Process of preparing dicamba by 3, 6-dichlorosalicylic acid

A technology of dichlorosalicylic acid and dicamba, which is applied in the field of preparation technology of dicamba and the preparation technology of herbicide dicamba, can solve the problems of low utilization rate of equipment, reduced waste water volume, long saponification time, etc., and achieves the utilization of equipment. Increased efficiency, reduced waste water, and automated effects

Inactive Publication Date: 2016-08-31
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The present invention aims to solve the problems of low yield, long saponification time, large amount of waste water and low utilization rate of equipment in the existing process for preparing dicamba by using 3,6-dichlorosalicylic acid, and provides a method using 3,6-dichlorosalicylic acid to prepare dicamba. The process of preparing dicamba from dichlorosalicylic acid can greatly increase the yield, shorten the saponification reaction time, significantly reduce the amount of waste water, and increase the utilization rate of equipment

Method used

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  • Process of preparing dicamba by 3, 6-dichlorosalicylic acid
  • Process of preparing dicamba by 3, 6-dichlorosalicylic acid

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Embodiment 1

[0039] A process for preparing dicamba using 3,6-dichlorosalicylic acid, comprising the following process steps:

[0040] A. Methylation reaction

[0041] Dissolve 3,6-dichlorosalicylic acid in lye, pump it into the methylation continuous reactor, fill it with methyl chloride gas, and add lye and methanol solution of the catalyst dropwise at the same time to carry out the methylation reaction. After the reaction is completed, the pressure is released to obtain a methylation reaction solution;

[0042] B. Saponification reaction

[0043] Put the methylation reaction solution obtained in step A into the saponification continuous reactor, add lye, keep the reaction temperature at 100°C, the pressure at 0.10MPa, and the time of 0.2h, after the reaction is complete, cool down to 30°C, release the pressure, and obtain the saponification reaction solution;

[0044] C. Recovery of methanol

[0045] The saponification reaction solution obtained in step B is entered into a distillati...

Embodiment 2

[0049] A process for preparing dicamba using 3,6-dichlorosalicylic acid, comprising the following process steps:

[0050] A. Methylation reaction

[0051] Dissolve 3,6-dichlorosalicylic acid in lye, pump it into the methylation continuous reactor, fill it with methyl chloride gas, and add lye and methanol solution of the catalyst dropwise at the same time to carry out the methylation reaction. After the reaction is completed, the pressure is released to obtain a methylation reaction solution;

[0052] B. Saponification reaction

[0053] Put the methylation reaction solution obtained in step A into the saponification continuous reactor, add lye, keep the reaction temperature at 140°C, the pressure at 0.50MPa, and the time for 1.5h, after the reaction is complete, cool down to 90°C, release the pressure, and obtain the saponification reaction solution;

[0054] C. Recovery of methanol

[0055] The saponification reaction solution obtained in step B is entered into a distillat...

Embodiment 3

[0059] A process for preparing dicamba using 3,6-dichlorosalicylic acid, comprising the following process steps:

[0060] A. Methylation reaction

[0061]Dissolve 3,6-dichlorosalicylic acid in lye, pump it into the methylation continuous reactor, fill it with methyl chloride gas, and add lye and methanol solution of the catalyst dropwise at the same time to carry out the methylation reaction. After the reaction is completed, the pressure is released to obtain a methylation reaction solution;

[0062] B. Saponification reaction

[0063] Put the methylation reaction solution obtained in step A into the saponification continuous reactor, add lye, keep the reaction temperature at 120°C, the pressure at 0.30MPa, and the time of 0.9h, after the reaction is complete, cool down to 60°C, release the pressure, and obtain the saponification reaction solution;

[0064] C. Recovery of methanol

[0065] The saponification reaction solution obtained in step B is entered into a distillatio...

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Abstract

The invention relates to a process of preparing dicamba by 3, 6-dichlorosalicylic acid, and belongs to the technical field of herbicide dicamba preparation processes. The process includes the steps of methylation reaction, saponification, methanol recovery, acidizing reaction and the like. By means of saponification with specific process parameters, efficiency can be greatly improved, saponification time is shortened, wastewater quantity is remarkably reduced, and equipment utilization rate is increased.

Description

technical field [0001] The invention relates to a preparation process of dicamba, more specifically, the invention relates to a process for preparing dicamba by using 3,6-dichlorosalicylic acid, which belongs to the technical field of the preparation process of herbicide dicamba. Background technique [0002] Dicamba is a benzoic acid herbicide, which has systemic conduction effect and has a significant control effect on annual and perennial broad-leaved weeds. Dicamba is used for post-emergence spraying, and the agent can be quickly absorbed by the leaves, stems and roots of weeds , conducts upward and downward through the phloem, and is mostly concentrated in the meristem and the part with vigorous metabolic activity, hindering the normal activity of plant hormones, thereby causing them to die. Poaceae plants can quickly metabolize and decompose the drug after absorbing it to make it ineffective, so they show strong drug resistance. It is relatively safe for grass crops s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/21C07C51/02C07C51/41
CPCC07C51/02C07C51/412C07C67/31C07C65/21C07C69/92
Inventor 彭琼王长江张安邦张弦张华王蕾
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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