Preparation method of lithium carbonate

A lithium carbonate and lithium sulfate technology, applied in the preparation of sulfate/bisulfate, lithium carbonate;/acid carbonate, etc., can solve the problem of agglomeration and mutual wrapping, reducing sulfate content, complex chemical composition, etc. problem, to achieve the effect of improving conversion rate, increasing reaction area and simple process

Pending Publication Date: 2022-01-21
JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complex chemical composition and many impurities (including insoluble and insoluble substances) in the acid clinker after acidification and roasting of spodumene, there are agglomeration and mutual wrapping phenomena, resulting in part of the lithium not being leached, but remaining in the filter residue.
During the purification process of the leachate, the coated impurity cannot be removed by chemical precipitation. When the leachate reacts with sodium carbonate to prepare lithium carbonate, on the one hand, the lithium covered by the impurity fails to participate in the lithium precipitation reaction, resulting in a low conversion rate of the reaction. The lithium yield of method has only 82~86% (CN 113003590A, a kind of method for making lithium carbonate by thermal reduction of spodumene); On the other hand, sulfate radical, potassium, sodium etc. will be partly wrapped by lithium carbonate and cannot be removed, resulting in The impurity content such as sulfate radical, potassium, sodium is higher in the gained lithium carbonate product (CN 110078099 A, a kind of method for preparing lithium carbonate from lepidolite leaching purification liquid; Sulfate content technology)

Method used

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  • Preparation method of lithium carbonate
  • Preparation method of lithium carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0047] (1) Add 1000ml of water into the mixing tank, and mix 1kg Li 2 Add acid clinker with O content of 4.62% and 500ml of water evenly, and continue pulping at 25°C for 25 minutes;

[0048](2) Put the slurry preparation prepared in step 1 into a neutralization tank, and after ultrasonic stirring for 20 minutes (ultrasonic frequency 28kHz), slowly add heavy calcium powder to adjust the pH value of the solution in the tank to 6, and leaching 15 with ultrasonic stirring at 30°C Minutes, after standing for 10 minutes, centrifuge and rinse to obtain leachate, leach slag collected in the slag storage tank;

[0049] (3) Put the leaching solution obtained in step 2 into an alkalization tank, heat up to 70°C while ultrasonically stirring, slowly add caustic soda to adjust the pH value to 10, and continue the reaction for 8 minutes, then add 18ml of carbonic acid with a concentration of 220g / L Sodium solution, continue to react at 70°C for 20 minutes after feeding, centrifuge and rin...

Embodiment 2

[0060] (1) According to the liquid-solid ratio of 3:1, step (4) in the embodiment 1 is centrifugally filtered in the washing water storage tank and 2000ml of washing water is added in the slurry mixing tank, and 1kg Li 2 Add the acid clinker with an O content of 4.62%, the remaining 960ml of filtered washing water and 40ml of supplementary water, and continue the slurry preparation at 35°C for 20 minutes;

[0061] (2) Put the slurry prepared in step 1 into a neutralization tank, and after ultrasonic stirring for 15 minutes, slowly add heavy calcium powder, and the rest are the same as step (2) of embodiment 1;

[0062] (3) the sodium carbonate solution that adds is configured by embodiment 1 step (7) gained thermal analysis mother liquor, all the other are with embodiment 1 step (3);

[0063] (4) Water is joined in the slag stirring tank by the liquid-solid ratio of 1.1:1, and all the other are with embodiment 1 step (4);

[0064] (5) Concentrate and filter and evaporate and ...

Embodiment 3

[0072] (1) Centrifugal filtration and washing water (1500ml) in the washing water storage tank of step (4) in Example 2 are added in the slurry mixing tank, and 1kg Li 2 The O content is 4.62% acid clinker and the remaining filtration and washing water (800ml) are evenly added (liquid-solid ratio 2.3:1), and the pulping is continued at 60°C for 25 minutes;

[0073] (2) Put the sizing liquid obtained in step (1) into a neutralization tank, and after ultrasonic stirring for 20 minutes, slowly add heavy calcium powder calcium carbonate to adjust the pH value of the solution in the tank to 7, and leaching with ultrasonic stirring at 60°C for 25 minutes, After standing for 20 minutes, centrifuge and rinse to obtain leachate, and leach slag is collected in the slag storage tank;

[0074] (3) Put the leaching solution obtained in step (2) into an alkalization tank, heat up to 90°C while ultrasonically stirring, add caustic soda to adjust the pH value to 11, and then continue to react...

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Abstract

The invention discloses a preparation method of lithium carbonate. The preparation method comprises the steps of size mixing, neutralization and leaching, alkalization and impurity removal, slag treatment, concentration and filtration, ion exchange, lithium precipitation, primary product washing and separation and drying. According to the method, many defects of the existing sulfuric acid method for producing lithium carbonate are overcome, and the leaching rate of lithium, the impurity removal and purification effect of the lithium sulfate solution, the conversion rate of lithium precipitation reaction and the lithium yield are effectively improved through combined application of the ultrasonic technology; the lithium yield of the whole process is further improved through recovery of lithium in the leaching residues and the alkalization residues and reuse of the heat-out mother liquor generated in the preparation process of the byproduct sodium sulfate. The method is simple in process, convenient to operate and high in industrial feasibility; the lithium yield is greater than 95%, the product purity is high, the quality is stable, and the standard of battery-grade lithium carbonate products in the industry is reached.

Description

technical field [0001] The invention belongs to the technical field of lithium resource extraction, and in particular relates to a method for preparing lithium carbonate by using acid clinker after acidification and roasting of lithium ore as a raw material. Background technique [0002] The production technologies for preparing lithium carbonate from spodumene mainly include sulfuric acid method, chlorination roasting method and pressure cooking method. Due to the serious pollution of the chlorination roasting method, and the removal of chloride ions during subsequent product purification is more complicated. The process of pressure cooking is complicated, the safety risk is high, and the waste residue produced cannot find a suitable use. At present, the sulfuric acid method is mainly used for the large-scale production of lithium carbonate. [0003] Extracting lithium carbonate from spodumene by sulfuric acid method is a relatively mature lithium extraction technology, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08C01D5/06
CPCC01D15/08C01D5/06C01P2006/80
Inventor 李南平葛建敏景晓辉沙亚利王晓青李庆玲
Owner JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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