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Preparation method of chlorophenoxycarboxylic acid

A technology of chlorophenoxy carboxylic acid and chlorophenoxy fatty alcohol, which is applied in the field of preparation of chlorophenoxy carboxylic acid, can solve the problems of high pressure in the treatment of three wastes, loss of active ingredients, poor chlorination selectivity, etc., and achieve improvement Product quality, avoiding effective costs, and improving the effect of chlorination selectivity

Inactive Publication Date: 2018-12-07
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The chlorination selectivity of the above method is poor, the post-treatment process will cause the loss of active ingredients, and the yield of the product is low
At the same time, when phenol is used as a raw material to synthesize chlorinated phenoxycarboxylic acid through chlorination and condensation, a large amount of waste water containing hydroxycarboxylic acid and waste salt will be produced, and a large amount of hazardous waste containing chlorophenol and chlorophenoxycarboxylic acid will be produced. Waste, three wastes treatment pressure, high treatment cost

Method used

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  • Preparation method of chlorophenoxycarboxylic acid
  • Preparation method of chlorophenoxycarboxylic acid
  • Preparation method of chlorophenoxycarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Add 139.58g 99% phenoxyethanol (1mol), 0.21g 99% aluminum oxide and 1.19g 99% 2,4,5-tri-tert-butylisothiazole successively to a 500mL four-necked flask, and pass through at -20°C Inject 154.69g of 99% chlorine gas, complete the heat preservation reaction for 30min, distill at 1kpa pressure and collect fractions at 110-120°C to obtain 207.89g of 2,4-dichlorophenoxyethanol with a content of 99.1%. The yield is expressed as phenoxyethanol Ethanol 99.48%.

[0051] Add 18.71g of ZSM-5 molecular sieve to the distilled 2,4-dichlorophenoxyethanol as a catalyst, add 415.8g of water, feed 99.9% oxygen to a pressure of 0.7MPa, react at 130°C, and feed a total of 38.44g Oxygen, filter at 90°C after the reaction is completed, cool the filtrate to 15°C, filter to obtain 2,4-dichlorophenoxyacetic acid wet material, dry the wet material to obtain 221.71g of 2,4-dichlorophenoxyacetic acid, content 98.8% , the yield is 99.08% based on phenoxyethanol.

[0052] Utilize nuclear magnetic r...

Embodiment 2

[0060] Add 139.58g of 99% phenoxyethanol (1mol), 0.77g of 99% magnesium chloride and 0.35g of 99% 4,4'-dichlorophenylsulfide to a 500mL four-necked flask, and add 137.70 g of 99% sulfuryl chloride, after dripping and keeping warm for 30 minutes, distill at 1kpa pressure and collect fractions at 105-115°C to obtain 173.31g of 4-chlorophenoxyethanol, with a content of 98.8%, and a yield of 99.24% based on phenoxyethanol .

[0061] Add 10.40 g MoO to the distilled 4-chlorophenoxyethanol 3 As a catalyst, add 390.0g of water, feed 99.9% oxygen to a pressure of 0.1MPa, react at 80°C, feed a total of 36.84g of oxygen, filter at 80°C after the reaction is completed, cool the filtrate to 15°C, and filter to obtain 4-chloro The wet material of phenoxyacetic acid was dried to obtain 187.16 g of 4-chlorophenoxyacetic acid with a content of 98.5%, and the yield was 98.84% based on phenoxyethanol.

Embodiment 3

[0063] Add 167.92g 99% phenoxybutanol (1mol), 0.08g 99% zinc chloride and 1.26g 99% 3,4-dichlorothiophene successively in a 500mL four-necked flask, and feed 157.56 g 99% chlorine gas, heat preservation reaction for 30min, distill at 1kpa pressure and collect fractions at 120-130°C to obtain 236.06g of 2,4-dichlorophenoxybutanol with a content of 98.9%. Alcohol 99.34%.

[0064] Add 16.52g of activated carbon as a catalyst to the distilled 2,4-dichlorophenoxybutanol, add 236.1g of water, feed air to a pressure of 1.2MPa, and react at 60°C. A total of 220.95g of air is fed, and the reaction is completed in Filter at 95°C, cool the filtrate to 15°C, filter to obtain 2,4-dichlorophenoxybutyric acid wet material, dry the wet material to obtain 2,4-dichlorophenoxybutyric acid 249.85g, content 98.6%, yield 98.94% based on phenoxybutanol.

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Abstract

The invention provides a preparation method of chlorophenoxycarboxylic acid, wherein the preparation method includes the following steps: S1) carrying out 2-site and / or 4-site selective chlorination reaction of phenoxy fatty alcohol with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxy fatty alcohol, wherein the catalyst A is Lewis acid, and the catalyst B is C5-22 thioethers, thiazoles, isothiazoles and thiophenes or halogenated derivatives thereof; and S2) carrying out catalytic oxidation reaction of chlorophenoxy fatty alcohol and water with anoxidizing agent under the action of a catalyst to obtain chlorophenoxycarboxylic acid. By redesigning of the process route and fine screening of the catalysts and the chlorinating agent, the method effectively reduces energy consumption, improves chlorination selectivity and avoids loss of effective components. The content of the obtained chlorophenoxycarboxylic acid can reach 98.5% or more and the total yield can reach 99% or more.

Description

technical field [0001] The invention relates to the technical field of herbicide preparation, in particular to a preparation method of chlorophenoxycarboxylic acid. Background technique [0002] At present, the preparation method of chlorophenoxycarboxylic acid mainly includes the following steps: [0003] 1) Using phenol as the main raw material, chlorinated phenols are obtained through chlorination. The chlorophenol produced in this step has an extremely unpleasant pungent odor, which leads to a very poor production site environment and poor chlorination selectivity. [0004] 2) Chlorophenol is condensed with chlorinated carboxylic acid under alkaline conditions, and the reaction solution is acidified and filtered to obtain chlorophenoxycarboxylic acid wet material, which is dried to obtain chlorophenoxycarboxylic acid. During the condensation process of the dichlorophenol or polychlorophenol in the chlorophenol in this step, condensation between two molecules will occur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/255C07C59/70C07C59/68
CPCC07C41/22C07C51/255C07C59/70C07C59/68C07C43/225
Inventor 孙国庆侯永生张利国迟志龙胡义山
Owner SHANDONG RUNBO BIOTECH CO LTD
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