Production process of bis (chlorosulfonyl) imide
A bischlorosulfonimide and production technology technology, applied in the field of bischlorosulfonimide production technology, can solve the problem of lowering the profit margin of the bischlorosulfonimide market, difficulty in large-scale use, and large production of three wastes, etc. problem, to achieve the effect of optimizing the reaction process parameters, improving the utilization rate and shortening the reaction cycle
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Embodiment 1
[0027] Add 97.1g (1mol) of sulfamic acid and 273.7g (2.3mol) of thionyl chloride to the reaction kettle, start stirring, turn on the condenser reflux device, control the temperature at 55°C, set the back pressure valve pressure to 0.4MPa, and wait for the solid After all dissolved, add 80g (1mol) sulfur trioxide into the reaction kettle at a constant speed within 3 hours. After adding sulfur trioxide, raise the temperature to 110°C to continue the reaction for 7.5 hours, return to normal pressure, open the condensate outlet valve of the condenser, Continue the reaction for 2 hours until no condensate flows out of the condenser, start vacuum distillation, collect fractions at 90-105°C, and obtain 212.4 g of the product of the present invention, dichlorosulfonimide liquid, with a reaction yield of 99.1% and a product purity of 99.9 %.
Embodiment 2
[0029] Add 97.1g (1mol) of sulfamic acid and 238g (2.0mol) of thionyl chloride into the reactor, start stirring, turn on the reflux device of the condenser, control the temperature at 40°C, set the pressure of the back pressure valve to 0.1MPa, and wait until the solids are completely After dissolving, add 80g (1mol) sulfur trioxide into the reaction kettle at a constant speed within 1 hour. After adding sulfur trioxide, raise the temperature to 90°C and continue the reaction for 5 hours, return to normal pressure, open the condensate outlet valve of the condenser, and continue the reaction After 1 hour, until no condensate flowed out from the condenser, vacuum distillation was started, and fractions at 90-105°C were collected to obtain 205.5 g of the liquid dichlorosulfonimide product of the present invention, with a reaction yield of 96.0% and a product purity of 99.8%.
Embodiment 3
[0031] Add 97.1g (1mol) of sulfamic acid and 297.5g (2.5mol) of thionyl chloride into the reaction kettle, start stirring, turn on the reflux device of the condenser, control the temperature at 70°C, set the pressure of the back pressure valve to 0.7MPa, and wait for the solid After all dissolved, add 80g (1mol) sulfur trioxide into the reaction kettle at a constant speed within 6 hours. After adding sulfur trioxide, raise the temperature to 120°C to continue the reaction for 10 hours, return to normal pressure, open the condensate outlet valve of the condenser, and continue React for 3 hours, until no condensate flows out from the condenser, start vacuum rectification, collect fractions at 90-105°C, and obtain 211.0 g of dichlorosulfonimide liquid of the present invention, with a reaction yield of 98.5% and a product purity of 99.9% .
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