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The preparation technology of 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt

A chlorophenoxyacetic acid dimethylamine salt and a preparation process technology, which is applied in the field of preparation of 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt, can solve the problems of precipitation and low use efficiency, and achieve no precipitation , low cost, and the effect of process route optimization

Inactive Publication Date: 2011-12-21
JIANGSU JIANGU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt products generally have precipitation phenomenon, and the use efficiency is low

Method used

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  • The preparation technology of 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt
  • The preparation technology of 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1. Add chloroacetic acid to the reaction kettle, add 30% caustic soda solution dropwise to neutralize the reaction, control the temperature at 5°C, and the pressure at normal pressure. When the pH value of the material is 7-8, it is the end of the reaction and sodium chloroacetate is generated;

[0017] 2. Add o-cresol to another reactor, control the temperature at 25°C, the pressure at normal pressure, and the reaction time for 35 minutes. Add 30% caustic soda solution dropwise to react to generate o-cresol sodium. After the reaction, heat preservation is performed;

[0018] 3. Add the sodium chloroacetate from the previous kettle to the o-cresol sodium reaction kettle of the next kettle through the metering tank, control the temperature at 125°C, the reaction time for 9 hours, and the pressure at normal pressure to produce 2 methylbenzene through condensation reaction Sodium oxyacetate;

[0019] 4. Transfer the above reaction materials to the chlorination reactor, add hydroc...

Embodiment 2

[0023] 1. Add chloroacetic acid to the reaction kettle, add 30% caustic soda solution dropwise to neutralize the reaction, control the temperature at 25°C, and the pressure at normal pressure. When the pH value of the material is 7-8, it is the end of the reaction and sodium chloroacetate is generated;

[0024] 2. Add o-cresol to another reactor, control the temperature at 40°C, the pressure at normal pressure, and the reaction time for 25 minutes. Add 30% caustic soda solution dropwise to react to generate o-cresol sodium. After the reaction, heat preservation is performed;

[0025] 3. Add the sodium chloroacetate from the previous kettle to the o-cresol sodium reaction kettle in the next kettle through the metering tank, control the temperature to 130°C, the reaction time is 8 hours, and the pressure is normal pressure, and 2 methylbenzene is produced through condensation reaction Sodium oxyacetate;

[0026] 4. Transfer the above reaction materials to the chlorination reactor, add ...

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Abstract

The invention discloses a dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid. The specific process steps are as follows: 1. adding chloroacetic acid to a reaction kettle, and dripping caustic soda solution to generate sodium chloroacetate; Phenol is added to another reactor, and caustic soda solution is added dropwise to generate sodium o-cresol; 3, the sodium chloroacetate of the previous kettle is added dropwise to the sodium o-cresol reactor of the next kettle to generate sodium 2-methylphenoxyacetate; 4. Transfer the above reaction materials into a chlorination reaction kettle, add hydrochloric acid to generate 2-methylphenoxyacetic acid crystals, add a mixed solvent of xylene and dichloroethane to dissolve the crystals into a solution, and carry out chlorination in the chlorination reaction kettle Reaction, generate 2-methyl-4-chlorophenoxyacetic acid, then transfer to the crystallization tank for crystallization, then put it into a centrifuge for centrifugation, and dry it into crystals after centrifugation; 4 Chlorine, dimethylamine aqueous solution and water are respectively added in the salt-forming reactor to generate the product 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt. The preparation process has few reaction steps, safe process, high efficiency, short cycle and low cost.

Description

Technical field [0001] The invention relates to a preparation process of 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt. Background technique [0002] 2-Methyl-4-chlorophenoxyacetic acid dimethylamine salt, abbreviated as 2methyl4-chlorodimethylamine salt solution, is a kind of phenoxycarboxylic acid herbicide with high efficiency, low toxicity, low residue and no weeds Resistance to environmental friendliness. It is widely used in the control of annual or perennial broad-leaved weeds in paddy fields, wheat fields, corn, sugarcane and other gramineous crop fields. At present, 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt products generally have precipitation phenomenon, and the use efficiency is low. Summary of the invention [0003] The invention discloses a process for preparing 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt, and aims to provide a process for preparing a 2-methyl-4-chlorodimethylamine salt solution with a reasonable ratio and a content...

Claims

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Application Information

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IPC IPC(8): C07C211/04C07C209/68C07C59/70C07C51/41
Inventor 张领
Owner JIANGSU JIANGU CHEM
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