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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

In the present invention, (a) bis(chlorosulfonyl)imide and NH 4 F(HF)n (n=0~10) in a nitrogen atmosphere are diethyl ether, diisopropyl ether, methyl-t-butyl ether, acetic acid. Preparing ammonium bis(fluorosulfonyl)imide by reacting in one or more solvents selected from the group consisting of methyl, ethyl acetate, 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, It provides a method for producing a bis(fluorosulfonyl)imide lithium salt, characterized in that the pH of the gas carried in step (b) is measured using a pH paper.
机译:在本发明中,(a)在氮气氛中的双(氯磺酰基)酰亚胺和NH 4 F(HF)n(n = 0〜10)是二乙醚,二异丙醚,甲基叔丁基。丁基醚,乙酸。通过在一种或多种选自甲基,乙酸乙酯,乙酸丙酯和乙酸丁酯的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;本发明提供一种双(氟磺酰基)酰亚胺锂盐的制造方法,其特征在于,步骤(b)中携带的气体的pH使用pH试纸进行测定。

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