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Continuous flow preparation method of diethyl methyl phosphite

A technology of diethyl methyl phosphite and methyl phosphorus dichloride, which is applied in the field of preparation of pesticide intermediates, can solve problems such as difficulty in realization, cumbersome recovery process, and low recovery rate, and achieve safe and efficient production, solve The effect of low efficiency and high degree of automation

Pending Publication Date: 2020-04-14
LIER CHEM CO LTD +1
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Problems solved by technology

In this method, organic bases such as N,N-dimethylaniline or N,N-diethylaniline are used as acid-binding agents, which have the disadvantages of high price, cumbersome recovery process and low recovery rate. There are problems such as long time-consuming, low efficiency and high safety risks in the dropping process
[0004] In the esterification reaction of methyl phosphorus dichloride and ethanol, the patent CN107236002A uses sodium ethoxide as an acid-binding agent, which has an advantage over organic bases in terms of raw material cost, but there are still problems of long time consumption, low efficiency and large safety risks. question
Shi Hongxin and others disclosed the method of using ammonia as an acid-binding agent in "Jiangsu Chemical Industry". This method clearly stated that the pH of the reaction solution should be controlled at 7.0-8.5, and the ammonia flux and actual reaction speed should be strictly controlled during the operation. It is relatively difficult to achieve a balance between

Method used

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  • Continuous flow preparation method of diethyl methyl phosphite
  • Continuous flow preparation method of diethyl methyl phosphite
  • Continuous flow preparation method of diethyl methyl phosphite

Examples

Experimental program
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Effect test

Embodiment 1-19

[0056] Such as figure 1 As shown, ethanol is passed into reactor module one for precooling, methylphosphorous dichloride is passed into reactor module two for precooling, and ethanol and methylphosphorous dichloride are in reactor module three Mixing, flow through reactor module three, completes the substitution reaction to generate a mixture containing diethyl methylphosphite and HCl.

[0057] The ammonia-saturated ethanol solution (the amount of ammonia is 25wt%) was filled in a three-necked bottle in advance, the bottle was corked, and placed in a -30°C cold bath environment. After the mixture exits the continuous flow microreactor, it is connected to a three-necked bottle containing ammonia-saturated ethanol solution, and the mixture is directly passed into the ammonia-saturated ethanol solution precooled to -30°C, and mixed with the ammonia-saturated ethanol solution.

[0058] The calculation method of the amount of ammonia saturated ethanol solution is as follows:

[0...

Embodiment 16

[0077] Embodiment 16 is continuous mixing, and the molar ratio of ammonia to methyl phosphorus dichloride is 2.2:1 per unit time; The mol ratios of phosphorus dichloride are respectively 2.2:1 and 5:1; Embodiment 17 is the tank type mixing of additional ammonia gas again, and the mol ratio of ammonia total amount and methyl phosphorus dichloride in the ammonia-saturated ethanol solution is 2.2:1, the molar ratio of additional ammonia to methyl phosphorus dichloride is 0.05:1. The results show that the increase of ammonia consumption is beneficial to the control of product purity. Furthermore, the continuous mixing method of tubular structure is better.

[0078] According to the method of the foregoing embodiment, the continuous mixing method of the tubular structure is adopted, and the molar ratio of the fixed materials is methyl phosphorus dichloride:ethanol:ammonia=1:10:2.2. Different water contents are screened in methyl phosphorus dichloride, including 0.13wt%, 0.08wt%, ...

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Abstract

The invention discloses a continuous flow preparation method of diethyl methyl phosphite, which comprises the following steps: continuously adding ethanol and methyl phosphorus dichloride into a feedport of a continuous flow reactor, and continuously obtaining diethyl methyl phosphite at a discharge port of the continuous flow reactor. The method has the advantages of small liquid holdup, safe and efficient production process, solving of the problems of long reaction time and low efficiency in kettle type reaction, high product yield and purity, and simple and efficient process operation.

Description

technical field [0001] The present invention relates to the preparation method of pesticide intermediate, more specifically relate to the continuous flow preparation method of diethyl methyl phosphite. Background technique [0002] Diethyl methyl phosphite is a key intermediate of the herbicide glufosinate-ammonium. [0003] Patents WO200905716, Tetrahedron (1982), 38, 2513, J.Am.Chem.Soc. (1958), 80, 1150, etc. disclose the preparation of methyl phosphorus dichloride and ethanol by esterification under the action of an acid-binding agent Diethyl methyl phosphite, the yield is about 90%. In this method, organic bases such as N,N-dimethylaniline or N,N-diethylaniline are used as acid-binding agents, which have the disadvantages of high price, cumbersome recovery process and low recovery rate. There are the problems of long time consumption, low efficiency and high safety risk in the dropping process. [0004] In the esterification reaction of methyl phosphorus dichloride a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/48B01J19/00
CPCC07F9/4866B01J19/0093
Inventor 程柯蒋海军徐敏杨清来红刚尹英遂
Owner LIER CHEM CO LTD
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