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System and method for continuously synthesizing clethodim

A technology of clethodim and microchannel reactor, which is applied in chemical instruments and methods, thioether preparation, chemical/physical/physicochemical processes, etc. It can solve the problems of long reaction time, low content of clethodim, low yield, etc. problems, to achieve safe preparation, increase the reaction speed, and the effect of continuous preparation

Active Publication Date: 2021-01-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of long reaction time, low yield and low content of clethodim in the existing clethodim synthesis technology

Method used

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  • System and method for continuously synthesizing clethodim
  • System and method for continuously synthesizing clethodim
  • System and method for continuously synthesizing clethodim

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]Chloramine (purity: 93.8%) and triketone (purity: 94.0%) are used as raw materials, and ethanol is used as a solvent. Firstly, triketone is dissolved in ethanol to prepare a triketone ethanol solution with a content of triketone of 50 wt%. Chloramine and refined triketone ethanol solution are pumped feed with flow rate 4ml / min and 20ml / min respectively, and feed time is 5min, and feed amount is respectively: chloramine 21.9g (0.19mol), refined triketone ethanol solution 91.8g (0.16mol), the feed molar ratio of chlorinated amine and fine triketone is 1.19. The two raw materials are strongly mixed and reacted in parallel microchannel reactor I with channel hydraulic diameter of 0.5mm and liquid holding volume of 7.2ml; the reaction materials are further mixed and reacted in microchannel reactor II, and the reaction materials are mixed and reacted in two reaction The total residence time in the device was 43 seconds. At the same time, control the reaction temperature of m...

Embodiment 2-4

[0046] Using the same continuous synthesis system of clethodim as in Example 1, the ethanol solution was obtained by dissolving the triketone in ethanol, and the content of the triketone in the ethanol solution was 50 wt%. Difference with embodiment 1 is: chlorinated amine and refined triketone mol ratio are 1.15, refined triketone flow rate 40ml / min, chlorinated amine flow rate is 8ml / min, the total amount of material in microchannel reactor I and II The reaction residence time was 22 seconds. During the reaction, the reaction temperatures of microchannel reactors I and II were the same. In Examples 2-4, the reaction temperatures were controlled to be 55° C., 65° C., and 70° C. respectively. The product results are shown in Table 1, respectively.

[0047] Table 1, the influence of different temperatures on the reaction

[0048]

[0049] As can be seen from the data in the above table, increasing the reaction temperature will speed up the mixing and mass transfer rate betw...

Embodiment 5-7

[0051] The same system for continuous synthesis of clethodim as in Example 1 was used. The difference with Example 1 is as follows: in the reaction process, the reaction temperature of the reaction material in the microchannel reactor I and II is 75°C, the refined triketone flow rate is 40ml / min, and the chloramine flow rate is 6.5~8ml / min, The residence time is 22 seconds, and the molar ratios of chlorinated amines and refined triketones in the feed are controlled to be 1.10, 1.15, and 1.20, respectively. The product results are shown in Table 2.

[0052] Table 2, the influence of chlorinated amine and fine triketone molar ratio on reaction

[0053]

[0054] As can be seen from the data in the table above, increasing the molar ratio of chlorinated amines and refined triketones, that is, increasing the amount of chlorinated amines, the conversion rate of refined triketones and the yield of clethodim also increase accordingly, and increasing the amount of chlorinated amines...

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Abstract

The invention belongs to the technical field of chemical product synthesis, and relates to a micro-reaction system and method for synthesizing herbicide clethodim. The system is formed by sequentiallyconnecting a micro-channel reactor I, a micro-channel reactor II and a collector in series. The synthesis method comprises the following steps of: by taking an ethanol solution of 5-[2-(ethanethiol)propyl]- 2-propionyl-1, 3-cyclohexanedione (referred to as refined triketone) and chloroallyloxyamine (referred to as chloroamine) as raw materials, respectively and continuously conveying the raw materials into the micro-channel reactor I through a metering pump to realize strong mixing and reaction; and continuing to mix and react the reacted materials in the micro-channel reactor II, controlling the temperature of the system through a heat exchanger, enabling the reaction product to enter the collector, and carrying out acid washing separation to obtain the product clethodim. According to the system and the method, low-energy-consumption, safe and continuous production of clethodim can be realized, the conversion rate of refined triketone is higher than 99% under the condition that themolar ratio of chloramine to refined triketone is 1.20, and the yield of the product clethodim is higher than 95%.

Description

technical field [0001] The invention belongs to the technical field of chemical product synthesis, and in particular relates to a microreactor system and method for synthesizing the herbicide clethodim. Background technique [0002] Clethodim is a cyclohexanone herbicide developed by American Chevron (Chevron) Chemical Company in 1982. This product has the advantages of good herbicidal activity, high selectivity and easy degradation, and has a broad market prospect. [0003] At present, the industry adopts batch reaction to prepare clethodim, first 5-[2-(ethylmercapto) propyl]-2-propionyl-1,3-cyclohexanedione (refined triketone) and Mix petroleum ether, raise the temperature to 30-35°C, then add chlorinated allyloxyamine (chlorinated amine) dropwise, and the dropwise addition is completed in 2-3 hours, keep warm at 30-35°C for 5-6 hours, and detect the fine three When the ketone content is less than 1%, the reaction ends; then, it is washed with acid water, and desolvated u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C07C319/20C07C323/47
CPCB01J19/0046B01J19/0093B01J2219/00867B01J2219/00889C07C319/20C07C323/47
Inventor 陈光文廉应江焦凤军韩梅杨梅尧超群
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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