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Industrial Clean Production Process of Captan

A technology of clean production and captan, applied in the field of pesticides, can solve problems such as low yield, inoperability of workers, strong odor, etc., and achieve the effect of high product yield, simple operation process and process method

Active Publication Date: 2011-12-14
YINGDE GREATCHEM CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The inventor has found through countless experiments that no matter how the existing captan production process changes the reaction conditions, it cannot make the trichlorothiochloromethane (ClSCCl) as raw material wherein 3 ) fully reacted completely
Due to the strong odor and high toxicity of trichlorothiochloromethane gas, if it remains in the product, it will cause workers to be unable to operate during post-processing and filtration, thereby affecting industrial production
In order to overcome the above problems, at present, an organic solvent is used as a reaction medium and an organic amine is used as an acid-binding agent to synthesize captan, because the organic solvent can dissolve the unreacted trichlorothichloromethane, thereby achieving the removal of trichlorothiochloromethane odor and its purpose of remaining in the product, but the captan yield of this process is only 40-80%, the yield is low, and triethylamine remains in the product, and at the same time, due to the need to recycle the solvent in industrial production, the operation Complexity, increased production costs, and serious environmental pollution due to the use of organic solvents, workers exposed to highly toxic solvents for a long time, harming human health

Method used

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  • Industrial Clean Production Process of Captan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 150 milliliters of water to a 250 milliliter four-necked bottle equipped with a stirrer, a thermometer and a dropping device. Start stirring and add 9.0 grams (content 96.0%) sodium hydroxide (or replace with 30.0-50.0wt% liquid sodium hydroxide) to dissolve, then add 30.0 grams (content 98.0wt%) 1,2,3,6-four The hydrophthalimide was dissolved for 0.5 hour, and 37.5 g (content 98.0 wt%) of trichlorothiochloromethane was added dropwise at 0-30° C., and kept for 2.0 hours. The acidity of the reaction material indicated the end of the reaction. The material is transferred to a purifying and temperature-intensive treatment kettle, heated to 50-60° C., kept for 3.0 hours, then cooled to 20° C., filtered, washed twice with 20 ml of water, and dried to obtain the original drug of captan. Yield 89.8%; Content 97.1wt% (Japan Shimadzu high performance liquid chromatograph external standard method quantification; Standard product captan fusing point is 178 ℃); Trichlorothiochl...

Embodiment 2

[0016] Add 150 milliliters of water in a 250 milliliter four-necked bottle equipped with stirrer, thermometer and dropping device, add 34.4 grams (content 98.0wt%) 1,2,3,6-tetrahydrophthaloyl under stirring Sodium, after dissolving, add 37.5 g (content 98.0wt%) of trichlorothiochloromethane dropwise at 0-30° C., and keep warm for 2.0 hours. The acidity of the reaction material indicates the end of the reaction. Transfer the material to a purifying and heating treatment kettle, heat up to 50-60°C, keep the temperature for 3.0 hours, then cool down to 20°C, filter, wash twice with 20 ml of water, and dry to obtain the original drug of captan. Yield 90.02%; Content 97.2wt% (Japan Shimadzu high performance liquid chromatograph external standard method quantification; Standard product captan fusing point is 178 ℃); Trichlorothiochloromethane content below 0.01wt% (gas chromatography internal standard method Quantitative); THPI content 0.28wt% (Japan Shimadzu high performance liquid...

Embodiment 3

[0018] The temperature of the purified heat treatment of the reacted material in Example 1 was increased from 50-60° C. to 70-80° C., while other conditions remained unchanged, to obtain the original drug of captan. The yield is 88.5%, the content is 96.9wt%, the THPI content is 0.32wt%, the trichlorothiochloromethane content is less than 0.01wt%, and the sodium chloride content is 0.18wt%. (The detection method is the same as above)

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Abstract

The invention relates to an industrial clean production process of captan, which is characterized in that it comprises the following steps: adding water into a reaction kettle, adding an alkali metal compound and 1,2,3,6-tetrahydrophthalamide under stirring imide or directly add phthalimide salt, after it is completely dissolved, add trichlorothiochloromethane dropwise at 0-30°C, and keep warm for 0.5-3.0 hours. Then the material is transferred to a purification and temperature-increasing treatment kettle, heated to 50-100° C., kept at this temperature for 0.5-5.0 hours, then cooled, filtered, rinsed, and dried to obtain the original drug of decaptan.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to an industrial clean production process of captan. Background technique [0002] Captan, the common name is captan, and the chemical name is N-(trichloromethylthio)cyclohex-4-ene-1,2-dicarboximide, which is a low-toxicity, broad-spectrum product developed by Chevron Chemical Company. Organic sulfur fungicides can be used to prevent and control various diseases on barley, rice, corn, cotton, vegetables, fruit trees, melons, tobacco and other crops, such as wheat rust, rice blast, tobacco black nitrile, apple rot, scab , powdery mildew, scab, etc., can also be mixed with a variety of pesticides. Captan is still the best-selling fungicide in Europe and some Asian regions. Its chemical structure is as follows: [0003] [0004] The inventor has found through countless experiments that no matter how the existing captan production process changes the reaction conditions, it cannot make th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
Inventor 贾凤聪蔡丹群覃建海黄汪海苏晓明吴光辉
Owner YINGDE GREATCHEM CHEM
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