Preparation method of battery grade lithium carbonate

A lithium carbonate, battery-grade technology, applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of waste of gas raw materials, affecting gas utilization rate, only 7.6%, etc.

Active Publication Date: 2017-09-29
JINGMEN GEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For example, the hydrogenation process is used in Chinese patent 200710019052.3 "A Process for Producing High-purity Lithium Carbonate Using Salt Lake Lithium Resources". The salt lake brine is used as raw material to prepare industrial-grade lithium carbonate, and CO 2 Gas hydrogenation, after the relevant impurity removal process, decomposes lithium bicarbonate under negative pressure conditions, and washes multiple times to prepare battery-grade lithium carbonate; there are also related journal documents "The influence of hydrogenation conditions on the purification of lithium carbonate" (Materials Guide B, 2011.7, 25, Wu Jian) ​​pointed out that 10g of lithium carbonate and carbon dioxide flow rate is 1L / min, react at 25 ℃ for 40min, the carbon dioxide utilization rate obtained is only 7.6%; "Coarse lithium carbonate purification process research" (inorganic salt Industry, 2013.8, 8, Li Yanru) chooses 10g of lithium carbonate to react with 1L / min carbon dioxide at 20°C for 150min, and the utilization rate of carbon dioxide is 2.02%. The amount is very small, which affects the mass transfer process, and then affects the CO 2 Gas utilization, resulting in waste of gas raw materials

Method used

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  • Preparation method of battery grade lithium carbonate
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  • Preparation method of battery grade lithium carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The embodiment of the present invention provides the preparation method of battery grade lithium carbonate, and concrete steps are as follows:

[0075] Hydrogenation reaction: Weigh a certain quality of industrial-grade lithium carbonate and ordinary pure water to make a slurry. Turn on the stirring paddle that comes with the hydrogenation kettle. The interior of the hydrogenation kettle and the stirring paddle are made of titanium to prevent corrosion of the reaction equipment under strong alkali conditions. ~180, 170~175, 165~170r / min, the speed of the fixed stirring blade can effectively control the reaction rate, the hydrogenation reaction rate is the highest under this stirring speed, and the gas feeding device is used to add the collected CO 2 Gas and High Purity CO 2 Gas (purity above 99.99%), the gas velocity is controlled at 2~2.6, 1~1.5, 1.0~1.5m 3 / min, the temperature is controlled at 20 ~ 25 ℃, by installing in each CO 2 storage tank (to collect CO 2 st...

Embodiment 2

[0089] The preparation method of battery grade lithium carbonate: weigh 200kg industrial grade lithium carbonate, add to 1m 3 Add 600L of industrial water to the first-stage hydrogenation kettle, maintain the temperature at 25°C, control the speed of the stirring paddle at 180r / min, and add the collected CO with a gas feeding device. 2 Gas, the gas velocity is controlled at 2.4m 3 / min, after 1.8 hours of reaction, the collected CO 2 Gas consumption is 300m 3 (Under standard atmospheric pressure), the pH meter detects that the pH value in the reactor is 8.2, filters the solution, and adds 50 kg of lithium carbonate from the resulting filter residue to a 200L secondary hydrogenation kettle, and adds 100L of industrial water to it, and the temperature is maintained at 25 °C, the speed of the stirring blade is controlled at 175r / min, and the collected CO is added with a gas feeding device. 2 Gas, the gas velocity is controlled at 1.2m 3 / min, after 1 hour of reaction, the col...

Embodiment 3

[0099] The method for preparing battery-grade lithium carbonate by hydrogenating industrial-grade lithium carbonate: Weigh 200kg industrial-grade lithium carbonate and add to 1m 3 Add 600L of industrial water to the reaction kettle, keep the temperature at 25°C, control the speed of the stirring paddle at 180r / min, and control the gas velocity at 2.4m 3 / min, after 5 hours of reaction, high-purity CO 2 The amount of gas used is 700m 3 (Under standard atmospheric pressure) the pH meter detects that the pH value in the reaction kettle is 7.5, filters the solution, and the resulting filtrate is passed into the decomposition kettle, the temperature is controlled at 90°C, the rotating speed of the stirring paddle is 180r / min, and after 2.5 hours of decomposition Reaction, filtered while hot to obtain the filter residue, the filter residue and food-grade Ca(OH) 2 Equal masses are mixed, the mixed mass and ordinary pure water are prepared into a causticizing solution at a mass rati...

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Abstract

The invention provides a preparation method of battery grade lithium carbonate. The preparation method is characterized by preparing slurry from industrial lithium carbonate, pumping the slurry into a first-order reaction kettle, introducing collected CO2, carrying out full reaction, then carrying out filtration to obtain filter residues, preparing slurry from the filter residues, pumping the slurry into a second-order reaction kettle, introducing collected CO2, carrying out full reaction, then carrying out filtration to obtain filter residues, preparing slurry from the filter residues, pumping the slurry into a third-order reaction kettle, introducing high-purity CO2, carrying out full reaction and then carrying out filtration; firstly pumping the filtrate obtained after each-order filtration into a decomposition reaction kettle, then transferring the filtrate to a causticization reaction kettle, adding a Ca(OH)2 solution, carrying out immediate filtration and washing to obtain filtrates, pumping the filtrates into a concentration kettle, pumping the concentrate into a synthesis kettle after the concentrate passes through a column filled with ion exchange resin and introducing high-purity CO2, thus preparing high-purity battery grade lithium carbonate. The preparation method has the beneficial effects that by utilizing the advantage that lithium carbonate can undergo hydrogenation and efficiently utilize high-purity CO2, CO2 is recycled in the reaction process and foreign ions in the kettles can be ensured to be removed, thus reducing the production cost.

Description

technical field [0001] The invention belongs to the technical field of battery-grade lithium carbonate, and in particular relates to a preparation method of battery-grade lithium carbonate. Background technique [0002] As an important compound of lithium salt, lithium carbonate has many industrial uses. According to GB / T 11075-2013, YS / T582-2013 and other relevant national and industry standards, industrial grade Li 2 CO 3 Content less than 99.5%, battery grade Li 2 CO 3 The content is 99.5% to 99.9%. [0003] Lithium carbonate is widely used in glass ceramics, new energy vehicles, alloys, and medicine. In recent years, with my country's policy of advocating low-carbon and environmental protection, the new energy industry has developed rapidly. The most notable is the rapid growth of the lithium battery industry. Lithium cobalt oxide, lithium nickel oxide, lithium nickel cobalt oxide, lithium iron phosphate and nickel cobalt manganese acid Lithium and other positive ele...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2006/80
Inventor 张云河许开华郭苗苗
Owner JINGMEN GEM NEW MATERIAL
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