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Method for recovering lithium hydroxide from waste filtrate generated in preparation of LiFePO4 material by liquid-phase method

A technology of lithium hydroxide and liquid phase method, which is applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., and can solve problems such as increased cost of lithium raw materials, large loss of lithium salts, and environmental pollution , to achieve the effect of improving utilization rate, low equipment requirements and reducing costs

Inactive Publication Date: 2010-09-15
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the classic synthetic route in the liquid phase method is to use ferrous salt, phosphoric acid and lithium hydroxide as raw materials. During this reaction, the loss of lithium salt is large, and the utilization rate is only about 33.3% (take ferrous sulfate as an example below). Part of the lithium remains in the solution after the reaction. If the lithium is not recycled, the cost of lithium raw materials will inevitably increase, the waste of lithium is serious, and the environmental pollution is also very serious.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of lithium iron phosphate material by liquid phase method: Weigh 3960.917 grams of ferrous ammonium sulfate hexahydrate (analytical pure) and 989.899 grams of phosphoric acid (analytical pure), dissolve the above substances with 7833mL 40% ethanol-water, and dissolve the dissolved solution Transfer to a 10L stainless steel high-pressure reactor, add 466.223 grams of lithium hydroxide for production under stirring, set the stirrer speed at 500 rpm after sealing the reactor, and set the temperature of the reactor at 160°C. After 20 hours of reaction Naturally cool to room temperature. After the reaction is completed, the solution is filtered: the precipitate is washed with deionized water, and the washed precipitate is baked in a vacuum oven at 80° C. to 120° C. for 2 to 4 hours, and then dried to obtain a lithium iron phosphate material.

[0021] 1) Recover the above-mentioned washing liquid and filtrate, put in 432.048 grams of potassium hydroxide, stir and ...

Embodiment 2

[0026] Preparation of lithium iron phosphate material by liquid phase method: Weigh 2808.586 grams of ferrous ammonium sulfate heptahydrate (analytical pure) and 989.899 grams of phosphoric acid (analytical pure), dissolve the above substances with 4519 mL deionized water, and transfer the dissolved solution to 10L Add 3013mL of absolute ethanol to the stainless steel high-pressure reaction kettle, add 466.223 grams of lithium hydroxide for production under stirring, seal the reaction kettle, set the stirrer speed at 400 rpm, and set the temperature of the reaction kettle at 180°C. After 20 hours of reaction, it was naturally cooled to room temperature. After the reaction is completed, the solution is filtered: the precipitate is washed with deionized water, and the washed precipitate is baked in a vacuum oven at 80° C. to 120° C. for 2 to 4 hours, and then dried to obtain a lithium iron phosphate material.

[0027] 1) Recover the above-mentioned washing liquid and filtrate, a...

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Abstract

The invention relates to a method for recovering lithium hydroxide from waste filtrate generated in the preparation of LiFePO4 material by a liquid-phase method, belonging to the technical field of LiFePO4 material preparation. The method comprises the steps of: adding potassium hydroxide or sodium hydroxide to recovered waste filtrate in the process of preparing LiFePO4 material by the liquid-phase method; heating for concentration and filtering; concentrating filtrate by heating, and then filtering; washing and drying precipitate to obtain a crude hydrated lithium hydroxide product; dissolving the crude product in deionized water, adding 8-hydrate barium hydroxide, stirring and filtering; concentrating filtrate by heating, and then filtering; washing and drying precipitate to obtain a lithium hydroxide product. The invention not only recovers most lithium hydroxide remained in a reacted solution to be used as a part of lithium source for preparing the LiFePO4 material, but also recovers and obtains other byproducts, thereby effectively improving the utilization rates of lithium hydroxide and other resources and decreasing the cost for preparing the LiFePO4 material.

Description

technical field [0001] The present invention relates to a kind of preparation LiFePO from liquid phase method 4 The invention discloses a method for recovering lithium hydroxide from waste filtrate of materials, belonging to the technical field of lithium iron phosphate material preparation. Background technique [0002] Due to the excellent comprehensive performance of lithium-ion batteries, it shows a broad space for development in portable energy storage tools, especially in the new energy vehicle industry. Nowadays, the development of new energy vehicles has been mentioned to an unprecedented height by various countries, and the power battery as the core component has naturally received extensive research and attention. As a new generation of lithium-ion battery cathode material, olivine-type lithium iron phosphate has the advantages of low synthetic raw material price, high specific energy, good thermal stability, and no pollution to the environment. It shows good mark...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D1/28
Inventor 刘大军徐小明
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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