Preparation method of battery-grade lithium carbonate

A lithium carbonate, battery-grade technology, applied in the field of preparation of battery-grade lithium carbonate, can solve the problems of long adsorption-regeneration time, high cost, low overall efficiency, etc., to avoid high acid-base and water consumption, yield and quality Stable, improved process continuity effect

Active Publication Date: 2016-12-07
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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Problems solved by technology

The repeated use of the eluent is complicated, resulting in long adsorption-regeneration time, low efficiency, and large consumption of adsorbent; the load of cation exchange to remove calcium and magnesium is also high, and the cost of resin regeneration is high; electrodialysis only affects the eluent The lithium in the
The joint application of the three steps has a long process, low overall efficiency and high cost
However, the average concentration of lithium in the enrichment solution obtained by this method is lower than 4g/L, and the resin adsorption and regeneration load is large, and the loss of lithium is relatively large.
[0007] U.S. Patent 6764584 discloses a method for obtaining concentrated lithium solution from seawater or brine. Lithium manganate adsorbent will be used to absorb and extract lithium, and the obtained eluate will be concentrated by two-stage conventional electrodialysis to obtain lithium containing 1.5%. Concentrate of about 1000000000000000000000000000000

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  • Preparation method of battery-grade lithium carbonate
  • Preparation method of battery-grade lithium carbonate
  • Preparation method of battery-grade lithium carbonate

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[0042] Such as figure 1 As shown, the present invention provides a method for preparing battery-grade lithium carbonate, which includes the following steps:

[0043] Step 1: Obtaining and pretreatment of raw materials.

[0044] The lithium-containing material liquid used in the present invention is derived from the eluate for lithium extraction by adsorption, wherein the weight ratio of magnesium to lithium ions is 0.3-20, and the lithium content is 80mg / L-10000mg / L. Preferably, the weight ratio of magnesium to lithium ions in the lithium-containing material liquid is controlled to be 0.5-10; the effect of controlling the lithium ion content to be 100mg / L-7000mg / L is better.

[0045] The solid impurities in the lithium-containing material liquid are removed, so that the content of the solid suspended solids (SS) after filtration is not higher than 5 mg / L.

[0046] After the pretreatment of the lithium-containing material liquid, the pH value is adjusted to 2-8 to obtain the first des...

Example Embodiment

[0090] Example 7

[0091] This embodiment is a process for preparing battery-grade lithium carbonate using the lithium-rich concentrate obtained in Example 5 or Example 6 as a raw material.

[0092] Add 2.5kg of flake caustic soda per ton of sodium carbonate. Under heating and stirring conditions, use deionized water to prepare a sufficient amount of 28% soda ash, and vacuum filter for use. At the same time, prepare a sufficient amount of 30% caustic soda solution with deionized water for later use.

[0093] Take 5L of the lithium-rich concentrate obtained in Example 6, heat it to 60°C, add 40mL of the soda lye solution at a ratio of 7L-9L per cubic meter under sufficient stirring, and then slowly add 30% caustic soda solution to form the first reaction Until the pH of the first reaction solution reached 13.0, a total of 139 mL of 30% caustic solution was consumed.

[0094] Continue to stir and react for 40 minutes and then filter to obtain filtrate and filter cake. The filter cake ...

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Abstract

The invention discloses a preparation method of battery-grade lithium carbonate. The preparation method comprises the following steps: taking a lithium adsorption and desorption eluent as a raw material, performing primary and secondary monovalent ion selective electrodialysis treatment, concentrating and enriching a lithium ion by utilizing the monovalent ion selectivity of a monovalent ion selective cation membrane and a monovalent ion selective anion membrane, and intercepting magnesium ions, sulfate ions and borate ions, thereby realizing efficient separation of lithium and magnesium as well as sulfate and borate ions and other impurity ions and lithium concentration and obtaining a lithium-rich concentrated solution with a lithium content of 10-20 g/L and a ratio of magnesium to lithium of 0.1-1; obtaining the battery-grade lithium carbonate through the steps of deep calcium and magnesium removal, heavy lithium conversion, filtering and washing, drying, cooling and the like. According to the preparation method disclosed by the invention, the preparation process of the battery-grade lithium carbonate is greatly shortened, the process continuity is obviously improved, the cost is reduced, and the bottleneck problem of magnesium removal and concentration by using the salt lake lithium adsorption and desorption eluent with high magnesium-lithium ratio is solved.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a method for preparing battery-grade lithium carbonate. Background technique [0002] Using salt lake, geothermal, oilfield water, seawater and other high-magnesium-lithium ratio and low-grade liquid lithium ores as raw materials, lithium is extracted by adsorption method, and the concentration of lithium chloride in the obtained lithium-rich eluent is generally lower than 1000mg / L, and entrained There are more magnesium salts and a small amount of impurities such as sulfate and borate, and the ratio of magnesium to lithium is higher than 1, even reaching more than 10. It must be further removed from magnesium and enriched before it can be used for lithium carbonate, lithium chloride, etc. Preparation of basic lithium salts. The existing treatment technology generally adopts precipitation method, cation exchange method or nanofiltration method to remove ...

Claims

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Application Information

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IPC IPC(8): C01D7/00B01D61/44B01D61/48
CPCB01D61/44B01D61/485C01D15/08C01P2006/80Y02A20/124
Inventor 温现明朱朝梁邓小川段东平马培华邵斐郭效瑛史一飞卿彬菊樊发英王亚男
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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