Method for preparing lithium hexafluoroantimonate through alkaline cooperation oxidation
A technology of lithium hexafluoroantimonate and lithium hydroxide, applied in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems of strong corrosiveness, harsh conditions, and high preparation costs, achieve low production costs, and eliminate waste water. Emissions, good product quality
Inactive Publication Date: 2018-07-31
CENT SOUTH UNIV
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This method uses anhydrous hydrofluoric acid as the reaction medium, which is highly corrosive and harsh, and the preparation cost is high
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Embodiment 1
[0037] Sb in the antimony white of the present invention 2 o 3 The mass percentage content is greater than 99.90%, analytical pure lithium hydroxide (LiOH ≥ 99%), analytical pure hydrofluoric acid (HF ≥ 40%), analytical pure hydrogen peroxide (H 2 o 2 ≥30%), the purity of hydrogen sulfide gas is greater than 99.0%.
[0038] Prepare a lithium hydroxide solution with a concentration of 8.0mol / L, add antimony white according to the liquid-solid ratio of solution volume L to antimony white mass kg 8 / 1, raise the temperature to 90°C and continue stirring for 1.0h, then use vacuum pumping The liquid-solid separation is realized by filtration; the temperature of the lithium antimonite solution is raised to 80°C, and then hydrogen peroxide is added with a constant flow pump at a flow rate of 0.20L / min, and the amount of hydrogen peroxide is controlled to be 1.2 times the theoretical amount. After the hydrogen peroxide is completely added, continue Stir the reaction for 1.5h, and th...
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Provided is a method for preparing lithium hexafluoroantimonate through alkaline cooperation oxidation. Antimony oxide is cooperatively dissolved in a high concentration lithium hydroxide aqueous solution, so that antimony is dissolved in the form of lithium niobate, slurry is subjected to solid liquid separation through vacuum filtration, a lithium niobate solution is added with aquae hydrogeniidioxidi to oxide precipitates, and the precipitates are washed to obtain a lithium pyroantimonate presoma; the lithium pyroantimonate is pulpified with water and neutralized with hydrofluoric acid toa desired pH value, the aquae hydrogenii dioxidi is added to the solution, a small amount of trivalent europium remaining in the ithium pyroantimonate is oxidized to pentavalence, the slurry is subjected to solid liquid separation by the vacuum filtration, hydrogen sulfide gas is introduced into the lithium hexafluoroantimonate solution to remove and purify heavy metal impurities, and after purification, the liquid is concentrated, crystallized and dried to obtain a lithium hexafluoroantimonate product. The essence of the method is firstly to utilize the principle of high solubility of the lithium niobate to cooperatively dissolve the antimony in the high concentration lithium hydroxide solution, uses the principle of low solubility of the lithium pyroantimonate to prepare lithium pyroantimonate presoma by adding the aquae hydrogenii dioxidi to conduct oxidation, and finally uses the principle that the length of a Sb-F bond is longer than a Sb-OH bond and the binding force is strong toreplace OH- in the lithium pyroantimonate by F- in an aqueous solution to make the lithium hexafluoroantimonate product. The method has the advantages of short process, good product quality and low cost.
Description
technical field [0001] The invention relates to a preparation method of lithium hexafluoroantimonate, in particular to a method for preparing lithium hexafluoroantimonate through combined oxidation of antimony white in an alkaline system. Background technique [0002] As an advanced new energy device, lithium-ion battery has the advantages of high energy density, high output voltage, large output power, small self-discharge, no memory effect, wide operating temperature range and fast charge and discharge, so it is widely used in Electronic products, vehicles, national defense and aerospace, etc. Among the main components of lithium-ion batteries, the research on electrolyte lithium salts is of great significance to promote the development of lithium batteries (Liu Xu et al. Research progress on lithium-ion battery electrolyte lithium salts. Power Technology, 2016,40(01):218- 220.). [0003] At present, the electrolyte lithium salts mainly used in lithium-ion batteries are ...
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Login to View More IPC IPC(8): C01G30/00
CPCC01G30/003C01P2002/72C01P2004/03C01P2006/80
Inventor 刘伟锋杨天足张杜超陈霖唐攒浪刘好男
Owner CENT SOUTH UNIV