Liquid phase circulation method in synthesis of thionyl chloride
A technology of thionyl chloride and liquid phase circulation, applied in the direction of sulfur and halogen compounds, etc., can solve the problems of complex process, large investment, and difficulty in obtaining high purity.
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Embodiment 1
[0091] A method for liquid phase circulation in the synthesis of thionyl chloride, comprising:
[0092] (1) The crude product sulfur oxychloride whose content of sulfur oxychloride accounts for 68% of the crude product sulfur oxychloride total amount is vulcanized in a vulcanization kettle, and also contains 15% sulfur dichloride in the crude product sulfur oxychloride , the temperature in the vulcanization kettle is that the residual temperature of the crude product thionyl chloride is 80° C., and the pressure is normal pressure. In the crude product thionyl chloride, add sulfur that is not excessive relative to the sulfur dichloride therein, and the addition of sulfur The amount is 80% of the amount of sulfur required for the complete reaction with the sulfur dichloride in the crude product thionyl chloride to obtain the sulfided crude product thionyl chloride; its components are: the content of thionyl chloride is 50% , the sulfur dichloride content is 15%, and the sulfur m...
Embodiment 2
[0103] (1) The crude product sulfur oxychloride whose content of sulfur oxychloride accounts for 65% of the crude product sulfur oxychloride is vulcanized in a vulcanization kettle, and the crude product sulfur oxychloride also contains 20% of sulfur dichloride , the temperature in the vulcanization kettle is that the residual temperature of the crude product thionyl chloride is 60° C., and the pressure is normal pressure. In the crude product thionyl chloride, sulfur that is not excessive relative to the sulfur dichloride therein is added, and the addition of sulfur The amount is 88% of the amount of sulfur required for the complete reaction of sulfur dichloride in the crude product thionyl chloride, so that other substances in the crude product thionyl chloride are converted into sulfur monochloride except thionyl chloride, Obtain the crude product thionyl chloride after sulfidation, in the crude product thionyl chloride after described sulfidation, its each component is: the...
Embodiment 3
[0113] A method for liquid phase circulation in the synthesis of thionyl chloride, comprising:
[0114] (1) Vulcanize the crude product sulfur oxychloride whose content of sulfur oxychloride accounts for 68% of the crude product sulfur oxychloride total amount in a vulcanization kettle, and also contain 25% of sulfur dichloride in the crude product sulfur oxychloride , the temperature in the vulcanization kettle is that the residual temperature of the crude product thionyl chloride is 70° C., and the pressure is normal pressure. To the crude product thionyl chloride, add sulfur that is not excessive relative to the sulfur dichloride therein, and the addition of sulfur The amount is 98% of the amount of sulfur required for the complete reaction of sulfur dichloride in the crude product thionyl chloride, and other substances in the crude product thionyl chloride except thionyl chloride are converted into sulfur monochloride to obtain The crude product sulfur oxychloride after vu...
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