A kind of preparation method of cyclic sulfuric acid ester
A technology of cyclic sulfate and oil, which is applied in the field of preparation of cyclic sulfate, can solve the problems of excessive waste water, high cost, and low yield, and achieve the effect of less waste water, low cost, and high yield
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[0020] The invention provides a kind of preparation method of cyclic sulfuric acid ester, comprising:
[0021] A) under the condition of inert gas protection, reaction gas is reacted with dioxane to obtain oil; said reaction gas is sulfur trioxide or sulfur dioxide;
[0022] B) Sublimation or distillation of the oil to obtain cyclic sulfuric acid ester.
[0023] The invention provides a preparation method of cyclic sulfuric acid ester.
[0024] The cyclic sulfuric acid ester described in the present invention is vinyl sulfite and vinyl sulfate. Vinyl sulfite and vinyl sulfate are well known to those skilled in the art.
[0025] The preparation method of the cyclic sulfuric acid ester provided by the invention firstly reacts the reaction gas with dioxane under the protection condition of an inert gas to obtain an oily substance.
[0026] Preferably, the dioxane is heated under the protection of an inert gas, and the reaction gas is mixed with the dioxane at a certain speed t...
Embodiment 1
[0062] Build a magnetic stirrer and a thermometer into a 1000ml three-necked bottle, replace the air in the bottle with nitrogen, put 650.0g of anhydrous dioxane under the protection of nitrogen, and heat the oil bath to 95°C;
[0063] Fully mix dry nitrogen and sulfur trioxide gas through a glass filler, adjust the flow rate so that the volume ratio is 1:1, the total flow rate is 3.7ml / min, the solution gradually changes from colorless to light yellow, after about 30 minutes, the consumption Sulfur trioxide 99.5g, continue to react for 5min;
[0064] Naturally stirred and cooled to room temperature, concentrated under reduced pressure to recover 532.4 g of dioxane to obtain 198.0 g of light yellow oil;
[0065] Transfer 198.0g of light yellow oil to a sublimator, keep a vacuum of 3mbar, gradually heat up the oil bath to 70°C, and sublimate to obtain 117.5g of white needle-like solid vinyl sulfate, with a purity of 99.64% and a yield of 76.17%.
[0066] Carry out GC identific...
Embodiment 2
[0068] Build a magnetic stirrer and a thermometer into a 1000ml three-necked bottle, replace the air in the bottle with nitrogen, put 610.0g of anhydrous dioxane under the protection of nitrogen, and heat the oil bath to 95°C;
[0069] Fully mix dry nitrogen and sulfur dioxide gas through the glass packing, adjust the flow rate to make the volume ratio 1:0.8, the total flow rate is 4.5ml / min, the solution gradually turns colorless to light yellow, after about 30 minutes, the consumption of sulfur dioxide is 86.0 g, continue to react for 5 minutes;
[0070] Naturally stirred to cool down to room temperature, and concentrated under reduced pressure to recover 496.0 g of dioxane to obtain 182.1 g of light yellow oil;
[0071] Transfer 182.1g of light yellow oil to a three-neck flask, keep a vacuum of 7mbar, raise the temperature of the oil bath to 45°C, collect 10.3g of the previous fraction, raise the temperature of the oil bath to 65°C, and distill to obtain 105.8g of vinyl sul...
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