A kind of preparation method of high-purity difluorosulfonimide
A technology of difluorosulfonimide and crude difluorosulfonimide is applied in the field of preparation of high-purity difluorosulfonimide, and can solve the residual problem of dichlorosulfonimide-fluoro-chlorosulfonimide , It is difficult to control the chloride ion impurity content and increase the complexity of the salt-forming process, so as to achieve the effects of short treatment process, significant separation effect and simple design
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[0019] The present invention is further described below in conjunction with specific embodiment:
[0020] A preparation method of high-purity difluorosulfonimide, the method comprises the following steps:
[0021] The first step is to add a protic solvent equivalent to 0.1% to 10% of the mass of the crude difluorosulfonimide to the crude product of difluorosulfonimide, and react at 10°C to 120°C for 10min to 10h. During the heat preservation process Slowly introduce HF gas equivalent to 0-10% of the mass of the crude product of difluorosulfonimide.
[0022] In the second step, the difluorosulfonimide obtained in the first step is distilled to obtain a high-purity difluorosulfonimide with a chloride ion content below 20 ppm. In the second step, the distillation is vacuum distillation. According to the present invention, the difluorosulfonimide after the above-mentioned impurity removal process is subjected to vacuum distillation, and the fraction at about 100°C / 15mmHg is coll...
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