Preparation method of ethyl methyl carbonate solution containing ethylene sulfate
A technology of ethyl methyl carbonate and vinyl sulfate, which is applied in the field of improving the preparation method of ethyl methyl carbonate solution, can solve problems such as unfavorable occupational health and hygiene, environmental dust pollution, inconvenient operation, etc., and achieves benefits for occupational health and hygiene, The process route is simple and controllable, solving the effect of low packaging efficiency
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Embodiment 1
[0021] This embodiment adopts the following preparation method: add 50 grams of vinyl sulfite, 300 grams of ethyl methyl carbonate and 0.6 grams of 5% ruthenium trichloride aqueous solution into a three-necked flask, stir evenly with a magnet in a 0-degree low-temperature bath, and drop Add the calcium hypochlorite aqueous solution of 242 grams 15% available chlorine content, control reaction system temperature in the dropwise addition process and be less than 5 degree, continue low-temperature stirring reaction 2 hours after dropwise addition finishes. Stand still to separate the liquids, and then wash the organic phase with 200 grams of pure water for 4 times, the temperature of the washing process is controlled at 2-8 degrees, and the obtained organic phase is first dried with anhydrous sodium sulfite, and then dried with molecular sieves to obtain 327 grams of 13.5% Ethyl methyl carbonate solution of mass concentration vinyl sulfate, detection moisture 5ppm, free acid 8ppm....
Embodiment 2
[0023] This embodiment adopts the following preparation method: add 50 grams of vinyl sulfite, 250 grams of ethyl methyl carbonate and 0.5 grams of 5% ruthenium trichloride aqueous solution into a three-necked flask, stir evenly with a magnet in a 0-degree low-temperature bath, and drop Add the sodium hypochlorite aqueous solution of 280 grams 13% available chlorine content, control reaction system temperature in the dropwise addition process and be less than 5 degree, continue low-temperature stirring reaction 2 hours after dropwise addition finishes. Stand to separate the liquids, and wash the organic phase with 150 grams of pure water for 5 times, the temperature of the washing process is controlled at 2-8 degrees, and the obtained organic phase is first dried with anhydrous magnesium sulfite, and then dried with molecular sieves to obtain 260 grams of 15.4% mass concentration vinyl sulfate ethyl methyl carbonate solution, detected moisture 6ppm, free acid 7ppm.
Embodiment 3
[0025] This embodiment adopts the following preparation method: add 50 grams of vinyl sulfite, 400 grams of ethyl methyl carbonate and 1 gram of 5% ruthenium trichloride aqueous solution into a three-necked flask, stir evenly with a magnet in a 0-degree low-temperature bath, and drop Add the potassium hypochlorite aqueous solution of 400 grams 9% available chlorine content, control reaction system temperature during dropwise addition and be less than 5 degree, continue low-temperature stirring reaction 2 hours after dropwise addition finishes. Stand to separate the liquids, and wash the organic phase with 300 grams of pure water for 3 times, the temperature of the washing process is controlled at 2-8 degrees, and the obtained organic phase is first dried with anhydrous calcium chloride, and then dried with molecular sieves to obtain 385 grams of 12.3% mass concentration of ethyl methyl carbonate solution of vinyl sulfate, detected moisture 5ppm, free acid 8ppm.
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