A kind of preparation method of lithium bisfluorosulfonyl imide
A technology of lithium bisfluorosulfonyl imide and bischlorosulfonimide, which is applied in the field of preparation of lithium bisfluorosulfonyl imide, can solve the problem of low purity of lithium bisfluorosulfonyl imide, many types and contents of impurities, There are many types of raw materials and reagents, etc., to achieve good fluorination effect, good economic and environmental benefits, and the effect of improving purity
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Embodiment 1
[0058] The preparation method of the bisfluorosulfonyl imide lithium of the present embodiment, such as figure 1 shown, including the following steps:
[0059] 1) Preparation of bischlorosulfonimide:
[0060] a) Under nitrogen protection, according to the ratio of 2.0:1.0:1.0 in the molar ratio of thionyl chloride, sulfamic acid and chlorosulfonic acid, 250g (100%, folded) of thionyl chloride and 102g (100%, 100% sulfamic acid was added to the reactor, and after stirring at room temperature, 123g (100%, 100%) chlorosulfonic acid was added at a constant speed, and the addition time was controlled to be 5h;
[0061] After the addition of chlorosulfonic acid, continue to stir and react at room temperature for 1 hour, then open the outlet valve of the reactor, discharge and recover the unreacted thionyl chloride and protective atmosphere in the reactor; the remaining liquid in the reactor is mixed liquid A;
[0062] b) After the pressure in the reactor is stable, the liquid in t...
Embodiment 2
[0071] The preparation method of the lithium bisfluorosulfonyl imide of the present embodiment (the process flow diagram is the same as that of Example 1), comprises the following steps:
[0072] 1) Preparation of bischlorosulfonimide:
[0073] a) Under nitrogen protection, according to the ratio of 2.5:1.0:1.0 in the molar ratio of thionyl chloride, sulfamic acid and chlorosulfonic acid, 250g (100%, folded) thionyl chloride and 81.5g (100% , 100 percent) sulfamic acid was added to the reactor, and after stirring at room temperature, 98 g (100 percent, 100 percent) chlorosulfonic acid was added at a constant speed, and the addition time was controlled to be 5 hours;
[0074] After the addition of chlorosulfonic acid, continue to stir and react at room temperature for 0.5h, then open the outlet valve of the reactor to discharge and recover the unreacted thionyl chloride and protective atmosphere in the reactor; the remaining liquid in the reactor is mixed liquid A ;
[0075] b)...
Embodiment 6
[0088] The preparation method of the bisfluorosulfonyl imide lithium of the present embodiment, such as figure 2 shown, including the following steps:
[0089] 1) Preparation of bischlorosulfonimide:
[0090] a) Under nitrogen protection, according to the ratio of 2.1:1.0:1.0 in the molar ratio of thionyl chloride, sulfamic acid and chlorosulfonic acid, 250g (100%, folded) thionyl chloride and 97.8g (100% , 100% sulfamic acid was added to the reaction kettle, and after stirring at room temperature, 117.6g (100%, 100% percent) chlorosulfonic acid was added at a constant speed, and the addition time was controlled to be 4h;
[0091] After the addition of chlorosulfonic acid, continue to stir and react at room temperature for 0.5h, then open the outlet valve of the reactor to discharge and recover the unreacted thionyl chloride and protective atmosphere in the reactor; the remaining liquid in the reactor is mixed liquid A ;
[0092] b) After the pressure in the reaction kettl...
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