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Method and device for continuous acylation synthesis of pretilachlor

A technology of chemical synthesis and pretilachlor, which is applied in the field of preparation of pretilachlor, can solve the problems of frequent personnel operations, long cycle time, unstable batch product quality, etc.

Active Publication Date: 2021-05-28
NUTRICHEM LAB CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to overcome the defects of long cycle, frequent personnel operation and unstable batch product quality in the existing process of synthesizing pretilachlor, and provide a simple and efficient continuous acylation method for synthesizing pretilachlor and a continuous Device for acylation synthesis of pretilachlor

Method used

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  • Method and device for continuous acylation synthesis of pretilachlor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Such as figure 1 Shown, raw material 2,6-diethylanilinopropyl ether (amine ether), chloroacetyl chloride, liquid caustic soda and toluene are metered by the first flowmeter 8 and the first regulating valve 9 is adjusted with 600L / h, 200L respectively / h, 265L / h, and 690L / h flow rates are pumped to the reactor body 101 (volume 5000L) through 4 feed lines, and the residence time is 2.3h. A stirring unit is arranged inside the reaction kettle body 101, and a stirring motor 6 for driving the stirring unit is arranged at the central position of the outer top of the reaction kettle body 101. The stirring unit includes a stirring rod 51 and a propulsion stirrer 52 arranged up and down along the stirring rod 51 axial direction And the turbine agitator 53, four baffles 7 are evenly arranged along the inner wall of the reactor body 101 in the circumferential direction. The raw materials 2,6-diethylanilinopropyl ether, chloroacetyl chloride, liquid caustic soda and toluene are in...

Embodiment 2

[0074] Such as figure 1 As shown, the raw materials 2,6-diethylanilinopropyl ether, chloroacetyl chloride, liquid caustic soda and toluene are metered by the first flow meter 8 and adjusted by the first regulating valve 9 at 1000L / h, 335L / h, and 442L respectively. / h, the flow rate of 1150L / h is pumped to the reactor body 101 (volume is 6300L) respectively through 4 feeding pipelines, and the residence time is: 1.72h. A stirring unit is arranged inside the reaction kettle body 101, and a stirring motor 6 for driving the stirring unit is arranged at the central position of the outer top of the reaction kettle body 101. The stirring unit includes a stirring rod 51 and a propulsion stirrer 52 arranged up and down along the stirring rod 51 axial direction And the turbine agitator 53, four baffles 7 are evenly arranged along the inner wall of the reactor body 101 in the circumferential direction. The raw materials 2,6-diethylanilinopropyl ether, chloroacetyl chloride, liquid caust...

Embodiment 3

[0076] According to the method of Example 1, the difference is that the stirring unit does not include the propulsion agitator 52 arranged axially along the stirring rod 51, that is, only the turbine agitator 53 provides turbine agitation for the materials in the reactor. The purity of the obtained pretilachlor is 95%, and the yield is 92%.

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Abstract

The invention relates to the field of preparation of pretilachlor, and discloses a method and device for continuous acylation synthesis of pretilachlor, the method comprising: 2,6-diethylanilinopropyl ether, chloroacetyl chloride, alkali source and The solvent is subjected to a contact reaction in the reactor to obtain a recycle stream a and a product stream b, and the recycle stream a is cooled by heat exchange and then circulated back to the reactor. The continuous acylation method for synthesizing pretilachlor provided by the invention not only has a high degree of automation and simple operation, but also has high purity and yield of the obtained pretilachlor product. The device for continuous acylation synthesis of pretilachlor provided by the invention occupies a small area, saves manpower while ensuring stable quality of acylation products, and is very suitable for industrial application.

Description

technical field [0001] The invention relates to the field of preparation of pretilachlor, in particular to a method and a device for continuous acylation synthesis of pretilachlor. Background technique [0002] Pretilachlor is a high-efficiency, low-toxicity, selective budding herbicide for paddy fields, which belongs to the transporting herbicide. The chemical name of pretiachlor: 2-chloro-2',6'-diethyl-N-(2-propoxyethyl)-N-acetylaniline, foreign common name: Pretiachlor, trade name: Rifit solnet. Successfully developed by Ciba-Geigy in Switzerland in 1979, it is an amide herbicide developed as a herbicide for transplanting rice. It can be used for manual or mechanical transplanting of rice fields, and can control most of the weeds in rice fields. , such as Cyperaceae plants and a variety of broad-leaved weeds, when used together with the safener Jiechadine, it can improve the safety of this agent on rice buds and seedlings, and can prevent and control rice field daughter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/02C07C233/18
CPCC07C231/02C07C233/18
Inventor 涂俊清张静张战葛喜乐王海艳
Owner NUTRICHEM LAB CO LTD
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