Battery-grade lithium carbonate preparation method based on phase transformation

A technology of phase transformation and lithium carbonate, which is applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of inability to process heterogeneous lithium carbonate raw materials, restricting the development of large-scale technology industries, and requiring high purity of raw materials, etc. , to achieve the effect of ensuring high purity and quality, fast speed and slow speed

Inactive Publication Date: 2016-04-20
TSINGHUA UNIV +1
View PDF15 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Therefore, the existing hydrogenation method and causticization method are both low-concentration reaction systems, which have problems such as low efficiency and high cost.
[0013] There are also bibliographical reports to use lithium chloride or lithium hydroxide as raw material, prepare battery-grade lithium carbonate with carbonate precipitation method (Li Liangbin, Hu Naigen, Huang Xuewu, Ge Yuwei, Zhu Shigui, Xiong Xunman, Ma Zhenqian, a kind of lithium chloride solution is used to prepare battery The method of grade lithium carbonate, CN101609888; Ma Jin, Ma Aijun, Xu Zhongji, He Guocai, Yi Chao, Lu Xingwu, Cheng Liang, Li Yuliang, Ji Wuren, Gong Dalei, Shao Chuanbing, Li Shourong, Zhang Enyu, Li Yu, Xue Yingying, A preparation process of battery-grade lithium carbonate, CN103351010A), the disadvantage of this method is that the purity of raw materials is very high, and it cannot handle heterogeneous lithium carbonate raw materials
[0014] In short, although the predecessors have done a lot of work in the preparation of battery-grade lithium carbonate, the existing processes have problems such as low efficiency, high raw material requirements, and high costs, which restrict the large-scale industrial development of these technologies

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Battery-grade lithium carbonate preparation method based on phase transformation

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] The invention provides a method for preparing battery-grade lithium carbonate based on phase transformation. The method uses heterogeneous lithium carbonate as a raw material, and uses water washing-phase transformation-causticization-carbonization-fine impurity removal method to prepare battery-grade lithium carbonate. Specific steps are as follows:

[0031] 1) Phase transformation: the lithium concentrate with a lithium carbonate content of 50-95wt% is mixed with water to make a 10-50wt% slurry, and then a phase transformation agent is added to control the mol ratio of lithium carbonate and the phase transformation agent to be 1: 1-5, stir (50-500 rpm) at 10-100°C for 0.5-5 hours, filter to obtain the lithium content (in the form of Li 2 O meter) 2.0-6.0wt% high-concentration lithium salt solution;

[0032] 2) Causticization: mix the lithium salt solution and the inorganic base in a molar ratio of 1:1-4, stir at 10-100°C (50-500 rpm) and react for 0.5-5 hours, filter...

Embodiment 1

[0039] Weigh 100 grams of lithium concentrate with a lithium carbonate content of 50wt%, mix it with water to make a 15wt% slurry, then add hydrochloric acid, control the molar ratio of lithium carbonate to hydrochloric acid to be 1:1, and stir (500 rpm) at 10°C for reaction 0.5 hour, filter, obtain lithium content (with Li 2 O meter) 2.0wt% lithium salt solution; Lithium salt solution and sodium hydroxide were mixed in a molar ratio of 1:1, stirred at 10°C (500 rpm) and reacted for 5 hours, filtered to obtain lithium content (in Li 2 (O) 2.0wt% causticizing solution; the causticizing solution is continuously passed through an ion exchange column filled with equal amounts of styrene cation exchange resin D-61 and acrylic acid cation resin D113 to obtain a refined causticizing solution; 40 liters of causticizing solution at the standard (0°C, 1 atm) carbon dioxide ratio, feed carbon dioxide into the refined causticizing solution, stir at 60°C (50 rpm) and react for 0.5 hours, s...

Embodiment 2

[0041] Weigh 100 grams of lithium concentrate with a lithium carbonate content of 95wt%, mix it with water to make a 50wt% slurry, then add sulfuric acid, control the molar ratio of lithium carbonate to sulfuric acid to be 1:3, and stir (50 rpm) at 100°C for reaction 5 hours, filter, obtain lithium content (with Li 2 O meter) 5.0wt% lithium salt solution; Lithium salt solution and potassium hydroxide were mixed in a molar ratio of 1:4, stirred at 100°C (50 rpm) and reacted for 0.5 hour, filtered to obtain lithium content (in Li 2 O meter) 5.0wt% causticizing solution; The causticizing solution is continuously passed through the ion exchange column filled with styrene cation exchange resin 734, D001 and quaternary ammonium type cation resin D254 (three weight ratios 10:2:1), Obtain refined causticizing solution; according to the ratio of 200 liters of standard (0°C, 1 atm) carbon dioxide per liter of refined causticizing solution, feed carbon dioxide into the refined causticizi...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a battery-grade lithium carbonate preparation method based on phase transformation, belonging to the technical field of the preparation of inorganic chemical materials. The preparation method comprises the following steps: by taking lithium concentrate as a raw material, first mixing the lithium concentrate and water to prepare 10 to 50% serous fluid, then adding a phase transformation agent, and reacting for 0.5 to 5 hours at 10 to 100 DEG C to obtain a high-concentration lithium salt solution; then mixing the lithium salt solution and inorganic alkali, and reacting to obtain a high-concentration causticization solution; introducing the causticization solution into a cation exchange column to obtain a refined causticization solution, and then introducing carbon dioxide into the refined causticization solution to obtain crude lithium carbonate; and finally mixing the crude lithium carbonate and an appropriate amount of composite refined impurity removal agent in water, and reacting to obtain a battery-grade lithium carbonate product with a main content more than or equal to 99.5 percent by weight. By adopting the phase transformation method, the concentration of the lithium salt solution is remarkably increased, the high-concentration causticization and carbonization can be realized, the preparation efficiency of the battery-grade lithium carbonate is increased, and a novel way is provided for the industrialized preparation of the battery-grade lithium carbonate.

Description

technical field [0001] The invention relates to a method for preparing battery-grade lithium carbonate based on phase transformation, and belongs to the technical field of preparation of inorganic chemical materials. Background technique [0002] The increasing demand for green new energy sources such as lithium-ion batteries in modern society has promoted the rapid development of related high-purity basic lithium salts and lithium battery materials. [0003] As a basic lithium salt material, battery-grade lithium carbonate is mainly used to manufacture positive electrode materials for lithium batteries. Lithium batteries have the advantages of good chemical properties, strong power storage capacity, long life, and small self-discharge, and are widely used in electric vehicles, notebook computers, portable phones and other fields. As the world's largest consumer of lithium, my country's demand for battery-grade lithium carbonate is increasing year by year. However, due to t...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2006/80
Inventor 向兰魏飞曾云张英才温海军袁波易美桂
Owner TSINGHUA UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap