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Method for preparing lithium carbonate superfine powder through solvating-out and reaction crystallization

A technology of reaction crystallization and ultra-fine powder, which is applied in the direction of lithium carbonate; High recovery rate and excellent product effect

Inactive Publication Date: 2012-04-11
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method operation period is very long (the gas-liquid reaction time in the specific embodiment provided by CN 101209846A generally reaches 20-40 hours, and the aging time reaches 24 hours, and the drying time reaches 48 hours); in the gas-liquid reaction process, lithium carbonate is easy to Accumulation clogging the ventilation line

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  • Method for preparing lithium carbonate superfine powder through solvating-out and reaction crystallization
  • Method for preparing lithium carbonate superfine powder through solvating-out and reaction crystallization
  • Method for preparing lithium carbonate superfine powder through solvating-out and reaction crystallization

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Embodiment 1

[0026] This embodiment is used to illustrate the method for preparing lithium carbonate ultrafine powder by the dissolution-reaction crystallization method provided by the present invention.

[0027] First prepare LiCl(1~16mol / L)-ethanol-water ternary system solution 50ml and Na 2 CO 3 Solution (1 ~ 4mol / L) 50ml. Then, the two reaction raw materials are quickly mixed and reacted in a 150ml reaction crystallizer under the action of ultrasound and the condition of 5-90°C. Due to the anti-solvent effect of ethanol, lithium carbonate can produce a very high degree of supersaturation and produce a large number of fine crystals. Moreover, ethanol itself is also a dispersant, and there is no need to introduce more other dispersants. The feed solution was filtered and dried to obtain a crystalline product. After the filtrate is rectified, ethanol can be separated for recycling. Experimental result shows, this method can reduce the secondary particle diameter of lithium carbonate ...

Embodiment 2

[0029] This embodiment is used to illustrate the method for preparing lithium carbonate ultrafine powder by the dissolution-reaction crystallization method provided by the present invention.

[0030] In the 150ml reaction crystallizer, add LiHCO 3 Solution (0.5~1.5mol / L) 50ml, control LiHCO 3 Under the condition that the temperature of the solution is 5-60° C., an ultrasonic device is introduced and turned on. Into the reaction crystallizer LiHCO 3 Ethanol is added into the solution, and the amount of ethanol added is 5-85%. After adding the dissolving agent, crystallization and precipitation appeared rapidly, and a large number of bubbles were generated in the solution, indicating that the addition of ethanol promoted the crystallization of lithium carbonate, and the crystallization process of lithium carbonate also promoted the formation of LiHCO. 3 Rapid decomposition, this process can be called dissolution-decomposition-reaction crystallization process.

[0031] The fe...

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Abstract

The invention relates to a method for preparing lithium carbonate superfine powder through solvating-out and reaction crystallization, which comprises the following step of: reacting water-soluble lithium salt with a reactant under the action of an introduced solvating-out agent to prepare the lithium carbonate superfine powder through reaction crystallization. The lithium carbonate superfine powder prepared by the method has the primary particle size of about 200 nanometers and the secondary particle size of about 2 micrometers averagely, and the Brunauer Emmett Teller (BET) specific surface area of more than 7.0m<2> / g. The method has the advantages that: the process is simple, and a product is high and stable in quality, high in recovery rate and convenient to industrialize.

Description

【Technical field】 [0001] The invention relates to the technical field of lithium carbonate, in particular to a method for preparing superfine lithium carbonate powder by dissolution-reaction crystallization. 【Background technique】 [0002] As a basic lithium salt, lithium carbonate is widely used in glass, ceramics, aluminum smelting, information, atomic energy industry, medicine and other industries. It is also the main raw material for the manufacture of metallic lithium and its isotopes, and various fine lithium salts (lithium molybdate, lithium hydroxide, lithium bromide, etc.). High-purity lithium carbonate (greater than 99.9%) is a necessity for lithium-ion batteries, magnetic materials, electronic materials and optical instruments. After entering the 21st century, with the rapid development of the new energy industry and the information industry, the demand for high-purity lithium carbonate at home and abroad is increasing. For example, in recent years, with the inc...

Claims

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Application Information

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IPC IPC(8): C01D15/08
Inventor 孙玉柱宋兴福汪瑾于建国
Owner EAST CHINA UNIV OF SCI & TECH
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