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Preparation process of trifluoromethyl sulfinyl chloride

A technology of trifluoromethylsulfinyl chloride and sodium trifluoromethylsulfinate, which is applied in the direction of organic chemistry, can solve the problems of high energy consumption in production methods, increased production costs of catalysts, and low product yields, achieving a reduction in The effect of high production cost, high purity and high yield

Inactive Publication Date: 2017-05-24
JIANGSU TUOQIU AGRI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although this patent uses sodium trifluoromethyl sulfinate and thionyl chloride as raw materials, its production method has high energy consumption, low product yield, and the use of catalysts increases production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Throw 2700kg of thionyl chloride into a 3000-liter still.

[0046] 2. Close the valve after feeding. Turn on the steam to raise the temperature to reflux, then turn off the steam to make the system dry, and start to add sodium trifluoromethylsulfinate when the temperature drops to 0°C.

[0047] 3. Keep 0~5℃ to cast sodium trifluoromethanesulfinate with a conversion rate of 675kg, and put the jacketed brine after the end. Heat the circulating water to 15-20°C and keep it warm for 7 hours, and then start to distill it into the rectification kettle. When the temperature of the distillation kettle reaches 95℃, turn off the steam and drop the water to wash the kettle when the temperature drops below 10℃.

[0048] 4. After discharging the waste water, check whether the inside of the kettle is broken, and then dry the kettle. After the waste water is discharged, open the manhole cover and check whether the enamel in the reaction kettle is damaged. If the enamel is damaged,...

Embodiment 2

[0053] 1. Throw 2600kg of thionyl chloride into a 3000-liter still.

[0054] 2. Close the valve after feeding. Turn on the steam to raise the temperature to reflux, then turn off the steam to make the system dry, and start to add sodium trifluoromethylsulfinate when the temperature drops to 0°C.

[0055] 3. Keep 0~5°C and pour sodium trifluoromethanesulfinate with a conversion rate of 600kg, and put the jacketed brine after the end. Heat the circulating water to 15-20°C and keep it warm for 5 hours, and then start to distill it into the rectification kettle. When the temperature of the distillation kettle reaches 95℃, turn off the steam and cool down to below 10℃, and then add water to wash the kettle dropwise.

[0056] 4. After discharging the waste water, check whether the inside of the kettle is damaged, and then dry the kettle. After the waste water is discharged, open the manhole cover and check whether the enamel in the reaction kettle is damaged. If the enamel is damag...

Embodiment 3

[0061] 1. Throw 2,800kg of thionyl chloride into a 3,000-liter still.

[0062] 2. Close the valve after feeding. Turn on the steam to raise the temperature to reflux, then turn off the steam to make the system dry, and start to add sodium trifluoromethylsulfinate when the temperature drops to 0°C.

[0063] 3. Keep 0~5°C and throw sodium trifluoromethanesulfinate with a conversion rate of 700kg, and put the jacketed brine after the end. Heat the circulating water to 15-20°C and keep it warm for 8 hours, and then start to distill it into the rectification kettle. When the temperature of the distillation kettle reaches 95℃, turn off the steam and cool down to below 10℃, and then add water to wash the kettle dropwise.

[0064] 4. After discharging the waste water, check whether the inside of the kettle is damaged, and then dry the kettle. After the waste water is discharged, open the manhole cover and check whether the enamel in the reaction kettle is damaged. If the enamel is da...

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Abstract

The invention provides a preparation process of trifluoromethyl sulfinyl chloride. The preparation process comprises the steps as follows: 1) a synthesis kettle is taken, and thionyl chloride is added; 2) thionyl chloride is heated until reflux and cooled to 0-5 DEG C, and sodium trifluoromethanesulfinate is fed; 3) the temperature is increased to 15-20 DEG C, distillation is performed, the steam is turned off and the temperature is reduced to 10 DEG C or lower when the temperature reaches 90-100 DEG C, and water is added to clean a distillation kettle; 4) the material is distilled into a rectifying still, the rectifying still starts to heat up, front cut fractions are collected after reflux for 3-5 hours, whether the material in the reflux pipe is transparent is observed when the temperature reaches 40-45 DEG C, and a finished product of trifluoromethyl sulfinyl chloride is collected if the material is transparent, and reflux is continued if the material is not transparent; 5) the finished product is stopped from being collected when the temperature reaches 45-50 DEG C, reflux is continued, and the finished product of trifluoromethyl sulfinyl chloride continues to be collected after the reflux temperature is reduced. The process is simple to operate, is green and has no pollutant discharge during preparation, is energy-saving, consumption-reducing and good in economic benefit, an adopted solvent is recyclable, obtained trifluoromethyl sulfinyl chloride has high purity and yield, and the production cost can be effectively reduced.

Description

technical field [0001] The invention belongs to the field of production of pesticide intermediates, and in particular relates to a production process of trifluoromethylsulfinyl chloride. Background technique [0002] Fipronil, common name in English is fipronil, chemical name (RS)-5-amino-1-(2,6-dichloro-a,a,a-trifluoro-p-tolyl)-4-trifluoromethyl Sulfinylpyrazole-3-carbonitrile, molecular formula: C 12 h 4 Cl 2 f 6 N 4 OS, molecular weight: 437.2, CAS number: 120068-37-3. [0003] Fipronil is a phenylpyrazole insecticide with a wide insecticidal spectrum. It mainly has gastric toxicity to pests, and also has contact killing and certain systemic effects. Its mechanism of action is to hinder insect γ-aminobutyric acid Controlled chloride metabolism, so it has high insecticidal activity against important pests such as aphids, leafhoppers, planthoppers, Lepidoptera larvae, flies and Coleoptera, and has no phytotoxicity to crops. The agent can be applied to the soil or spr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C313/02
CPCC07C313/02
Inventor 廖大章廖大泉孙伯文
Owner JIANGSU TUOQIU AGRI CHEM CO LTD
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