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Method for preparing battery-grade lithium fluoride and byproduct industrial-grade lithium fluoride from industrial-grade lithium carbonate
The invention discloses a method for preparing battery-grade lithium fluoride from industrial-grade lithium carbonate. The method comprises the following steps: pretreating and crushing the industrial-grade lithium carbonate; pulping, introducing carbon dioxide, carrying out primary hydrogenation reaction, filtering, and carrying out primary hydrogenation to obtain a liquid; adding an organic phosphate type complexing agent, reacting for a certain time, and filtering to obtain a lithium bicarbonate crude solution; dropwise adding a small amount of HF, reacting for a certain time, and filtering to obtain filtrate A; heating the filtrate A for pyrolysis, filtering to obtain a filter cake B, washing the filter cake B, adding water for pulping, introducing carbon dioxide for secondary hydrogenation reaction to obtain a lithium bicarbonate refined solution, dropwise adding HF into the lithium bicarbonate refined solution, filtering to obtain a filter cake C, and washing and drying the filter cake C to obtain the battery-grade lithium fluoride. The invention provides a method for deeply removing impurity ions such as Ca < 2 + > and Mg < 2 + >, and waste liquids in different steps are fully recycled, so that the recycling rate of lithium resources reaches 98% or above, and the quality of obtained battery-grade lithium fluoride is superior to the requirements in the standard HG/T 4507-2013.
本发明公开一种从工业级碳酸锂制备电池级氟化锂的方法,将工业级碳酸锂进行预处理粉碎;打浆并通入二氧化碳进行一次氢化反应,过滤后进行一次氢化液;加入有机磷酸盐型络合剂并反应一定时间后过滤得碳酸氢锂粗液;滴加少量HF并反应一定时间后过滤得滤液A;将滤液A加热进行热解后过滤得滤饼B,滤饼B洗涤后加入水打浆并通入二氧化碳进行二次氢化反应后得碳酸氢锂精制液,向碳酸氢锂精制液中滴加HF后过滤得滤饼C,滤饼C经洗涤、烘干后得电池级氟化锂。本发明提供一种深度除Ca2+、Mg2+等杂质离子的方法,并将不同步骤中的废液充分循环利用,不仅使得锂资源的回收利用率达到98%以上,得到的电池级氟化锂质量优于标准HG/T 4507‑2013中要求。
Method for preparing battery-grade lithium fluoride and byproduct industrial-grade lithium fluoride from industrial-grade lithium carbonate
The invention discloses a method for preparing battery-grade lithium fluoride from industrial-grade lithium carbonate. The method comprises the following steps: pretreating and crushing the industrial-grade lithium carbonate; pulping, introducing carbon dioxide, carrying out primary hydrogenation reaction, filtering, and carrying out primary hydrogenation to obtain a liquid; adding an organic phosphate type complexing agent, reacting for a certain time, and filtering to obtain a lithium bicarbonate crude solution; dropwise adding a small amount of HF, reacting for a certain time, and filtering to obtain filtrate A; heating the filtrate A for pyrolysis, filtering to obtain a filter cake B, washing the filter cake B, adding water for pulping, introducing carbon dioxide for secondary hydrogenation reaction to obtain a lithium bicarbonate refined solution, dropwise adding HF into the lithium bicarbonate refined solution, filtering to obtain a filter cake C, and washing and drying the filter cake C to obtain the battery-grade lithium fluoride. The invention provides a method for deeply removing impurity ions such as Ca < 2 + > and Mg < 2 + >, and waste liquids in different steps are fully recycled, so that the recycling rate of lithium resources reaches 98% or above, and the quality of obtained battery-grade lithium fluoride is superior to the requirements in the standard HG/T 4507-2013.
本发明公开一种从工业级碳酸锂制备电池级氟化锂的方法,将工业级碳酸锂进行预处理粉碎;打浆并通入二氧化碳进行一次氢化反应,过滤后进行一次氢化液;加入有机磷酸盐型络合剂并反应一定时间后过滤得碳酸氢锂粗液;滴加少量HF并反应一定时间后过滤得滤液A;将滤液A加热进行热解后过滤得滤饼B,滤饼B洗涤后加入水打浆并通入二氧化碳进行二次氢化反应后得碳酸氢锂精制液,向碳酸氢锂精制液中滴加HF后过滤得滤饼C,滤饼C经洗涤、烘干后得电池级氟化锂。本发明提供一种深度除Ca2+、Mg2+等杂质离子的方法,并将不同步骤中的废液充分循环利用,不仅使得锂资源的回收利用率达到98%以上,得到的电池级氟化锂质量优于标准HG/T 4507‑2013中要求。
Method for preparing battery-grade lithium fluoride and byproduct industrial-grade lithium fluoride from industrial-grade lithium carbonate
一种由工业级碳酸锂制备电池级氟化锂及副产工业级氟化锂的方法
GUI GANG (Autor:in) / LIU CHANG (Autor:in) / ZHENG LEI (Autor:in) / MA HUIJUAN (Autor:in) / YU GUOWEI (Autor:in)
31.12.2024
Patent
Elektronische Ressource
Chinesisch
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