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Method for preparing diethyl chlorophosphite

A technology of diethyl chlorophosphite and triethyl phosphite, which is applied in the field of preparing diethyl chlorophosphite, can solve the problems of low reaction yield, adding catalyst and the like, so as to simplify the operation process and improve the product content , the effect of reducing the cost of synthesis

Active Publication Date: 2020-03-06
山东亿盛实业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems in the prior art that catalyst needs to be added, reaction yield is low and safety risks exist, a method for preparing diethyl chlorophosphite is now provided to solve the above problems

Method used

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  • Method for preparing diethyl chlorophosphite
  • Method for preparing diethyl chlorophosphite
  • Method for preparing diethyl chlorophosphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for preparing diethyl chlorophosphite, the specific synthesis steps are as follows:

[0030] Microchannel reactor model: RMCS1010, single-chip reaction unit liquid holding capacity 0.75mL, pipeline and joint liquid holding capacity 2.9mL; two infusion pump models: PF100 semi-preparative medium-pressure infusion pump.

[0031] (1) 500 g of triethyl phosphite is continuously delivered to the pre-cooling module A of the microchannel reactor, and the temperature of the triethyl phosphite is controlled to be 10° C., and the pre-cooling module A is connected to the channel A;

[0032] (2) 207g of phosphorus trichloride is delivered to the pre-cooling module B, and the temperature of the phosphorus trichloride is controlled to be 10° C.; the pre-cooling module B is connected to the channel B; the channel A and the channel B are respectively connected to the reaction module;

[0033] (3) open channel A and channel B, adjust the triethyl phosphite feeding pump flow rate...

Embodiment 2

[0038] A method for preparing diethyl chlorophosphite, the specific synthesis steps are as follows:

[0039] Microchannel reactor model: RMCS402, single-chip reaction unit liquid holding capacity 9.2mL, pipeline and joint liquid holding capacity 7.8mL; two infusion pump models: PF100 semi-preparative medium-pressure infusion pump.

[0040] (1) 10 kg of triethyl phosphite is continuously delivered to the pre-cooling module A of the microchannel reactor, and the temperature of the triethyl phosphite is controlled to be 0° C., and the pre-cooling module A is connected to the channel A;

[0041] (2) 4.13 kg of phosphorus trichloride is delivered to the pre-cooling module B, and the temperature of the phosphorus trichloride is controlled to be 0° C.; the pre-cooling module B is connected to the channel B; the channel A and the channel B are respectively connected to the reaction module;

[0042] (3) open channel A and channel B, adjust the triethyl phosphite feeding pump flow rate ...

Embodiment 3

[0047] A method for preparing diethyl chlorophosphite, the specific synthesis steps are as follows:

[0048] Microchannel reactor model: RMCS402, single-chip reaction unit liquid holding capacity 9.2mL, pipeline and joint liquid holding capacity 7.8mL; two infusion pump models: PF100 semi-preparative medium-pressure infusion pump.

[0049] (1) 50kg of triethyl phosphite is continuously delivered to the pre-cooling module A of the microchannel reactor, and the temperature of the triethyl phosphite is controlled to be -5°C, and the pre-cooling module A is connected to the channel A;

[0050] (2) 20.66 kg of phosphorus trichloride is delivered to the pre-cooling module B, and the temperature of the phosphorus trichloride is controlled to be -5°C; the pre-cooling module B is connected to the channel B; the channel A and the channel B are respectively connected to the reaction module;

[0051] (3) open channel A and channel B, adjust the triethyl phosphite feeding pump flow rate to...

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Abstract

The invention relates to a method for preparing diethyl chlorophosphite, and belongs to the technical field of fine chemical engineering. The method comprises the following specific steps: a channel Ais triethyl phosphite, a channel B is phosphorus trichloride, the channel A and the channel B are opened, and according to flux of a microchannel reactor, the triethyl phosphite and the phosphorus trichloride are mixed in a reaction module; and as the two materials are continuously pumped in, the diethyl chlorophosphite is continuously obtained at a material outlet, and the reaction is completeduntil the materials are all fed in. The method has the following beneficial effects: (1) in the absence of a catalyst, by controlling the feeding amount and the reaction temperature, the high-yield high-quality product is prepared by using the microchannel reactor; (2) no phosphorus trichloride remaining in the product, the risk of safety accidents is reduced, and damage to the environment is avoided; (3) the synthetic cost of diethyl methylphosphonite is reduced; and (4) the method realizes continuous production, simplifies the operation process, and reduces the production costs.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for preparing diethyl chlorophosphite. Background technique [0002] Diethyl chlorophosphite reacts with Grignard reagent methylmagnesium chloride to prepare diethyl methylphosphonite, which is an important raw material for the herbicide glufosinate-ammonium. In the prior art, diethyl chlorophosphite is synthesized batchwise in a kettle mode, and phosphorus trichloride is added dropwise to triethyl phosphite with a catalyst at a certain temperature. This method needs to add additional catalyst, and the reaction time is long, and the real yield of reaction (yield% * content %) is about 85%, which makes the cost of diethyl methylphosphonite high. And in the reaction, phosphorus trichloride is excessive and the reaction is not complete, so that more phosphorus trichloride remains in the product. Excess phosphorus trichloride will remain in the reaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/146
CPCC07F9/146
Inventor 王永昌刘顺领赵吉祥郭廷松王尊永刘朝月
Owner 山东亿盛实业股份有限公司
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