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Continuous preparation method of herbicide intermediate of 2, 4-dichlorophenol

A technology of dichlorophenol and intermediates, applied in the field of herbicide intermediates 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, etc., to achieve The effect of improving the production site environment, production safety and controllability, and reducing energy consumption

Inactive Publication Date: 2012-09-12
荆州沙隆达控股有限公司
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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 complicated, 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 the chemical synthesis reaction are not high, and the output is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0013] After heating 1,000 parts of phenol to 40°C, it enters the tail gas absorption tower to absorb residual chlorine, and then mixes with 1,500 parts of chlorine in the pre-chlorination tower and enters the chlorination tower from bottom to top. At a temperature of 40-60°C, after a continuous chlorination reaction occurs in a three-stage plate chlorination tower, the liquid material after the reaction can be flowed into a 2,4-dichlorophenol receiving tank, and the yield is 94.19%. The plate-type chlorination tower is made of glass-lined material.

[0014] The tail gas enters the tail gas absorption tower after passing through the separator, and the hydrogen chloride in the tail gas is recovered by water to be an acid with a concentration of 30.5%, and the yield is 97.19%. , Most of the chlorine is not absorbed by water, and returns to the pre-chlorination tower after passing through the water flushing pump, water seal pipe, and dryer.

Embodiment 2

[0016] After heating 1,000 parts of phenol to 40°C, it enters the tail gas absorption tower to absorb residual chlorine, and then mixes with 1,450 parts of chlorine in the pre-chlorination tower and enters the chlorination tower from bottom to top. At a temperature of 60-70°C, after a continuous chlorination reaction occurs in a 5-stage packed chlorination tower, the liquid material after the reaction can be flowed into a 2,4-dichlorophenol receiving tank, and the yield is 95.33%. The packed chlorination tower is made of graphite.

[0017] The tail gas enters the tail gas absorption tower after passing through the separator, and the hydrogen chloride in the tail gas is recovered by water to be an acid with a concentration of 30.5%, and the yield is 80.19%. , Most of the chlorine is not absorbed by water, and returns to the pre-chlorination tower after passing through the water flushing pump, water seal pipe, and dryer.

Embodiment 3

[0019] After heating 1,000 parts of phenol to 40°C, it enters the tail gas absorption tower to absorb residual chlorine, and then mixes it with 1,400 parts of chlorine in the pre-chlorination tower and enters the chlorination tower from bottom to top. At a temperature of 70-80°C, after a continuous chlorination reaction occurs in a 6-stage plate chlorination tower, the liquid material after the reaction can be flowed into a 2,4-dichlorophenol receiving tank, and the yield is 96.03%. The plate type chlorination tower is lined with PTFE.

[0020] The tail gas enters the tail gas absorption tower after passing through the separator, and the hydrogen chloride in the tail gas is recovered by water to be an acid with a concentration of 30.5%, and the yield is 88.23%. , Most of the chlorine is not absorbed by water, and returns to the pre-chlorination tower after passing through the water flushing pump, water seal pipe, and dryer.

[0021] The method of the invention is easy to oper...

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Abstract

The invention provides a continuous preparation method of an herbicide intermediate of 2, 4-dichlorophenol. The method includes the steps of continuously and reversely feeding phenol and chlorine gas in a mass ratio of 1: (1.4-1.5), subjecting fed materials to continuous chlorination reaction through a multistage chlorination tower, enabling reacted liquid materials to flow into a 2, 4-dichlorophenol receiving tank, and recycling the gas with water through a tail gas absorption tower. The continuous preparation method replaces existing batch type mode to prepare the intermediate 2, 4-dichlorophenol of 2, 4-D acid, operation is simple, safety of preparation is controllable, discharge of three wastes is reduced, power consumption is reduced, and unit time output is increased. Simultaneously, the preparation can further improve yield of products, and recycle by-product acid with concentration of 30.5% during the reaction.

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 intermediates 2,4-dichlorophenol. 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 ...

Claims

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Application Information

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IPC IPC(8): C07C39/30C07C37/62
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廖艳
Owner 荆州沙隆达控股有限公司
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