Synthesis method and synthesis device of diethyl methylphosphite

Abstract

The invention relates to a synthesis method and a synthesis device of diethyl methylphosphite. The synthesis method comprises the following steps: (1) mixing methyl phosphine dichloride, absolute ethyl alcohol and a solvent to carry out a synthesis reaction; (2) carrying out reduced pressure deacidification treatment on the reaction solution obtained in the step (1); and (3) separating and purifying the deacidified reaction solution obtained in the step (2) to obtain diethyl methylphosphite. According to the synthesis method, an acid-binding agent is not needed, hydrogen chloride gas generatedby the synthesis reaction can be discharged through reduced-pressure deacidification treatment, the generation of solid waste residues containing acid-binding agent hydrochloride is avoided, the separation and treatment of the solid waste residues are reduced, and the dosage of ethanol is reduced by adding a solvent, so that the ethanol does not need to play a role as a solvent, the energy consumption is reduced, the resources are saved, the process is high in yield, simple to operate and environment-friendly, and the atom economy is good.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing diethyl methylphosphonite and a synthesis device thereof. Background technique [0002] Diethyl methylphosphonite is a very important organic intermediate, mainly used in the synthesis of herbicide glufosinate-ammonium and flame retardant. At present, the synthesis methods of diethyl methylphosphonite mainly include the Grignard reagent method and the esterification method of methylphosphonite dichloride. [0003] The Grignard reagent method mainly includes three key steps: Grignard reaction, phosphorylation reaction and esterification reaction. For example, CN103374030A discloses a method for preparing glufosinate-ammonium and a preparation method of an intermediate thereof, wherein the synthetic method of diethyl methylphosphinate as an intermediate is as follows: first pass phosphorus trichloride and triethyl phosphite The reaction obtain...

AI Technical Summary

Problems solved by technology

Although the method does not need to use an acid-binding agent, the temperature of the synthesis reaction is as high as 85-120°C, and the higher temperature can easily lead to the occurrence of side reactions

[0009] Therefore, although the methyl phosphine dichloride esterification method has less pollution, it needs to use a large amount of various inorganic or organic acid-binding agents to generate solid waste residue containing acid-binding agent hydrochloride, and the reaction process control requirements are relatively high, otherwise Very easy to produce by-products

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