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Method for producing low-magnesium battery-stage lithium carbonate from lithium sulfate solution

A lithium sulfate and lithium carbonate technology, applied in carbonate preparations and other directions, can solve problems such as the inability to produce low-magnesium battery-grade lithium carbonate, and achieve the effects of solving the problem of soda ash impurity removal, simple production process and stable product quality.

Active Publication Date: 2008-02-20
TIANQI LITHIUM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Magnesium content exceeds 50PPm in the product that above-mentioned each method produces, can not reach the requirement of producing low-magnesium battery grade lithium carbonate

Method used

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  • Method for producing low-magnesium battery-stage lithium carbonate from lithium sulfate solution

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Experimental program
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Effect test

Embodiment 1

[0038] Present embodiment 1 method comprises the following steps (referring to Fig. 1)

[0039] 1. Put Li 2 6.0m with an O content of 20g / L 3 Lithium sulfate solution is heated to 70°C, add 10kg of sodium hydroxide, react for 10 minutes, the pH value reaches 10, then add Na2 CO 3 8kg, react for 30 minutes, detect CO 3 2- up to 0.5g / L, filtered to obtain purified lithium sulfate solution and purification residue, and measured the purified lithium sulfate solution Ca 2+ =0.0025g / L, Fe 3+ =0.0003g / L, Mg 2+ =0.0018g / L; Then the purified lithium sulfate solution is evaporated and concentrated to 60g / L, and filtered to obtain the clean lithium sulfate solution;

[0040] 2. Put 1.4m 3 The temperature of the condensed water was raised to 80°C, then 420kg of soda ash was added, stirred until it was completely dissolved, then 60kg of purified slag was added, left to stand for 20 minutes and filtered to obtain a purified soda ash solution, and the Na 2 CO 3 =298g / L, Ca 2+ =0.00...

Embodiment 2

[0044] Present embodiment 2 method comprises the following steps (referring to Fig. 1):

[0045] 1. Put Li 2 5.65m with an O content of 25g / L 3 Heat up the lithium sulfate solution to 80°C, add 12kg of sodium hydroxide, react for 15 minutes, adjust the pH value to 11, add Na 2 CO 3 10kg, react for 30 minutes, detect CO 3 2- up to 0.4g / L, filtered to obtain purified lithium sulfate solution and purification slag, and measured the purified lithium sulfate solution Ca 2+ =0.001g / L, Fe 3+ =0.00025g / L, Mg 2+ =0.0015g / L; Then the purified lithium sulfate solution is evaporated and concentrated to 55g / L, and filtered to obtain the lithium sulfate solution;

[0046] 2. Put 1.65m 3 The temperature of the condensed water is raised to 85°C, then 500kg of soda ash is added, stirred until it is completely dissolved, then 30kg of purified slag is added, left to stand for 30min (minutes) and filtered to obtain a purified soda ash solution, and the Na 2 CO 3 =305g / L, Ca 2+ =0.0035g...

Embodiment 3

[0050] The present embodiment comprises the following steps (see Fig. 1):

[0051] 1. Put Li 2 4.05m with an O content of 27g / L 3 Heat up the lithium sulfate solution to 90°C, add 9kg of sodium hydroxide, react for 12 minutes, adjust the pH value to 9, add Na 2 CO 3 6kg, react for 30 minutes, detect CO 3 2- up to 0.3g / L, filter to obtain purified lithium sulfate solution and purification residue, and measure the purified lithium sulfate solution Ca 2+ =0.0036g / L, Fe 3+ =0.00035g / L, Mg 2+ =0.004g / L; Then the purified lithium sulfate solution is evaporated and concentrated to 65g / L, and filtered to obtain the pure lithium sulfate solution;

[0052] 2. Put 1.35m 3 The temperature of the condensed water was raised to 90°C, then 400kg of soda ash was added, stirred until it was completely dissolved, then 45kg of purified slag was added, left to stand for 40 minutes and filtered to obtain a purified soda ash solution, and the Na 2 CO 3 =295g / L, Ca 2+ =0.0025g / L, Mg 2+ =0...

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Abstract

The invention provides a method to produce a low-magnesium battery grade lithium carbonate from lithium sulfate solution. The method comprises the steps that: (1) purification treatment of lithium sulfate solution as following: lithium sulfate solution is co-precipitated to lower the impurities ions Fe3+, Mg2+, Al3+ and Ca2+, and condensed and filtered to further eliminate impurities, and obtain purification residues and a pure finish solution of lithium sulfate; (2) soda is dissolved and added with purification residues obtained from the purified lithium sulfate solution, and used for a filtering media to filter calcium and magnesium and obtain purified soda solution; (3) the purified soda solution is added with complexant EDTA, and stirred for complexation reaction, and slowly added with condensed and impurities eliminated pure finish solution of lithium sulfate, and a crude lithium carbonate is prepared; (4) the crude lithium carbonate is stirred, cleaned, dried and smashed, thus obtaining the low-magnesium battery grade lithium carbonate. The method of the invention has the advantages of simple production technique, stable product quality and low cost, and expertly employs the waste residues in the process, not only solves the difficulty of impurities elimination for soda, but also enhances the recycling ratio of lithium, which is suitable for the production application of the positive pole material of Li-ion battery.

Description

Technical field: [0001] The invention relates to a method for preparing low-magnesium battery-grade lithium carbonate from a lithium sulfate solution. technical background: [0002] Due to the special properties of lithium and lithium compounds, it is more and more widely used in many fields of national economy. In recent years, the lithium battery industry has developed very rapidly. The demand for lithium carbonate for the production of lithium battery cathode materials has not only increased significantly, but lithium carbonate has been gradually replaced by low-cost battery-grade lithium carbonate from the initial high-purity lithium carbonate. With the large-scale application of battery-grade lithium carbonate, higher requirements have been placed on the magnesium in the product. In the past, the magnesium content in the product was required to be controlled to be less than 150PPm, but now the magnesium content is required to be less than 50PPm. [0003] The existing ...

Claims

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Application Information

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IPC IPC(8): C01D7/02
Inventor 姚开林金鹏霍立明黄春莲涂明江梁平武张炳元赵伟
Owner TIANQI LITHIUM CORP
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