Industrialized cleaning production process of captan

A technology for cleaner production and sterilization, applied in the field of pesticides, can solve the problems of workers being unable to operate, increasing production costs, harming human health, etc., and achieving the effect of simple operation process and process method, safe and reliable production process, and reduction of three waste discharges.

Active Publication Date: 2010-01-13
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 folpet 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 selected as the reaction medium, and an organic amine is used as an acid-binding agent to synthesize fendol, because the organic solvent can dissolve the unreacted trichlorothichloromethane, thereby achieving the removal of trichlorothiochloromethane odor and the purpose of residues in the product, but the yield of faldol in this process is only 40-80%, the yield is low, and there are residues of triethylamine in the product. Simultaneously, due to the need to recycle the solvent in industrial production, it causes The operation is complicated, the production cost increases, and due to the use of organic solvents, the environment is seriously polluted, and workers are exposed to highly toxic solvents for a long time, which will damage human health

Method used

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  • Industrialized cleaning 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. Add 8.3 grams (content 96.0%) sodium hydroxide and 30.0 grams phthalimide (content 98.0wt%) and catalyst benzyltriethylammonium chloride after starting to stir, dissolve 0.5 hour, then mix mixture in 4 37.5 g (content 98.0 wt%) of trichlorothiochloromethane was added dropwise at ℃, and the reaction was kept for 2.0 hours. If the reaction material turned sour, it indicated that the reaction was over. Transfer the material to a purification and temperature-raising treatment kettle, heat up to 50-60°C, keep the temperature for 3.0 hours, then cool down to 20°C and filter, wash the filter cake twice with 20 ml of water, and dry to obtain the light yellow white non-flammable powder Setting solid powder. Yield 89.8%; content 97.1% (quantitative by external standard method of Japan Shimadzu high performance liquid chromatography; standard substance...

Embodiment 2

[0016] The temperature of the purified heat treatment of the reacted material in Example 1 is increased from 50-60° C. to 70-80° C., and the other conditions remain unchanged, so as to obtain the original drug of fendan. The yield is 88.5%, the content is 96.9 wt%, the content of phthalimide is 0.65 wt%, the content of trichlorothiochloromethane is less than 0.01 wt%, and the content of sodium chloride is 0.18 wt%. (detection method is with embodiment 1)

Embodiment 3

[0018] The material reacted in Example 1 is purified and heat-treated at 50-60° C. to 90-100° C., kept for 2.0 hours, and other conditions remain unchanged, to obtain the sterilized elixir. The yield is 89.3%, the content is 97.02wt%, the content of trichlorothiochloromethane is less than 0.01wt%, the content of phthalimide is 0.55wt%, and the content of sodium chloride is 0.2wt%. (detection method is with embodiment 1)

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Abstract

The invention relates to an industrialized cleaning production process of captan, which is characterized by comprising the following steps: adding the water into a reaction kettle, stirring the water and adding an alkali metal compound and phthalimide or directly adding phthalimide salt and adding a catalyst; dripping perchloromethylmercaptan at 0-30 DEG C after the compounds are completely dissolved; keeping the temperature and reacting for 0.5-3.0 hours; transferring the material to a purifying and temperature-rising processing kettle; heating and rising the temperature to 50-100 DEG C; keeping the temperature for 0.5-5.0 hours; and cooling, filtering, washing and drying to obtain the captan original medicine.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to an industrial clean production process of folpet. Background technique [0002] Folpet, the common name is folpet, and the chemical name is N-(trichloromethylthio)phthalimide, which is a low-toxic, broad-spectrum organic sulfur fungicide developed by Chevron Chemical Company. Vegetable downy mildew, powdery mildew, leaf spot, etc. have good preventive and protective effects. Foldan 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 folpet production process changes the reaction conditions, it cannot make the trichlorothiochloromethane (ClSCCl) as raw material wherein 3 ) fully reacted thoroughly. Due to the strong odor and high toxicity of trichlorothiochloromethane gas, if it remains in the product, it will cause workers t...

Claims

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Application Information

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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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