Method for preparing glycol sulfite
A technology of ethylene sulfite and dimethyl sulfite, which is applied in the field of preparation of ethylene sulfite, can solve the problems of high chlorohydrin content, long reaction time, poor safety, etc., and achieve high product purity, The effect of high reaction yield and stable reaction
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Embodiment 1
[0014] Add 1100g (10mol) dimethyl sulfite, 620g (10mol) ethylene glycol, and 8.6g p-toluenesulfonic acid to a 2000ml three-neck flask equipped with a stirrer, a fractionating column, and a thermometer, and heat to 70°C to start the reaction , through the method of fractional distillation, the methanol generated by the reaction is continuously removed. During the reaction, the temperature of the reaction is gradually increased. When the temperature of the reaction system reaches above 170°C and no methanol is distilled out, it indicates that the reaction has been carried out. completely. Finally, fractionate and purify the obtained product, and extract the fraction at 172-173°C, which is the product ethylene sulfite. Yield 970 g, purity 99% (HPLC).
Embodiment 2
[0016] In a 2000ml three-neck flask equipped with a stirrer, a fractionation device, and a thermometer, add 1100 (10mol) dimethyl sulfite, 682g (11mol) ethylene glycol, and 7.5g p-toluenesulfonic acid, and heat the reaction system to 70°C Start the reaction, and continuously remove the methanol generated by the reaction by means of fractional distillation. During the reaction, gradually increase the reaction temperature. When the temperature of the reaction system reaches above 170°C and no methanol is distilled out, it indicates that the reaction Completed. Finally, fractionate and purify the obtained product, and extract the fraction at 172-173°C, which is the product ethylene sulfite. Yield 965 g, purity 99% (HPLC).
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