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Continuous preparation method for phytocide 2,4-D acid

A herbicide and sulfuric acid technology, applied in the field of herbicide 2, can solve the problems of chemical synthesis reaction selection and low yield, complex stirred tank reactor structure, and difficult to disassemble the benzene nucleus, so as to improve the production site environment , safe and controllable production, and the effect of reducing energy consumption

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
The structure of the stirred tank reactor is complex, the power consumption and cooling consumption are large, the material is not mixed uniformly, and the product quality cannot be guaranteed
The selection and yield of chemical synthesis reactions are not high, and the output is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0014] In the first tower reactor, 2,4-dichlorophenoxyacetic acid sodium and hydrochloric acid are added in a volume ratio of 1:1 through the chain control of the metering pump, and the reaction temperature is controlled at 100°C. continuous response. Then the reacted material overflows into the first cooling tower, cools down to 80°C through the jacket circulating water, and then overflows into the second cooling tower and cools down to below 50°C through the coil. Finally, the cooled material was filtered and washed in an automatic centrifuge to obtain the 2,4-D acid with a purity of 98.5% and a yield of 98%.

Embodiment 2

[0016] In the first tower reactor, 2,4-dichlorophenoxyacetic acid sodium and hydrochloric acid are added in a volume ratio of 1.2:1 through the interlock control of the metering pump, and the reaction temperature is controlled at 90 ° C. continuous response. Then the material in the reactor is overflowed into the second tower reactor for continuous reaction. The reacted material then overflows into the first cooling tower, cools down to 75°C through the jacket circulating water, and then overflows into the second cooling tower and cools down to below 50°C through the coil. Finally, the cooled material overflowed into a bag filter for suction filtration and washing to obtain the 2,4-D acid with a purity of 98.0% and a yield of 97%.

Embodiment 3

[0018] In the first tower reactor, 2,4-dichlorophenoxyacetic acid sodium and sulfuric acid are added in a volume ratio of 1.5:1 through the chain control of the metering pump, and the reaction temperature is controlled at 50 ° C. continuous response. Then the material in the reactor overflows to the second tower reactor and the third tower reactor successively, and continuous reaction takes place. The reacted material then overflows into the first cooling tower, cools down to 70°C through the jacket circulating water, and then overflows into the second cooling tower and cools down to below 50°C through the coil. Finally, the cooled material overflowed into a bag filter for suction filtration and washing to obtain the 2,4-D acid with a purity of 97.6% and a yield of 97%.

[0019] The yield of the herbicide 2,4-D acid continuously prepared by the method of the invention can be increased to 97%, and more than 10 tons can be prepared per hour. Both the yield and the output are g...

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Abstract

The invention provides a continuous preparation method for phytocide 2,4-D acid, which comprises the following steps: continuously reacting 2,4-sodium dichlorphenoxyacetic acid with acid, of which a volume ratio is (1-1.5):1, in a multistage tower reactor under the temperature at 50-100 DEG C, and then introducing the materials after reacting into a cooling tower and cooling the materials to be below 50 DEG C, and lastly, filtering and cleaning the materials after being cooled, thereby obtaining the phytocide 2,4-D acid. According to the invention, the present intermittent method is replaced by the continuous preparation method for preparing the phytocide 2,4-D acid; the operation is convenient and the production is safe and controllable; the labor intensity of workers is greatly reduced, the energy consumption is reduced and the unit time output is increased; and meanwhile, according to the continuous preparation method provided by the invention, the reactive solubility is increased, the generation of byproduct is reduced and the yield of product is increased.

Description

technical field [0001] The invention belongs to the field of preparation methods of herbicides, in particular to a continuous preparation method of herbicide 2,4-D acid. 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. According to the results of 14C tracing, it is confirmed that this subs...

Claims

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Application Information

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IPC IPC(8): C07C59/135C07C51/02
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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