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.
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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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