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METHOD FOR PREPARING LITHIUM FLUOROSULFATE USING ORGANIC METAL LITHIUM REAGENT

机译:使用有机金属锂试剂制备氟硫酸锂的方法

摘要

Disclosed in the present invention is a method for preparing lithium fluorosulfate using an organic metal lithium reagent, comprising the following steps: (1) using an organic metal lithium reagent as a lithium source, and at a low temperature with perfluorohexane as a solvent, slowly mixing with fluorosulfuric acid and reacting to obtain a lithium fluorosulfate crude product. The crude product is washed five times using the reaction solvent. (2) Performing decompression and draining on the crude product, and then adding the product into a poor organic solvent of lithium fluorosulfate and washing three times, and then vacuum drying the poor organic solvent to obtain a solid. (3) Adding carbonate-ester, -nitrile, and -alcohol organic solvents to the solid for extraction, filtration, and concentration, and adding a low-polarity aprotic solvent to the concentrated solution for static crystallization. (4) Crystal re-filtration, and vacuum drying to obtain a lithium fluorosulfate product. In the above preparation steps, anhydrous operations are performed under the protection of an inert gas. The preparation method provided in the present invention can be used to prepare lithium fluorosulfate and features high yield and stable product quality, and can further effectively reduce the content of such impurities as potassium ions, sodium ions, calcium ions, fluorine ions, sulphate radical ions, and water in the product.
机译:本发明公开了一种用于使用有机金属锂试剂制备氟硫酸锂的方法,包括以下步骤:(1)使用有机金属锂试剂作为锂源,并用全氟己烷作为溶剂,慢慢地与氟硫酸和反应混合,得到氟硫酸锂粗产物。使用反应溶剂洗涤粗产物五次。 (2)在粗产物上进行减压和排出,然后将产物加入氟磺酸锂的差的有机溶剂中并洗涤三次,然后真空干燥差的有机溶剂以获得固体。 (3)将碳酸酯 - 酯, - 腈和 - 醇有机溶剂加入固体中,用于提取,过滤和浓缩,并向浓缩溶液中添加低极性非质子溶剂以进行静态结晶。 (4)晶体再过滤,真空干燥,得到氟硫酸锂产物。在上述制备步骤中,在惰性气体的保护下进行无水操作。本发明提供的制备方法可用于制备氟磺酸锂,具有高产率和稳定的产品质量,可以进一步有效地降低钾离子,钠离子,钙离子,氟离子,硫酸盐根茎离子等杂质的含量和产品中的水。

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