A kind of method of processing o-sulfonamidobenzoic acid methyl ester crystallization mother liquor
A technology of methyl benzoate and crystallization mother liquor, which is applied in the direction of organic chemistry, can solve the problems that methyl o-sulfonamide benzoate cannot be recovered, increases the cost of sewage treatment, and is difficult to pass, so as to achieve environmental protection and reduce sewage Disposal cost, organic matter reduction effect
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Embodiment 1
[0021] 3000kg from the production of methyl o-sulfonamide benzoate concentration, the crystallization mother liquor of the intermediate methyl o-sulfonamide benzoate produced in the crystallization process is vacuum pumped into the enamel distillation still of 5000L volume, and 30% sodium hydroxide solution (liquid caustic soda) is added ) to pH = 9, then heated to above 64°C, distilled methanol, stopped heating and distillation when the temperature of the kettle reached 90°C, opened the reactor jacket and circulated water to cool down to 25°C, added water to adjust the Baume degree to 8Be, filtered, Add 30% sulfuric acid to the filtrate until pH = 1, and a white powdery solid is precipitated. After qualitative analysis, the white powdery solid is insoluble saccharin. 211kg of insoluble saccharin is separated by drying, and the waste liquid flows into the sewage treatment station for treatment. After testing, the content of insoluble saccharin after drying (on a dry basis) is ...
Embodiment 2
[0023] With 300g from the intermediate methyl o-sulfonamidobenzoate crystallization mother liquor produced in the process of producing methyl o-sulfonamide benzoate crystallization refining process, vacuum into the glass still of 1000ml capacity, add potassium hydroxide to pH=9, then Heat to above 64°C, distill methanol, stop heating and distillation when the kettle temperature reaches 90°C, cool down to 23°C in a cold water bath, filter out calcium sulfate, add water to the filtrate to adjust the Baume degree to 7Be, then add 30% hydrochloric acid to When pH=1, a white powdery solid is precipitated, and the qualitative analysis shows that the white powdery solid is insoluble saccharin. Dry and separate 20.5 g of insoluble saccharin, and discard the waste liquid. After testing, the content of insoluble saccharin after drying (on a dry basis) is 98.19%.
Embodiment 3
[0025] 300g of the intermediate methyl o-sulfonamide benzoate crystallization mother liquor produced during the concentration and crystallization process from the production of methyl o-sulfonamide benzoate is vacuum pumped into a glass still with a volume of 1000ml, calcium hydroxide is added to pH=9, and then Heat to above 64°C, distill methanol, stop heating and distillation when the temperature of the kettle reaches 90°C, cool down to 24°C in a cold water bath, add water to adjust Baume to 6Be, filter, add 30% hydrochloric acid to the filtrate until pH = 1, A white powdery solid was precipitated, which was found to be insoluble saccharin through qualitative analysis. Dry and separate 20.3 g of insoluble saccharin, and discard the waste liquid. After testing, the content of insoluble saccharin after drying (on a dry basis)) is 98.06%.
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