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Brine battery grade lithium carbonate preparation method

A brine battery and lithium carbonate technology, applied in battery electrodes, secondary batteries, circuits, etc., to achieve the effects of low production cost, easy industrial production, and short process flow

Active Publication Date: 2018-08-21
INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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  • Description
  • Claims
  • Application Information

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The above technical methods have not been reported at home and abroad so far

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  • Brine battery grade lithium carbonate preparation method

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Effect test

Embodiment 1

[0026] Embodiment 1 (including Embodiment 1-1, 1-2, 1-3)

[0027] The old brine with a Li content of 1500mg / L adopts ion-selective membrane separation technology (old brine membrane separation method) to enrich lithium and reduce magnesium, moderately remove magnesium with sodium carbonate solution, concentrate, and obtain a lithium chloride lithium-rich solution with a Li content of 12.5 g / L, the Mg content is 13.2 mg / L, and the Ca content is 2.8 mg / L; the Li / Ca mass ratio of the solution is ≈4464, and the Mg / Li mass ratio is ≈0.00106.

Embodiment 1-1

[0029] Take 3L of lithium-rich solution, add it to the reaction kettle, raise the temperature to 70°C, and add Na 2 CO 3 solution (wherein, Na 2 CO 3 content of 282g / L, Mg content of 29mg / L; Na 2 CO 3 The dosage is 1.16 times of the stoichiometric amount) 1.18L, after adding Na 2 CO 3 solution, continue to stir and react for 100 minutes, filter, and then fully wash the filter cake with 600 mL of pure water at a temperature of 80°C, and then dry the obtained lithium carbonate filter cake (containing 29.5% of attached water) at 130°C to obtain brine battery grade The lithium carbonate product was 159.7g; the primary yield of lithium was 79.50%.

[0030] The product is Li 2 CO 3 content of 99.4%, Mg content of 0.045%, Ca content of 0.005%, D 50 (average particle size) 3.6 μm.

[0031] After the synthesis is completed, the resulting synthetic mother liquor and washing liquid after filtration contain about 9g / L of Li 2 CO 3 , can be recovered according to the convention...

Embodiment 1-2

[0033] Take 3L of lithium-rich solution, add it to the reactor, raise the temperature to 90°C, add MgCl 2 ·6H 2 O 17.5g, stirring and dissolving; adding Na under stirring condition 2 CO 3 solution (wherein Na 2 CO 3 content of 282g / L, Mg content of 29mg / L; dissolved polyethylene glycol 0.51g; Na 2 CO 3 The dosage is 1.16 times of stoichiometric) 1.18L, add Na 2 CO 3 Solution, continue to stir and react for 60 minutes, filter, and then fully wash the filter cake with 670 mL of pure water at a temperature of 85 ° C, and then dry the obtained lithium carbonate filter cake at 230 ° C to obtain 170.7 g of brine battery-grade lithium carbonate product; The primary yield is 81.02%.

[0034] The product is Li 2 CO 3 content of 94.7%, Mg content of 1.28%, Pb content 50 4.2 μm.

[0035] After the synthesis is complete, the resulting synthetic mother liquor after filtration contains Li 2 CO 3 About 8g / L, containing about 56g / L NaCl, recovered according to conventional meth...

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Abstract

The invention discloses a brine battery grade lithium carbonate preparation method, which comprises: carrying out lithium enriching and magnesium reduction treatment on salt lake old halogen to obtaina lithium-rich lithium chloride solution with a Li content of 6.0-30 g / L, a Mg content of 8.0-1740 mg / L and a Ca content of 1.2-50 mg / L, adding a Na2CO3 solution under a stirring condition, continuously carrying out a stirring reaction, synthesizing, filtering, and drying to prepare the brine battery grade lithium carbonate product with a Li2CO3 content of 93.9-99.4% and a Mg content of 0.04-1.3%. According to the present invention, the deep magnesium removal is not required, and the high value of the impurity magnesium is achieved; by using the brine battery grade lithium carbonate as the lithium source, the uniform doping of the lithium ion battery positive electrode materials such as lithium iron phosphate and a ternary material magnesium (or magnesium and rare earth) is easily achieved, and the electrical properties of the lithium ion positive electrode material is easily improved; and the preparation method has characteristics of low production cost, short process flow, high performance price ratio of the product, easy industrial production and significant economic benefits.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical industry, and in particular relates to a method for preparing brine battery-grade lithium carbonate by using a lithium-rich solution of old brine from a salt lake as a raw material. The brine battery grade lithium carbonate can be used as a lithium source for producing lithium iron phosphate and ternary materials, which are positive electrode materials for lithium ion batteries. Background technique [0002] Battery grade lithium carbonate (Li 2 CO 3 ) is an important inorganic chemical product. With the rapid development of the electronics and electric vehicle industries, the usage of battery-grade lithium carbonate is increasing rapidly. The purity, selling price and added value of battery grade lithium carbonate are higher than those of industrial grade lithium carbonate. At present, battery-grade lithium carbonate is mainly used to prepare lithium-ion battery cathode materials (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/485H01M10/0525
CPCH01M4/485H01M4/5825H01M10/0525Y02E60/10
Inventor 刘述平廖祥文李超
Owner INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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