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Device and method for preparing captan

A technology for captandan and a reaction device, which is applied in the field of devices for preparing captandan, can solve the problems of cumbersome reaction steps, waste of water resources, a large amount of water sources, etc., and achieves the effects of eliminating the hydrolysis of phthalic anhydride, having significant economic benefits and low reaction temperature.

Pending Publication Date: 2018-08-31
NINGXIA G R FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are obvious shortcomings in the above-mentioned preparation method: (1) the reaction steps are loaded down with trivial details, and the intermediate (phthalimide) needs to be purified to more than 99% before it can be used in the next step reaction and obtain qualified grams of bacteria If the intermediate is directly used in the next step without purification, the crude captan obtained in the end must be purified to obtain qualified captan; in addition, purification requires a large amount of water, resulting in a large amount of waste water, not only waste precious water resources, but also bring pressure on environmental protection
(2) The raw material used is toxic and odorous thichloromethane, and it cannot react completely, and the environmental protection is poor
Although the above-mentioned preparation method has solved the technical problem that the toxic and odorous raw material thiochloromethane cannot be completely reacted and the environmental protection is poor, the crude product of captan obtained in the end has to be purified to obtain the qualified captan original drug, and the product is the highest. The content is 97.2%, and the yield is 90.3%; and the steps of the above preparation method are cumbersome, the reaction residence time is long, and continuous production is not possible

Method used

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  • Device and method for preparing captan
  • Device and method for preparing captan
  • Device and method for preparing captan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] (1) According to phthalic anhydride, NH 3 , NaOH, trichlorothiochloromethane in a mol ratio of 1: 1.05: 1: 0.98 to get each raw material; drop into 15Kg phthalic anhydride (99.5%) and 7.2Kg ammoniacal liquor (content 25%) in the primary reactor, at 10m / s Carry out strong mixing under the stirring line speed of 10m / s, enter secondary reactor after staying 5min; Add 12.61Kg sodium hydroxide solution (content 32%) in secondary reactor again, carry out strong mixing under the stirring line speed of 10m / s After staying for 5 minutes, enter the third-stage reactor; then add 18.57Kg trichlorothiochloromethane (99%) to the third-stage reactor, and react at -5°C to 0°C under high-shear stirring at 2900r / min 15min (sequentially through the third-stage reactor for 5min, the fourth-stage reactor for 5min and the fifth-stage reactor for 5min), the reaction product was obtained;

[0072](2) After the reaction product obtained in step (1) was filtered, it was dried at 105° C. to 115°...

Embodiment 2

[0077] (1) According to phthalic anhydride, NH 3 , NaOH, trichlorothiochloromethane in a molar ratio of 1:1:1.05:0.98 to get each raw material; drop 15Kg phthalic anhydride (99.5%) and 6.86Kg ammonia water (content 25%) into the primary reactor, and enter after staying for 2min Secondary reactor; Add 13.24Kg sodium hydroxide solution (content 32%) in secondary reactor again, enter tertiary reactor after staying 10min; Add 18.00Kg trichlorothiochloromethane ( 99%), under high-shear stirring at 2800r / min, react at -5°C to 0°C for 19min (stop in the third-stage reactor for 15min, the fourth-stage reactor for 2min and the fifth-stage reactor for 2min), get the reaction product;

[0078] (2) After the reaction product obtained in step (1) was filtered, it was dried at 105° C. to 115° C. for 20 minutes to obtain 29.53 Kg of the original captan.

[0079] As detected by HPLC, the content of captan was 97.50%, and the yield was 95.01%; very little trichlorothiochloromethane was detec...

Embodiment 3

[0081] (1) According to phthalic anhydride, NH 3 The mol ratio of NaOH, trichlorothiochloromethane is 1: 1.1: 1.1: 0.97 to get each raw material; Drop into 15Kg phthalic anhydride (99.5%) and 7.54Kg ammoniacal liquor (content 25%) in the primary reactor, enter after staying 6min Secondary reactor; Add 13.87Kg sodium hydroxide solution (content 32%) in secondary reactor again, enter tertiary reactor after staying 10min; Add 18.38Kg trichlorothiochloromethane ( 99%), under high-shear stirring at 3000r / min, react at -5°C to 0°C for 32min (in turn, stay in the third-stage reactor for 8min, the fourth-stage reactor for 15min and the fifth-stage reactor for 9min), get the reaction product;

[0082] (2) After the reaction product obtained in step (1) was filtered, it was dried at 105° C. to 115° C. for 20 minutes to obtain 29.53 Kg of the original captan.

[0083] As detected by HPLC, the content of captan was 97.56%, and the yield was 95.08%; very little trichlorothiochloromethane...

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Abstract

The invention relates to a device for preparing captan. The device comprises a first mixing device, a second mixing device, a first reaction device, a second reaction device, a third reaction device,a filtration device and a drying device; the first mixing device is provided with a phthalic anhydride inlet and an ammonia water inlet; a feed inlet of the second mixing device is connected with a discharge hole of the first mixing device, and the second mixing device is provided with a sodium hydroxide inlet; a feed inlet of the first reaction device is connected with a discharge hole of the second mixing device, and the first reaction device is provided with a trichloromethyl sulfochloride inlet; a feed inlet of the second reaction device is connected with a discharge hole of the first reaction device; a feed inlet of the third reaction device is connected with a discharge hole of the second reaction device; a feed inlet of the filtration device is connected with a discharge hole of thethird reaction device; an inlet of the drying device is connected with a discharge hole of the filtration device. When the device is adopted by preparing the captan, intermediate purification is notneeded, a product high in content and yield can be obtained directly, the technology is simple, the reaction retention time is short, and continuous production can be achieved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and more specifically relates to a device and method for preparing 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, 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 structural formula is shown in formula (I): [0003] [0004] The usual synthesis route of captan is: phthalic anhydride (phthalic anhydride) is used as the starting material, and phthal...

Claims

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Application Information

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IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 孙国庆迟志龙李涛高技峰张学举
Owner NINGXIA G R FINE CHEM CO LTD
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