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Method for preparing battery-grade lithium carbonate of three different morphologies

A battery-grade, lithium carbonate technology, applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of low purity of lithium carbonate products, long process flow, uneven particle size distribution, etc., to improve atom economy , cost reduction effect

Inactive Publication Date: 2017-08-04
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at technical defects such as low purity of lithium carbonate products prepared by traditional methods, uneven particle size distribution, need for further refining and purification, and long process flow, the present invention proposes a method using CO 2 As carbon source, the method for preparing battery-grade lithium carbonate in organic phase crystallization

Method used

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  • Method for preparing battery-grade lithium carbonate of three different morphologies
  • Method for preparing battery-grade lithium carbonate of three different morphologies
  • Method for preparing battery-grade lithium carbonate of three different morphologies

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) LiCl solution removal of impurities: use n-butanol as the extractant to extract 3mol / L LiCl solution, the volume ratio of the organic phase to the aqueous phase is 4:1, and a small amount of Ca 2+ , Mg 2+ 、Na + 、BO 4 3- Impurities are separated.

[0030] (2) Preparation of organic phase reaction solution: mix n-butanol loaded with LiCl and trialkylamine to obtain an organic phase reaction solution, and the volume fraction of trialkylamine is 33%.

[0031] (3) Generate Li 2 CO 3 : Add the organic phase reaction solution into a container with a stirring device, start the stirring device, pass carbon dioxide gas into the organic phase through a gas distributor in a stirring state, stir and react at room temperature for 45 minutes, and remove the solid-liquid mixture after the reaction is completed. The two phases are separated. The solid product is washed with a small amount of ethanol and deionized water to remove organic matter and other impurities entrained i...

Embodiment 2

[0033] (1) LiCl solution removal of impurities: use isoamyl alcohol as the extractant to extract 3mol / L LiCl solution, the volume ratio of the organic phase to the aqueous phase is 2:1, and a small amount of Ca 2+ , Mg 2+ 、Na + 、BO 4 3- Impurities are separated.

[0034] (2) Preparation of the organic phase reaction liquid: the isoamyl alcohol loaded with LiCl was mixed with trioctylamine to obtain the organic phase reaction liquid, and the volume fraction of trioctylamine was 60%.

[0035] (3) Generate Li 2 CO 3 : Add the organic phase reaction solution into a container with a stirring device, start the stirring device, pass carbon dioxide gas into the organic phase through a gas distributor in a stirring state, stir and react at room temperature for 30 minutes, and mix the solid-liquid The two phases are separated. The solid product is washed with a small amount of ethanol and deionized water to remove organic matter and other impurities entrained in the product. Aft...

Embodiment 3

[0037] (1) LiCl solution removal of impurities: use n-butanol as the extractant to extract 4mol / L LiCl solution, the volume ratio of the organic phase to the aqueous phase is 4:1, and a small amount of Ca 2+ , Mg 2+ 、Na + 、BO 4 3- Impurities are separated.

[0038] (2) Preparation of organic phase reaction solution: mix n-butanol loaded with LiCl and trialkyl tertiary amine to obtain an organic phase reaction solution, and the volume fraction of trialkyl tertiary amine is 33%.

[0039] (3) Generate Li 2 CO 3: Add the organic phase reaction solution obtained in step (2) into a container with a stirring device, start the stirring device, feed carbon dioxide gas into the organic phase through a gas distributor in a stirring state, and stir and react at 10°C for 30 minutes After the reaction, the solid and liquid phases were separated. The solid product is washed with a small amount of ethanol and deionized water to remove organic matter and other impurities entrained in th...

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Abstract

The invention discloses a method for preparing battery-grade lithium carbonate of three different morphologies (micro-layers, microflowers and nanorods) from carbon dioxide as a carbon source and lithium chloride as a raw material in an organic phase, and belongs to the technical field of chemical synthesis. The method comprises the following steps: firstly, preparing a 1-12mol / L LiCl solution, by taking a polarity organic matter as an extraction agent, adding into an organic phase according to a certain volume ratio, oscillating for more than 10 minutes till two phases are in extraction balance, taking out the organic phase, adding an amino organic matter, introducing a CO2 gas in a stirring state, reacting for 10-60 minutes at 10-60 DEG C, separating the two phases of a gas phase and a solid phase after the reaction is completed, washing a solid product with ethanol and deionized water, and drying, thereby obtaining a battery grade Li2CO3 product. Lithium carbonate particles of three morphologies of micro-layers, microflowers and nanorods are high in purity and uniform in particle size distribution and meets national standards YST552-2013.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to methods for preparing battery-grade lithium carbonate with three different shapes. Background technique [0002] Lithium carbonate is an important industrial product and an important intermediate for the production of other lithium salts. It is widely used in traditional industries such as chemical industry, metal smelting, ceramic material manufacturing, medical and health care, and air conditioning and refrigeration. In recent years, due to the rapid development of electronic information, lithium batteries and atomic energy, especially my country's new energy automobile industry has entered a period of rapid growth, the expansion of cathode material production capacity has driven the rapid development of the upstream battery-grade lithium carbonate industry and the rapid growth of demand . [0003] Compared with the product specifications of industrial-gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2004/16C01P2004/20C01P2004/45C01P2004/50C01P2004/51C01P2004/61C01P2004/64C01P2006/80
Inventor 秦炜李浪隋金淞
Owner TSINGHUA UNIV