The synthetic method of dichlorosulfonimide salt
A technology of bischlorosulfonimide salt and bischlorosulfonimide, applied in the field of preparation of intermediate bischlorosulfonimide alkali metal salt, can solve the problem of low product purity, low yield, difficult application, etc. problem, to achieve the effect of high purity and yield, low water content, and simple and easy preparation process
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Embodiment 1
[0017] Embodiment 1: Potassium dichlorosulfonimide (KN(SO 2 Cl) 2 , referred to as KCSI).
[0018] Under the conditions of nitrogen protection and circulating water bath, 428 grams (2mol) of dichlorosulfonimide was slowly added dropwise in the vigorously stirred 900g dimethyl carbonate (10mol) solvent, and a circulating water bath at 5°C was selected to control the dilution temperature as 12°C.
[0019] Then, dry 152g (2.04mol) of potassium chloride (moisture content: 58ppm) was added to the above solution at room temperature, slowly heated to 125°C under stirring condition, and reacted for 4 hours.
[0020] After the reaction, the reaction solution was filtered to obtain 1400 g of the reaction solution, which was then concentrated to 840 g at 95° C.
[0021] The above concentrated solution was cooled to 5°C for crystallization, filtered and dried under vacuum at 100°C for 12 hours to obtain 451 g of anhydrous potassium bischlorosulfonimide with a yield of 88.9% and a water...
Embodiment 2
[0022] Embodiment 2: Sodium dichlorosulfonimide (NaN(SO 2 Cl) 2 , referred to as NaCSI).
[0023] Under the conditions of nitrogen protection and circulating water bath, 428g (2mol) of bischlorosulfonimide was slowly added dropwise into the vigorously stirred 900g dimethyl carbonate (10mol) solvent, and a circulating water bath at 8°C was selected to control the dilution temperature at 12 ℃.
[0024] Then, 120 g (2.04 mol) of dry sodium chloride (moisture content: 64 ppm) was added to the above solution at room temperature, slowly heated to 125° C. under stirring condition, and reacted for 4 hours.
[0025] After the reaction, the reaction solution was filtered to obtain 1380 g of the reaction solution, which was then concentrated to 830 g at 95° C.
[0026] The above concentrated solution was cooled to 5°C for crystallization, filtered and then vacuum-dried at 100°C for 12 hours to obtain 401 g of anhydrous sodium bischlorosulfonimide with a yield of 84.4% and a water cont...
Embodiment 3
[0027] Embodiment 3: Lithium dichlorosulfonimide (LiN(SO 2 Cl) 2 , referred to as LiCSI) preparation.
[0028] Under the conditions of nitrogen protection and circulating water bath, 428g (2mol) of bischlorosulfonimide was slowly added dropwise into 900g of dimethyl carbonate (10mol) solvent which was stirred vigorously, and a circulating water bath at 2°C was selected to control the dilution temperature to 5 ℃.
[0029] Then, dry 86.5g (2.04mol) lithium chloride (moisture content: 57ppm) was added to the above solution at room temperature, slowly heated to 125°C under stirring condition, and reacted for 4 hours.
[0030] After the reaction, the reaction solution was filtered to obtain 1420 g of the reaction solution, which was then concentrated to 860 g at 95° C.
[0031] The above concentrated solution was cooled to 5°C for crystallization, filtered and dried under vacuum at 100°C for 12 hours to obtain 378g of anhydrous lithium bischlorosulfonyl imide with a yield of 85....
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