Method for preparing low-sulfur ternary precursor

A technology of precursors and reactors, applied in the field of preparation of low-sulfur ternary precursors, can solve the problems of ternary materials affecting cycle performance

Active Publication Date: 2013-10-09
XTC NEW ENERGY MATERIALS(XIAMEN) LTD
View PDF4 Cites 22 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] During the preparation of battery materials, precipitation and crystallization directly affect the physical and chemical properties of the product. The precipitation product contains a large number of impurities, such as Ca, Mg, Fe, Cu, Zn, etc. Among them, cationic impurities are easily cleaned and removed by beating and pressure washing, while anionic impurities ( Cl - , SO 4 2- , NO 3 - ) and so on cannot be removed by conventional washing methods. During the precipitation process, the anions are physically and chemically adsorbed on the surface and inside of the ternary precursor particles, forming the precipitation of basic metal sulfate double salt, which exists in the product, resulting in S content High, the preparation of ternary materials seriously affects the cycle performance. In order to effectively control the sulfate content in the product, it is necessary to control the precipitation stage and the discharge stage to reduce the SO in the ternary precursor. 4 2- content, to meet the requirements of battery materials

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add the cobalt-nickel-manganese solution, sodium hydroxide and ammonia water into the double-layer inner cylinder structure reaction, and control the stirring intensity to 1.25kW / m 3 , The material stays in the reactor for 8 hours, and the pH value of the precipitation is 11.0. After the product is qualified, the solution is filtered and removed, and the temperature is 60°C, and the LiOH concentration is 2.0mol / L. The washing time was 120min with continuous agitation at 50rpm. After filtering and removing the solution, use a plate and frame filter press to pressurize and wash and dry 6 times. The washing time is 10 minutes each time. After washing, the conductivity of the mother liquor is 15uS / cm. After washing, the ternary precursor is quickly dried and screened in a rotary kiln. , the sulfur content in the ternary precursor was detected to be 1300ppm.

Embodiment 2

[0021] Add the cobalt-nickel-manganese solution, sodium hydroxide, and ammonia water into the double-layer inner cylinder structure reaction, and control the stirring intensity to 1.30kw / m 3 , the material stays in the reactor for 6 hours, and the pH value of the precipitation is 11.5. After the product is qualified, the solution is filtered and removed, and the temperature is 40°C, and the LiOH concentration is 1.0mol / L. The washing time was 160min with continuous agitation at 70rpm. After filtering and removing the solution, use a plate and frame filter press to pressurize and wash and blow dry 8 times. The washing time is 15 minutes each time. The conductivity of the mother liquor after washing is 12uS / cm. , the sulfur content in the ternary precursor was detected to be 900ppm.

Embodiment 3

[0023] Add the cobalt-nickel-manganese solution, sodium hydroxide, and ammonia water into the double-layer inner cylinder structure reaction, and control the stirring intensity to 1.40kw / m 3 , the material stays in the reactor for 12 hours, and the pH value of the precipitation is 10.5. After the product is qualified, the solution is filtered and removed, and the temperature is 60 ° C, and the LiOH concentration is 4mol / L. 100rpm continuous stirring washing time 200min. After filtering and removing the solution, use a plate and frame filter press to pressurize and wash and dry 6 times. The washing time is 20 minutes each time. After washing, the conductivity of the mother liquor is 20uS / cm. After washing, the ternary precursor is quickly dried and screened in a rotary kiln. , the sulfur content in the ternary precursor was detected to be 1600ppm.

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 method for preparing a low-sulfur ternary precursor, relating to lithium-ion anode materials. The method for preparing the low-sulfur ternary precursor, provided by the invention, is efficient, simple and convenient, and the sulfur content of the ternary precursor can be reduced through controlling a precipitation stage and an after-treatment method and is reduced to 2,000ppm so as to meet the requirements of lithium-ion batteries for ternary materials. The method comprises the steps of: (1) simultaneously introducing three solutions, namely ternary material liquid, a sodium hydroxide solution and ammonia water, into a reaction kettle, stirring, and carrying out chemical crystallization so as to obtain a ternary precursor; (2) filtering the ternary precursor obtained in the step (1) so as to remove mother liquor, then, conveying the ternary precursor into a turbine-stirring alkaline cleaning tank, carrying out water-bath heating, stirring and then filtering; (3) washing a product obtained after alkaline cleaning by using a plate and frame filter until the conductivity of the washed water is not higher than 20 us/cm; and (4) quickly drying a washed qualified material by a rotary kiln, and sieving to obtain the low-sulfur ternary precursor, wherein the S impurity content of the obtained low-sulfur ternary precursor is not higher than 2,000ppm.

Description

technical field [0001] The invention relates to lithium ion cathode materials, in particular to a preparation method of a low-sulfur ternary precursor. Background technique [0002] With the continuous development of lithium-ion battery material technology, the application of lithium-ion batteries continues to expand, the market demand has increased sharply, and the types of lithium-ion cathode materials have diversified: lithium cobaltate, lithium manganate, ternary materials, lithium iron phosphate, vanadic acid Lithium, etc. Lithium cobalt oxide is currently the most widely commercialized cathode material. Due to its high price, it is not conducive to environmental protection, and its specific capacity is relatively low. It is gradually being replaced by a new type of green and environmentally friendly ternary cathode material. [0003] At present, the preparation methods of ternary materials are mainly divided into high-temperature solid-phase method and liquid-phase co-...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00
Inventor 马跃飞钱文连王凯郑超郑隽
Owner XTC NEW ENERGY MATERIALS(XIAMEN) LTD
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