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Method for synthesizing 99% alpha-chloro-methyl propionate by using micro reaction method

A methyl chloropropionate, microreaction technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of easy production of β-chloropropionic acid, low yield, etc. Environmentally friendly, high product quality, less backmixing effect

Inactive Publication Date: 2018-11-06
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] During the production of α-chloropropionic acid in the reaction kettle, chlorine gas is continuously introduced, which is easy to produce impurities such as β-chloropropionic acid and dichloropropionic acid, resulting in a low yield

Method used

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  • Method for synthesizing 99% alpha-chloro-methyl propionate by using micro reaction method
  • Method for synthesizing 99% alpha-chloro-methyl propionate by using micro reaction method
  • Method for synthesizing 99% alpha-chloro-methyl propionate by using micro reaction method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for synthesizing 99% α-methyl chloropropionate by micro-reaction method, comprising the following steps:

[0030] Step A1, add the mixed solution that is made up of 354.7kg propionic acid, 6.7kg sulfuric acid, 6.2kg phosphorus trichloride in storage tank I; Add 285.5kg methanol in storage tank II; Add 346.9kg chlorine in chlorine gas tank; Tank I is connected to the microreactor through the material delivery channel I, and the delivery power is provided by the liquid platform delivery pump I; the storage tank II is connected to the microreactor through the material delivery channel II, and the delivery power is provided by the liquid platform delivery pump II; the chlorine tank passes through The chlorine delivery device is connected with the microreactor;

[0031] Step A2, turn on the microreactor heating device, raise the temperature to 110°C, turn on the liquid platform delivery pump I, and pass the mixed solution of propionic acid, sulfuric acid and phospho...

Embodiment 2

[0034] A method for synthesizing 99% α-methyl chloropropionate by micro-reaction method, comprising the following steps:

[0035] Step A1, add the mixed solution that is made up of 354.7kg propionic acid, 6.7kg sulfuric acid, 6.2kg phosphorus trichloride in storage tank I; Add 285.5kg methanol in storage tank II; Add 346.9kg chlorine in chlorine gas tank; Tank I is connected to the microreactor through the material delivery channel I, and the delivery power is provided by the liquid platform delivery pump I; the storage tank II is connected to the microreactor through the material delivery channel II, and the delivery power is provided by the liquid platform delivery pump II; the chlorine tank passes through The chlorine delivery device is connected with the microreactor;

[0036] Step A2, turn on the microreactor heating device, raise the temperature to 120° C., turn on the liquid platform delivery pump I, and pass the mixed solution of propionic acid, sulfuric acid and phosp...

Embodiment 3

[0039] A method for synthesizing 99% α-methyl chloropropionate by micro-reaction method, comprising the following steps:

[0040] Step A1, add the mixed solution that is made up of 354.7kg propionic acid, 6.7kg sulfuric acid, 6.2kg phosphorus trichloride in storage tank I; Add 285.5kg methanol in storage tank II; Add 346.9kg chlorine in chlorine gas tank; Tank I is connected to the microreactor through the material delivery channel I, and the delivery power is provided by the liquid platform delivery pump I; the storage tank II is connected to the microreactor through the material delivery channel II, and the delivery power is provided by the liquid platform delivery pump II; the chlorine tank passes through The chlorine delivery device is connected with the microreactor;

[0041] Step A2, turn on the microreactor heating device, raise the temperature to 115° C., turn on the liquid platform delivery pump I, and pass the mixed solution of propionic acid, sulfuric acid and phosp...

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Abstract

The invention discloses a method for synthesizing 99% alpha-chloro-methyl propionate by using a micro reaction method. The method comprises the following steps: putting a mixed liquid consisting of propionic acid, sulfuric acid and phosphorus trichloride into a storage tank I; putting methanol into a storage tank II; introducing chlorine into a chlorine tank; powering on a micro reactor heating device, heating to 110-120 DEG C, and conveying the mixed liquid of propionic acid, sulfuric acid and phosphorus trichloride in the storage I into a micro reactor; at the same time, introducing chlorineinto the micro reactor; after reactions of three to four plates, feeding methanol into the micro reactor to carry out an esterification reaction; carrying out sampling and analysis on a material received at outlets of fifth to sixth plates, and distilling in a distillation tower, thereby obtaining the 99% alpha-chloro-methyl propionate. The method is simple in process, safe in production, environmental-friendly and high in efficiency; due to adoption of the micro reactor, contents of impurities such as beta-chloro-methyl propionate and dichloro-methyl propionate are greatly reduced, and the yield is increased by 94% or greater from 75% of a kettle reaction.

Description

technical field [0001] The invention relates to the field, in particular to a method for synthesizing 99% α-methyl chloropropionate by using a micro-reaction method. Background technique [0002] Methyl α-chloropropionate, also known as methyl 2-chloropropionate, is a product in which α-H of methyl propionate is replaced by chlorine. It is a colorless, clear and transparent liquid with an ether-like odor. In industry, its α-chlorine and carbonyl activities are often used in the synthesis of medicines, pesticides and spices. α-Methyl chloropropionate is an intermediate of fungicides metalaxyl, benalaxyl and procymidone, herbicides diclofop, pretilachlor, etc. [0003] Reactors are used to produce 99% methyl α-chloropropionate by traditional techniques, and the synthetic route is: [0004] [0005] And there is following problem in this synthetic route and can't solve: [0006] During the production of α-chloropropionic acid in the reaction kettle, chlorine gas is contin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08C07C51/363C07C53/19
CPCC07C51/363C07C67/08C07C53/19C07C69/63
Inventor 王进李冬良潘光飞李成斌
Owner 浙江禾本科技股份有限公司