Sulfur-based unsaturated heterochain boron trifluoride salt electrolyte as well as preparation method and application thereof
A boron trifluoride, unsaturated technology, applied in the field of sulfur-based unsaturated heterochain boron trifluoride salt electrolyte and its preparation, can solve problems such as uncertainty of correlation or inference, and achieve improved electrochemical performance , broaden the electrochemical window and improve the effect of cycle performance
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Embodiment 1
[0069] Example 1: Raw materials
[0070] Preparation method: under nitrogen atmosphere, mix 0.01 mol of raw material and boron trifluoride tetrahydrofuran complex (2.8 g, 0.02 mol) in 15 ml of ethylene glycol dimethyl ether, and react at room temperature for 12 hours. The obtained mixed solution was dried under reduced pressure under the conditions of 40° C. and a vacuum degree of about -0.1 MPa to remove the solvent to obtain an intermediate. Lithium ethoxide (1.04g, 0.02mol) was dissolved in 10ml of ethanol and slowly added to the intermediate, stirred at 45°C for 8 hours, and the resulting mixture was dried under reduced pressure at 40°C and a vacuum of about -0.1MPa. , the obtained solid was washed three times with n-butyl ether, filtered and dried to obtain product M1, and Q was -S-BF 3 Li. The yield was 80%, NMR as figure 1 shown.
Embodiment 2
[0071] Example 2: Raw materials
[0072] Preparation method: under argon atmosphere, metal lithium sheet (0.14g, 0.02mol) was slowly added to 0.01mol of raw material, reacted at room temperature for 3 hours, then heated to 50°C until the reaction of lithium sheet was complete to obtain an intermediate. Boron trifluoride butyl ether complex (3.96g, 0.02mol) and 10ml THF were added to the intermediate, and the reaction was stirred at room temperature for 10 hours. Drying under reduced pressure, the obtained solid was washed three times with isopropyl ether, filtered and dried to obtain product M2, Q is -S-BF 3 Li. The yield was 81%, NMR as figure 2 shown.
Embodiment 3
[0073] Example 3: Raw materials
[0074] Preparation method: under argon atmosphere, mix 0.01 mol of raw material and boron trifluoride ether complex (2.98 g, 0.021 mol) in 15 ml of THF, and react at room temperature for 12 hours. The obtained mixed solution was dried under reduced pressure under the conditions of 30° C. and a vacuum degree of about -0.1 MPa to remove the solvent to obtain an intermediate. 14ml of butyllithium in hexane solution (c=1.6mol / L) was added to the intermediate, and the reaction was stirred at room temperature for 6 hours. The obtained mixed solution was dried under reduced pressure at 30°C and a vacuum degree of about -0.1MPa. The obtained crude product was washed 3 times with cyclohexane, filtered and dried to obtain the product M3, and Q was -S-BF 3 Li. The yield was 83%, NMR as image 3 shown.
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