Continuous production processes of dicamba methyl ester and dicamba methyl ester emulsifiable concentrate

A dicamba methyl ester and production process technology, applied in the field of pesticides, can solve the problems of high production cost, great human injury, complicated process route, etc., achieve product yield and purity improvement, improve production operation environment, and simple process route Effect

Inactive Publication Date: 2019-05-17
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] As a traditional dosage form, emulsifiable concentrate has the advantages of good drug efficacy and simple operation, but its disadvantages are also prominent, such as complex process route, high difficulty, low safety, in

Method used

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  • Continuous production processes of dicamba methyl ester and dicamba methyl ester emulsifiable concentrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Dissolve 90kg of salicylic acid in 900kg of 98% sulfuric acid at 5°C, keep it warm for 30 minutes until dissolved, add 63.6kg of bromine to generate 5-bromosalicylic acid, heat up to 35°C to pass chlorine, and synthesize 5-bromo-3 - Chlorosalicylic acid, add 360kg sulfur trioxide, 4.5kg iodine, heat preservation 50 ℃ and carry out reaction to synthesize 5-bromo-3,6-dichlorosalicylic acid, after the reaction is completed, dilute fuming sulfuric acid to 30% in terms of sulfuric acid concentration %, washed with water and dried to obtain 5-bromo-3,6-dichlorosalicylic acid. (From salicylic acid to 5-bromo-36-dichlorosalicylic acid yield is 75%)

[0076] Add 140kg of 5-bromo-3,6-dichlorosalicylic acid to 600kg of 10% liquid caustic soda, raise the temperature to 50°C until it is fully dissolved, add 60kg of tin metal powder, and react for 1 hour to control 5-bromo-3,6- Dichlorosalicylic acid is completely converted into 3,6-dichlorosalicylic acid, the metal powder is separa...

Embodiment 2

[0081] Dissolve 90kg of salicylic acid in 900kg of 98% sulfuric acid at 5°C, keep it warm for 30 minutes until dissolved, add 63.6kg of bromine to generate 5-bromosalicylic acid, heat up to 35°C to pass chlorine, and synthesize 5-bromo-3 - Chlorosalicylic acid, add 360kg sulfur trioxide, 4.5kg iodine, heat preservation 50 ℃ and carry out reaction to synthesize 5-bromo-3,6-dichlorosalicylic acid, after the reaction is completed, dilute fuming sulfuric acid to 30% in terms of sulfuric acid concentration %, washed with water and dried to obtain 5-bromo-3,6-dichlorosalicylic acid. (From salicylic acid to 5-bromo-36-dichlorosalicylic acid yield is 75%)

[0082] Add 140kg of 5-bromo-3,6-dichlorosalicylic acid into 600kg of 10% liquid caustic soda, raise the temperature to 50°C until it is completely dissolved, add 60kg of aluminum metal powder, and react for 1 hour to control 5-bromo-3,6 -Dichlorosalicylic acid is completely converted to 3,6-dichlorosalicylic acid, and the metal po...

Embodiment 3

[0087] Dissolve 90kg of salicylic acid in 900kg of 98% sulfuric acid at 5°C, keep it warm for 30 minutes until dissolved, add 63.6kg of bromine to generate 5-bromosalicylic acid, heat up to 35°C to pass chlorine, and synthesize 5-bromo-3 - Chlorosalicylic acid, add 360kg sulfur trioxide, 4.5kg iodine, heat preservation 50 ℃ and carry out reaction to synthesize 5-bromo-3,6-dichlorosalicylic acid, after the reaction is completed, dilute fuming sulfuric acid to 30% in terms of sulfuric acid concentration %, washed with water and dried to obtain 5-bromo-3,6-dichlorosalicylic acid. (From salicylic acid to 5-bromo-36-dichlorosalicylic acid yield is 75%)

[0088] Add 140kg of 5-bromo-3,6-dichlorosalicylic acid into 600kg of 10% liquid caustic soda, raise the temperature to 50°C until it is fully dissolved, add 60kg of zinc metal powder, and react for 1 hour to control 5-bromo-3,6 -Dichlorosalicylic acid is completely converted to 3,6-dichlorosalicylic acid, and the metal powder is s...

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Abstract

The invention provides a continuous production process of dicamba methyl ester. The process comprises the following steps: A) 5-bromo-3,6-dichlorosalicylic acid is subjected to a reaction under an alkaline condition and under the action of metal powder to remove bromine atoms in para-positions of hydroxyl, and 3,6-dichlorosalicylic acid is obtained; B) 3,6-dichlorosalycylic acid and halomethane are subjected to an etherification reaction in a mixed solvent of water and methanol, and methyl 3,6-dichloro-2-methoxybenzoate is obtained; C) methanol is removed by distillation; D) a system after distillation is left to stand for laying, an organic phase is distilled, and dicamba methyl ester is obtained. By means of the preparation process, continuous production can be realized, workers are notrequired to make direct contact with materials, the control degree is high, the production operation environment is greatly improved and safer, the process route and equipment are simple, the production cost is low, besides, the product yield and purity are greatly improved, and a superior route suitable for mass industrial production is provided.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a continuous production process of dicamba methyl and its emulsifiable oil. Background technique [0002] Dicamba (dicamba), also known as Baicao, has a chemical name of 3,6-dichloro-2-methoxybenzoic acid, a herbicide of the benzoic acid family, and is a low-toxicity, high-efficiency, broad-spectrum herbicide , It has a significant control effect on annual and perennial broad-leaved weeds, but it is relatively safe on grass crops such as wheat, corn, millet, and rice. With the prohibition and restriction of metsulfuron-methyl and chlorsulfuron-methyl preparations, the safety, human health and super weed problems caused by glyphosate have become increasingly prominent. As a traditional high-efficiency herbicide, dicamba has attracted attention and is resistant to dicamba With the continuous development of genetically modified crops, dicamba ushers in new opportunities for deve...

Claims

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Application Information

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IPC IPC(8): C07C67/11C07C67/31C07C67/54C07C69/92A01N25/02A01N37/40A01P13/00
Inventor 孙国庆侯永生李尊亮胡义山周长涛
Owner SHANDONG RUNBO BIOTECH CO LTD
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