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LiFSI Method for producing bis fluorosulfonyl imide lithium salt LiFSI with reduced fluorine anion content

机译:LiFSI生产氟阴离子含量降低的双氟磺酰亚胺酰亚胺锂盐LiFSI的方法

摘要

The present invention (a) Bis(chlorosulfonyl)imide and NH 4 F(HF)n (n=0~10) under nitrogen atmosphere, diethyl ether, diisopropyl ether, methyl-t-butyl ether, methyl acetate, acetic acid Preparing ammonium bis(fluorosulfonyl)imide by reacting in at least one solvent selected from the group consisting of ethyl, propyl acetate, and butyl acetate; (b) After the reaction in step (a) is terminated, the reaction product is cooled to 50 to 70°C, and then nitrogen gas is supplied to the reaction solution and bubbling is performed until the pH of the flying gas is 6 to 8. Step to do; (c) reacting the ammonium bis(fluorosulfonyl)imide obtained in step (b) with a lithium base to prepare a bis(fluorosulfonyl)imide lithium sa (d) introducing the bis(fluorosulfonyl)imide lithium salt and antisolvent prepared in step (c) into a reactor; (e) adding lithium methoxide or lithium methoxide solution to the reactor and stirring; And (f) filtering the solution stirred in step (e) and drying the filtrate; including, The pH of the gas flying in the step (b) is measured using a pH paper, After mixing the reactants in step (c), a process of bubbling until the pH of the flown gas is 6-8 by supplying nitrogen gas to the reaction solution is further performed. It provides a method for producing a sulfonyl)imide lithium salt.
机译:(a)双(氯磺酰基)酰亚胺和NH 4 F(HF)n(n = 0〜10),在氮气氛下,乙醚,二异丙醚,甲基叔丁基醚,乙酸甲酯,乙酸通过在选自乙基,乙酸丙酯和乙酸丁酯中的至少一种溶剂中反应来制备双(氟磺酰基)酰亚胺铵; (b)在步骤(a)中的反应终止后,将反应产物冷却至50至70℃,然后将氮气供应至反应溶液中并进行鼓泡直至飞行气体的pH为6至6。 8.一步做; (c)使步骤(b)中得到的双(氟磺酰基)酰亚胺铵与锂碱反应,制得双(氟磺酰基)酰亚胺锂盐。 (d)将步骤(c)中制备的双(氟磺酰基)酰亚胺锂盐和抗溶剂引入反应器中; (e)向反应器中加入甲醇锂或甲醇锂溶液并搅拌; (f)过滤在步骤(e)中搅拌的溶液并干燥滤液;包括,使用pH试纸测量步骤(b)中飞行的气体的pH,将步骤(c)中的反应物混合后,通过通入氮气鼓泡直至气体的pH为6-8。将反应溶液进一步进行。它提供了一种生产磺酰基)酰亚胺锂盐的方法。

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