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Novel technology for synthesizing acetochlor intermediate chloroethyl methyl ether

A technology of chloromethyl ethyl ether and synthesis process, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of low etherification rate, cumbersome process, low utilization rate of hydrochloric acid, etc., and achieve improvement Improve quality, simplify process steps, and reduce the effect of material turnover process

Active Publication Date: 2014-05-21
SHANDONG VICOME GREENLAND CHEMICAL CO LTD
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Problems solved by technology

[0004] In order to solve the problems of cumbersome process, low utilization rate of hydrochloric acid and low etherification rate, the present invention provides a new synthesis process of acetochlor intermediate chloromethyl ethyl ether

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  • Novel technology for synthesizing acetochlor intermediate chloroethyl methyl ether

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Embodiment Construction

[0015] Aiming at the problems of cumbersome steps in the existing synthesis process, low utilization rate of raw materials and low etherification rate, the present invention provides a new synthesis process of acetochlor intermediate chloromethyl ethyl ether. The new synthesis process comprises the following steps:

[0016] (1) Put the ammonium chloride into the ether distillation still containing the etherified base acid, mix well, add concentrated sulfuric acid dropwise at a uniform speed and stir, and the ammonium chloride will generate hydrogen chloride gas under the action of concentrated sulfuric acid;

[0017] (2) After drying the hydrogen chloride gas obtained in step (1) through concentrated sulfuric acid, it is passed into the etherification reaction kettle containing paraformaldehyde and ethanol, and the temperature is kept at about 60°C. When there is a large amount of The reaction ends when hydrogen chloride gas that has not participated in the reaction comes out. ...

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Abstract

The invention discloses a novel technology for synthesizing acetochlor intermediate chloroethyl methyl ether. The novel technology for synthesizing acetochlor intermediate chloroethyl methyl ether comprises the following steps of putting ammonium chloride into an ether distillation still containing an etherified base acid, mixing well, adding dropwisely concentrated sulfuric acid into the mixture at a uniform speed with stirring so that ammonium chloride and concentrated sulfuric acid undergo a reaction to produce hydrogen chloride gas, feeding the obtained hydrogen chloride gas into an etherification reactor containing paraformaldehyde and ethanol, and keeping a temperature below 70 DEG C, wherein when a mass of the unreacted hydrogen chloride gas in the etherification reactor escapes, the etherification reaction is finished. The novel technology provided by the invention has the advantages that 1, hydrochloric acid is replaced by the etherified base acid, so that processes are simplified; a hydrogen chloride gas generation technology and an etherified base acid distillation technology are combined; a material circulation flow is simplified; and a hydrochloric acid use amount is reduced, and 2, the obtained hydrogen chloride gas is dried by concentrated sulfuric acid and then is fed into the etherification reactor so that ether quality is improved.

Description

technical field [0001] The invention relates to an etherification process in the synthesis of acetochlor, in particular to a new synthesis process of acetochlor intermediate chloromethyl ethyl ether. Background technique [0002] As we all know, acetochlor is an excellent herbicide, which is widely used in corn, cotton, peanut and soybean fields for pre-emergent weeding. [0003] At present, the synthesis of acetochlor mainly includes several processes of condensation, etherification, acylation, and desolventization, and etherification includes several independent process units such as hydrogen chloride gas generation, etherification, and bottom acid distillation. First, put ammonium chloride and hydrochloric acid into the hydrogen chloride generating kettle, turn on the stirring and vacuum, add concentrated sulfuric acid dropwise at a constant speed, and react to obtain hydrogen chloride; the generated hydrogen chloride is passed into the etherification reaction kettle to p...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/22C07C43/12
Inventor 来庆利李先江朱立军董金居张成林
Owner SHANDONG VICOME GREENLAND CHEMICAL CO LTD
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