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Solvent process for synthesizing cartap

The technology of the salicylate and the solvent method is applied in the field of preparation of salicylate, which can solve the problems of low operability, poor quality, serious three wastes, etc., and achieves the effects of stable quality, good quality and easy control.

Inactive Publication Date: 2008-11-12
JIANGSU TIANRONG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Cartap is an insecticide derived from nereistoxin, which is more efficient and has a wider spectrum than the previous domestically produced pesticides such as dimehypo, monosultap, and cyclosultap. In the early 1980s, some people tried to In my country's current situation, using the existing equipment and technology of insecticide manufacturers, dimehypo is used as raw material to produce cartap through cyanidation and hydrolysis reactions, but due to the complex composition and many impurities of dimehypo, resulting in cyanidation The reaction yield is high, the quality is poor, and the project investment is large, the operation is complicated, the three wastes are serious, and it is impossible to carry out large-scale industrial production
In the 1990s, some people used aromatic hydrocarbons as solvents and monosultap as raw materials to produce cartap through cyanidation and hydrolysis reactions. Some breakthroughs were made, and industrial production was initially realized. However, due to the use of aromatic hydrocarbon solvents, cyanidation, The hydrolysis reaction is difficult to control, the operational flexibility is small, and it is difficult to achieve stable production yield. In addition, due to the unreasonable recovery process of aromatic solvents, there are more three wastes, difficult treatment and high cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 760kg (2.05kmol) of 95% monosultap is made into an alkaline aqueous solution of 22% by weight, 780kg (4.78kmol) of 30% sodium cyanide solution, in the presence of 1875kg (18.75kmol) of 99% dichloroethane solvent , react at 5-8°C for more than 1 hour, statically separate layers, the lower layer is thiocyanide dichloroethane solution, add 250kg of washed and recovered dichloroethane upper layer water, add 250kg of methanol, and feed 9.58kmol hydrogen chloride gas Reaction, the temperature is controlled at -5~5°C, and the reaction time of hydrogen chloride is 14~22 hours. After the end, dichloroethane is recovered under the condition of negative pressure -0.02~-0.06Mpa, and the crude product is recrystallized and refined by adding 700kg of water, and then purified by Cooling and crystallization, centrifugation, and drying analysis gave 515kg of product, and its content was 98% (1.85kmol) through high performance liquid phase detection.

[0026] The recovered dichloroethane...

Embodiment 2

[0028] 760kg (2.05kmol) of 95% monosultap is made into an alkaline aqueous solution of 22% by weight, 836kg (5.12kmol) of 30% sodium cyanide solution, in the presence of 2278kg (22.78kmol) of 99% dichloroethane solvent , react at 7-10°C for more than 1 hour, statically separate layers, the lower layer is thiocyanide dichloroethane solution, add 300kg of washed and recovered dichloroethane upper layer water, add 304kg of methanol, and pass in 11.18kmol hydrogen chloride gas , control the temperature at 5-15°C, and pass the reaction time of hydrogen chloride for 14-22 hours. After the end, recover dichloroethane under the condition of negative pressure -0.02-0.06Mpa, add 700kg of water to the crude product for recrystallization and refinement, and then crystallize by cooling , centrifugation, and drying analysis to obtain 516kg of product, and its content is 98% (1.85kmol) through high performance liquid phase detection.

[0029] The recovered dichloroethane is washed with 220kg...

Embodiment 3

[0031] 95% monosultap 760kg (2.05kmol) is made into the alkaline aqueous solution of weight content 22%, 30% sodium cyanide solution 780kg (4.78kmol), in the presence of 99% trichloromethane solvent 2240kg (18.56kmol), React at 5-8°C for more than 1 hour, static volume layering, the lower layer is thiocyanide trichloromethane solution, add 250kg of washing and recovery chloroform stratification water, add 228kg of methanol, and feed 7.28kmol hydrogen chloride gas to control The temperature is -15~25°C, and the reaction time of hydrogen chloride is 12~18 hours. After the completion, the chloroform is recovered under the condition of negative pressure -0.02~-0.06Mpa, and the crude product is recrystallized and refined by adding 700kg of water, and then crystallized by cooling and centrifuged. , drying and analyzing to obtain 507kg of product, and its content is 98% (1.815kmol) through high performance liquid phase detection.

[0032] The recovered chloroform is washed with 200kg...

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PUM

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Abstract

The present invention discloses a solvent process for synthesizing cartap, comprising that a monosultap alkaline aqueous solution and sodium cyanide undergo a cyanation reaction in a halohydrocarbon solvent and at a temperature of between 20 DEG C below zero and 80 DEG C to give an intermediate thiocyanide solution; and then, the intermediate thiocyanide solution together with methanol and hydrochloric acid gas undergoes a hydrolysis reaction at a temperature of between 50 DEG C below zero and 100 DEG C, for 2 to 30 hours, to give a crude product of the cartap. The method solves the problems in the production of complex process, serious three wastes, instable product yield and instable quality, etc. The method can be suitable for large-scale industrialized and commercialized production.

Description

technical field [0001] The invention belongs to the field of pesticides, in particular to a preparation method of cartap. Background technique [0002] Cartap is an insecticide derived from nereistoxin, which is more efficient and has a wider spectrum than the previous domestically produced pesticides such as dimehypo, monosultap, and cyclosultap. In the early 1980s, some people tried to In my country's current situation, using the existing equipment and technology of insecticide manufacturers, dimehypo is used as raw material to produce cartap through cyanidation and hydrolysis reactions, but due to the complex composition and many impurities of dimehypo, resulting in cyanidation The reaction yield is high, the quality is poor, and the project investment is large, the operation is complicated, the three wastes are serious, and it cannot be industrialized on a large scale. In the 1990s, some people used aromatic hydrocarbons as solvents and monosultap as raw materials to prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/04
Inventor 许网保魏明阳周国平王良虞国新毛建新
Owner JIANGSU TIANRONG GROUP
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