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Continuous preparation method of herbicide intermediate 2, 4-dichlorphenoxyacetic acid

A technology of sodium dichlorophenoxyacetate and intermediates, which is applied in the field of herbicide intermediates 2, can solve the problems of difficult production management, many side reactions, and high labor intensity, so as to improve the production site environment and controllable production safety , the effect of reducing labor intensity

Active Publication Date: 2012-09-12
先正达集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2,4-D acid showed high activity in common auxin quantification method, but its effect was quite low in oat elongation test using standard auxin quantification method
2,4-D acid can be transferred quite quickly in plants. According to the results of 14C tracing, it is confirmed that this substance undergoes rapid catabolism in the order of carboxyl carbon and then methylene carbon, but its benzene nucleus is not Not easy to disassemble
There are outstanding problems such as poor mass transfer effect, many side reactions, low product yield, poor quality, low production efficiency, high labor intensity, large equipment investment, high manufacturing cost, difficult production management, and poor production stability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0012] 2,4-dichlorophenol and chloroacetic acid with a molar ratio of 1:1.2 are configured into an aqueous solution with a concentration of 35% and a concentration of 45%, and at a temperature of 80°C, successive reactions occur through three-stage condensation reaction towers, And the pH of the reaction is controlled to be 8 by adding a sodium hydroxide aqueous solution with a concentration of 30%. The content of the material analysis is: 2,4-dichlorophenol sodium: 0.1%, chloroacetic acid: 0.5%, sodium salt: 32.03%; Finally, the temperature of the reacted liquid material was lowered to 35° C. by reusing water, and suction filtration was performed to obtain the sodium 2,4-dichlorophenoxyacetate with a yield of 96.13%.

Embodiment 2

[0014] 2,4-dichlorophenol and chloroacetic acid with a molar ratio of 1:1.4 are configured into an aqueous solution with a concentration of 35% and a concentration of 45%, and at a temperature of 100°C, successively react through 4 stages of condensation reaction towers, And by adding the sodium carbonate aqueous solution that concentration is 30%, the mode control reaction pH is 10, gets material analysis content: 2,4-sodium dichlorophenolate: 0.1%, chloroacetic acid: 0.5%, sodium salt: 33.82%; Finally The liquid material after the reaction was cooled to 40° C. by reusing water and suction-filtered to obtain the sodium 2,4-dichlorophenoxyacetate with a yield of 98.00%.

Embodiment 3

[0016] 2,4-dichlorophenol and chloroacetic acid with a molar ratio of 1:1.5 are configured into aqueous solutions with a concentration of 35% and a concentration of 45%, and at a temperature of 110°C, successively react through five stages of condensation reaction towers, And the pH of the reaction is controlled to be 12 by adding a potassium hydroxide aqueous solution with a concentration of 30%. The content of the material analysis is: 2,4-dichlorophenol sodium: 0.1%, chloroacetic acid: 0.1%, sodium salt: 30.17%; Finally, the reacted liquid material was cooled to 45° C. by reusing water and filtered with suction to obtain the sodium 2,4-dichlorophenoxyacetate with a yield of 95.07%.

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PUM

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Abstract

The invention provides a continuous preparation method of herbicide intermediate 2, 4-dichlorphenoxyacetic acid, which comprises the steps of subjecting 2, 4-dichlorphenoxyacetic acid with a mole ratio of 1: (1.2-1.5) and chloroacetic acid to consecutive reaction through a multistage condensation reaction tower at a temperature of 80-110 DEG C, controlling the PH value of the reaction to be 8-12 through addition of alkali liquor, and finally cooling the liquid material after reaction, subjecting the liquid material to suction filtration and obtaining the 2, 4- dichlorphenoxyacetic acid. Existing interval methods are replaced with the continuous preparation method for preparing the herbicide 2, 4-D acid intermediate 2, 4-dichlorphenoxyacetic acid, the preparation method is easy to operate, the production is safe and can be controlled, the labor intensity of workers is reduced greatly, the production field environment is improved, the safety of the reaction is improved, the discharge of the three wastes is reduced and the production during unit time is increased.

Description

technical field [0001] The invention belongs to the field of preparation methods of herbicide 2,4-D acid intermediates, in particular to a continuous preparation method of herbicide intermediate 2,4-dichlorophenoxyacetic acid sodium. Background technique [0002] 2,4-dichlorophenoxyacetic acid is a representative synthetic plant growth hormone (auxin), referred to as 2,4-D acid. 2,4-D acid shows high activity in common auxin quantification method, but its effect is quite low in oat elongation test using standard auxin quantification method. And it turns purple when treated with chromotropic acid, so it can be used for colorimetric quantification. Since Zimmerman (P.W.Zimmermann, 1942) discovered the role of 2,4-D acid, many synthetic auxins centered on this substance have developed rapidly in agriculture. This substance is used on a large scale as a herbicide and an agent for preventing early fruit abscission. 2,4-D acid can be transferred quite quickly in plants. Accordi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/70C07C51/41C07C51/367
Inventor 刘国平刘跃李作荣李波殷宏刘建华薛光才鄢圣光熊金华张世钢李传林范文涛
Owner 先正达集团股份有限公司
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