Method for preparing high-purity lithium carbonate

A technology of high-purity lithium carbonate and lithium carbonate, which is applied in the direction of electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of dependence on dispersants and the influence of dispersant stability, and achieve small distribution range, uniform particle size, and high purity high effect

Active Publication Date: 2015-06-10
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is easy to operate and has high production efficiency. Compared with the previous technology, it has been significantly improved. However, this method still relies more on the role of dispersant, and the stability of dispersant during use has a great impact on the particle size of the product.

Method used

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  • Method for preparing high-purity lithium carbonate

Examples

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Embodiment 1

[0020] A preparation method of nanoscale high-purity lithium carbonate, the steps are as follows:

[0021] 1) After heating 75.6g of pure water to 60°C, mix it with 37.8g of lithium hydroxide monohydrate, add 1.1g of sodium dodecylbenzenesulfonate and fully stir for 20min, as a lithium source;

[0022] 2) Mix 30.0g carbonamide (urea) with 30.0g pure water as a carbonic acid source;

[0023] 3) Add the reaction precursor lithium source and carbonic acid source into a 250mL stainless steel hydrothermal synthesis reaction kettle in sequence, seal the kettle after fully stirring, put the hydrothermal synthesis reaction kettle into an oven, and raise the temperature to 100°C at a rate of 3°C / min. Insulated for 10 hours and taken out, quenched with cooling water, opened the kettle, filtered the lithium carbonate slurry in the reaction kettle to obtain a lithium carbonate filter cake, and washed 2 times while hot with boiled pure water to obtain a lithium carbonate wet material;

[...

Embodiment 2

[0026] A preparation method of nanoscale high-purity lithium carbonate, the steps are as follows:

[0027] 1) Slowly add 8.9g of anionic polyacrylamide (molecular weight 3 million to 22 million) into a plastic container filled with 89.0g of pure water (pH≈7), and mechanically stir at 100r / min until the solid is completely dissolved, and then 60 Mesh filtration makes dispersant solution;

[0028] 2) After heating 59.8g of pure water to 70°C, mix it with 29.9g of lithium hydroxide monohydrate, and add 5.4g of the dispersant solution obtained in step 1), and fully stir for 15min, as a lithium source;

[0029] 3) Mix 22.5g carbonamide (urea) with 22.5g pure water as a carbonic acid source;

[0030] 4) Add the reaction precursor lithium source and carbonic acid source into a 250mL stainless steel hydrothermal synthesis reaction kettle in sequence, seal the kettle after fully stirring, put the hydrothermal synthesis reaction kettle into an oven, and raise the temperature to 110°C a...

Embodiment 3

[0033] A preparation method of nanoscale high-purity lithium carbonate, the steps are as follows:

[0034] 1) After heating 41.3g of pure water to 80°C, mix it with 20.5g of lithium hydroxide monohydrate, and dropwise add 0.06g of anionic sodium polyacrylate (molecular weight: 1000-5000), stir well for 10min, as a lithium source;

[0035] 2) Mix 15.0g carbonamide (urea) with 15.0g pure water as a carbonic acid source;

[0036] 3) Add the reaction precursor lithium source and carbonic acid source into a 250mL stainless steel hydrothermal synthesis reaction kettle in sequence, seal the kettle after fully stirring, put the hydrothermal synthesis reaction kettle into an oven, and raise the temperature to 120°C at a rate of 3°C / min. Take out after being kept warm for 5h, open the kettle after quenching with cooling water, filter the lithium carbonate slurry in the reaction kettle to obtain lithium carbonate filter cake, and wash 4 times while hot with boiled pure water to obtain li...

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Abstract

The invention belongs to the technical field of preparation of nanoscale lithium salt and particularly discloses a method for preparing high-purity lithium carbonate. The method includes the steps that firstly, pure water is heated to 60-80 DEG C, the pure water and lithium hydroxide monohydrate are mixed with the mass ratio being two to one, then, a small amount of water-soluble dispersant is added into the mixture and is sufficiently stirred, and the mixture serves as a lithium source; secondly, percarbamide and pure water are mixed in equal mass to serve as a carbonic acid source, and the molar ratio of the percarbamide to the lithium hydroxide monohydrate is 1:1.80-1.95; thirdly, the lithium source and the carbonic acid source are added into a hydro-thermal synthesis reaction still and are sufficiently stirred, then, the still is closed and placed in a drying oven, the still is heated to 100 DEG C-120 DEG C at the speed of 3 DEG C/min and is taken out after being contained for 5-10 h, lithium carbonate size in the still is filtered to obtain a filter cake, the hot filter cake is washed for 2-4 times through boiling pure, and then wet materials are obtained; fourthly, the wet materials are dried for 8-15 h at the temperature being 250 DEG C-350 DEG C, the pressure being -0.1 Mpa- -0.08 Mpa, and finally lithium carbonate powder with the particle diameter being 20-90 nm is obtained.

Description

technical field [0001] The invention relates to the technical field of preparation of nanoscale lithium salts, in particular to a preparation method of nanoscale high-purity lithium carbonate. Background technique [0002] Lithium-ion batteries have high capacity, high voltage, low energy consumption, no memory effect, no pollution, and small size. It is widely used in electronic products such as mobile phones, PDAs, notebook computers, portable CDs, etc., and is gradually expanding to the fields of electric vehicles, space technology, and national defense industry. It is the most concerned product nowadays. One of the new batteries. Lithium-ion batteries are composed of negative electrode materials, positive electrode materials, and electrolytes. However, the existing electrode and electrolyte materials have reached the limit of performance. The development of a new generation of lithium-ion batteries urgently needs a breakthrough in material technology. Studies have show...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCH01M4/58H01M10/0525Y02E60/10
Inventor 翟建明纪东海黄磊徐涛陈格
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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