Method for preparing battery grade lithium hydroxide monohydrate

A lithium hydroxide, battery-level technology, applied in the direction of lithium oxide; efficiency and reduce energy consumption

Active Publication Date: 2015-09-30
JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for preparing battery-grade lithium hydroxide mainly include: spodumene concentrate sulfuric acid leaching freezing method and ordinary lithium carbonate lime causticization method. The lithium carbonate lime causticization method has not been applied on a large scale due to high cost. Spodumene The process of sulfuric acid leaching and freezing of concentrate is widely used, but the current process of spodumene concentrate sulfuric acid leaching and freezing must go through three times of crystallization and purification after leaching lithium from the ore to obtain lithium sulfate leaching solution to obtain qualified battery-grade monohydric hydroxide For lithium products, after three times of evaporation and crystallization, not only the amount of investment in the evaporator is large, but also the energy consumption is high, and a considerable part of the lithium liquid will be taken away by the evaporated steam during the evaporation and concentration of the lithium hydroxide solution, resulting in a further increase in the yield of lithium. This is the most fundamental reason why the lithium yield of this process has been low all the time. At the same time, another important reason for the low lithium yield is that the surface of the sodium sulfate decahydrate that is frozen and separated from the high-concentration lithium hydroxide solution is also frozen. A considerable part of lithium is taken away, so in order to reduce the production cost of battery-grade lithium hydroxide, in addition to shortening the process flow, the loss of lithium must also be reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A preparation method of battery-grade lithium hydroxide monohydrate, comprising the following steps:

[0018] (1) Add 4000L of lithium sulfate solution obtained from leaching spodumene concentrate with sulfuric acid with a calcium content of 0.06g / L and a lithium content of 15g / L in a 5000L reactor, and raise the temperature of the lithium sulfate solution to 80 ℃, then add sodium hydroxide to adjust the pH value of the lithium sulfate solution to 9, then add 965g of sodium oxalate and continue to stir at 80°C for 20 minutes, then filter to obtain a lithium sulfate purification solution with a lithium content of 15g / L;

[0019] (2) Add 357Kg of sodium hydroxide with a mass content of 96% to 4000L of lithium sulfate purification solution with a lithium content of 15g / L to fully dissolve, then freeze to -2°C to precipitate sodium sulfate decahydrate, and then perform centrifugation to obtain Lithium hydroxide freezing liquid and sodium sulfate decahydrate, heat ex...

Embodiment 2

[0024] A preparation method of battery-grade lithium hydroxide monohydrate, comprising the following steps:

[0025] (1) Add 4000L of lithium sulfate solution obtained from lithium adsorbed by sulfuric acid desorption adsorbent with a calcium content of 0.06g / L and a lithium content of 14g / L in a 5000L reactor, and raise the temperature of the lithium sulfate solution to 60°C, then add sodium hydroxide to adjust the pH of the lithium sulfate solution to 11, then add 885g of sodium oxalate to continue stirring at 60°C for 30 minutes, then filter to obtain a lithium sulfate purification solution with a lithium content of 14g / L;

[0026] (2) Add 333Kg of sodium hydroxide with a mass content of 96% to 4000L of lithium sulfate purification solution with a lithium content of 14g / L to fully dissolve, then freeze to 0°C to precipitate sodium sulfate decahydrate, and then perform centrifugation to obtain hydrogen Lithium oxide refrigerated liquid and sodium sulfate decahydrate,...

Embodiment 3

[0031] A preparation method of battery-grade lithium hydroxide monohydrate, comprising the following steps:

[0032] (1) Add 4000L of lithium sulfate solution obtained by dissolving lithium carbonate with sulfuric acid with a calcium content of 0.06g / L and a lithium content of 16g / L in a 5000L reactor, and raise the temperature of the lithium sulfate solution to 70°C, and then Add sodium hydroxide to adjust the pH of the lithium sulfate solution to 10, then add 900g of sodium oxalate and continue to stir at 70°C for 25 minutes, then filter to obtain a lithium sulfate purification solution with a lithium content of 16g / L;

[0033](2) Add 381Kg of sodium hydroxide with a mass content of 96% to 4000L of lithium sulfate purification solution with a lithium content of 16g / L to fully dissolve, then freeze to -1°C to precipitate sodium sulfate decahydrate, and then perform centrifugation to obtain Lithium hydroxide freezing liquid and sodium sulfate decahydrate, heat exchange bet...

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Abstract

The invention discloses a method for preparing battery grade lithium hydroxide monohydrate, which comprises steps: edulcoration and purification of lithium sulfate solution, freezing separation, preparation of lithium hydroxide monohydrate crude products, dissolution and purification of the lithium hydroxide monohydrate crude products and recrystallization. The method for preparing the battery grade lithium hydroxide monohydrate can obtain lithium hydroxide monohydrate finished products just through twice crystallization, and improves leaching efficiency of lithium. Sodium sulfafe decahydrate which is frozen and separated is washed through low temperature water, the lithium in the sodium sulfafe decahydrate is effectively recycled, the technological process is reduced, the yield of the lithium is further greatly improved, the investment of evaporator equipment is reduced, and the cost effectiveness is obvious.

Description

technical field [0001] The invention belongs to the technical field of battery material production, and in particular relates to a method for preparing battery-grade lithium hydroxide monohydrate. Background technique [0002] As one of the raw materials for lithium-ion battery materials, battery-grade lithium hydroxide is in increasing demand every year. At present, the methods for preparing battery-grade lithium hydroxide mainly include: spodumene concentrate sulfuric acid leaching freezing method and ordinary lithium carbonate lime causticization method. The lithium carbonate lime causticization method has not been applied on a large scale due to high cost, and spodumene The sulfuric acid leaching and freezing process of concentrate is widely used, but the current process of spodumene concentrate sulfuric acid leaching and freezing process requires three times of crystallization and purification to obtain qualified battery-grade monohydric hydroxide after leaching lithium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/02
Inventor 何国端李南平蒋燕锋
Owner JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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