kettle is dehydrogenated under high vacuum and steam heating conditions, and the feed liquid in the deacidification kettle is deacidified Then enter the rectification kettle for rectification to obtain more than 99% of dimethyl phosphite, pass the aforementioned hydrogen chloride gas into ammonia water, and add a protective agent therein, and the protective agent is dichloroethane. Turn on the stirring system for stirring during the aforementioned esterification reaction, and the stirring time is 15 minutes. Turn on the heat conduction oil heating system d...

Embodiment 2

[0034]65.8Kg of methanol is measured into the esterification reaction kettle through the methanol metering tank, 106Kg of phosphorus dichloride enters the esterification reaction kettle after passing through the metering tank, and the materials enter at the same time according to the proportion. Acid tank, the gas generated by the esterification reaction is returned to the esterification tank through the first and second grade condensers of the esterification, and the feed liquid in the deacidification tank is dehydrogenated under high vacuum and steam heating conditions, and the deacidification of the deacidification tank is carried out. The liquid enters the rectifying kettle for rectification to obtain more than 99% of dimethyl phosphite, and the aforementioned hydrogen chloride gas is passed into ammonia water, and a protective agent is added thereto, and the protective agent is ethylene dichloride. Turn on the stirring system for stirring during the aforementioned esterifi...

Embodiment 3

[0039] 66.3Kg of methanol is measured into the esterification reaction kettle through the methanol metering tank, 106Kg of phosphorus dichloride enters into the esterification reaction kettle after passing through the metering tank, and the materials enter at the same time according to the proportion. Acid tank, the gas generated by the esterification reaction is returned to the esterification tank through the first and second grade condensers of the esterification, and the feed liquid in the deacidification tank is dehydrogenated under high vacuum and steam heating conditions, and the deacidification of the deacidification tank is carried out. The liquid enters the rectifying kettle for rectification to obtain more than 99% of dimethyl phosphite, and the aforementioned hydrogen chloride gas is passed into ammonia water, and a protective agent is added thereto, and the protective agent is ethylene dichloride. Turn on the stirring system for stirring during the aforementioned es...

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PUM

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Abstract

The present invention relates to a synthesis process of glyphosate intermediate dimethyl phosphite, the steps are as follows: methanol is metered through a methanol metering tank and enters an esterification reactor, phosphorus dichloride is metered through a metering tank and enters the esterification reactor, materials enter the esterification reactor simultaneously in ratio, after esterification reaction, a material liquid flows into a deacidification kettle via an inner liquid seal tube, a gas generated by the esterification reaction returns back to the esterification reactor via a first condenser and a secondary condenser, hydrogen chloride is removed form the material liquid in the deacidification kettle under high vacuum and steam heating conditions, and after deacidification by the deacidification kettle, the material liquid enters a rectifying kettle for rectifying. Continuous production of the dimethyl phosphite can be achieved, a great development space is provided for production capacity improvement and further significant reduction of operating cost, and purity is increased to 99.0% or more.

Description

technical field [0001] The invention relates to the field of pesticide processing, in particular to a synthesis process of a glyphosate intermediate dimethyl phosphite. Background technique [0002] Dimethyl phosphite is an important product in fine chemical industry. It is not only an intermediate for the production of glyphosate, trichlorfon, rice blast, omethoate and other pesticides, but also a raw material for organophosphorus corrosion inhibitors, dye additives, plastic additives and flame retardants, and can be used for synthetic water treatment It can also be used as a methylating agent to synthesize quaternary ammonium salt fungicides, antistatic agents, softeners and other products. [0003] Dimethyl phosphite is generally prepared industrially from the reaction of phosphorus trichloride and methanol: PCl 3 +3CH 3 OH→(CH 3 O) 2 POH+2HCl↑+CH 3 The Cl↑ reaction process and mechanism are: [0004] PCl 3 +CH 3 OH→CH 3 OPCl 2 +HCl↑(1) [0005] CH 3 OPCl 2 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 黄中桂蔡小林袁晓林付志平史正光朱凯明黄锋杨镭郑宏亮刘心龙
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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