Method for recovering lithium from lithium iron phosphate waste materials for preparing cell-level lithium carbonate

A lithium ferrous phosphate, battery-grade technology, applied in the field of preparation of battery-grade lithium carbonate, can solve the problems of low production efficiency, low product purity, and low lithium yield, and achieve low production cost, high product purity, and lithium recovery high rate effect

Inactive Publication Date: 2018-06-19
江西赣锋循环科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a large amount of slag, low production efficiency, less than 60% lithium yield, and low product purity.
The main problems of this method are that there is a lot of dust in the roasting process of iron-lithium waste, the total yield of lithium is low, and the product quality is poor (high calcium and phosphorus impurities).
[0006] How to so

Method used

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  • Method for recovering lithium from lithium iron phosphate waste materials for preparing cell-level lithium carbonate
  • Method for recovering lithium from lithium iron phosphate waste materials for preparing cell-level lithium carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] A. Take 100kg of lithium iron phosphate waste (Li% is 4.1%), add 150L of tap water, and add 39kg of 98% (wt%) H 2 SO 4 , then add 10kg 99% (wt%) sodium chlorate, reaction time 1h, filter to obtain lithium-containing solution 1 with a volume of V 1 =310L;

[0051] Table 1 Chemical composition of lithium-containing solution 1

[0052] element

Li

Al

Fe

Na

Ca

pH

Contentg / L

12.2

4.2

8.9

0.3

0.8

1.8

[0053] B. Add 100 kg of lithium iron phosphate waste to the lithium-containing solution 1 obtained in step A, stir and react for 30 minutes, the end point pH is 4.5, filter to obtain lithium-containing solution 2 and filter residue, and return the filter residue to step A for acid-dissolved oxidation reaction;

[0054] C. Add 1.9 kg of activated carbon to the lithium-containing solution 2 obtained in step B, control the temperature at 20° C., stir for 2 hours, and filter to obtain lithium-containing solution 3; ...

Embodiment 2

[0060] A. Take 100kg of filter residue (Li% is 3.7%), add 350L of washing water, add 84kg of 31% (wt%) HCl, and then add 60kg of 50% (wt%) hydrogen peroxide, the reaction time is 2h, and filter to obtain lithium-containing The volume of solution 1 is V 2 =430L;

[0061] Table 2 Chemical composition of lithium-containing solution 1

[0062] element

Li

Al

Fe

Na

Ca

pH

Contentg / L

8.9

2.8

6.5

0.2

0.5

1.5

[0063] B. Add 100 kg of lithium iron phosphate waste to the lithium-containing solution 1 obtained in step A, stir and react for 90 minutes, the end point pH is 4.0, filter to obtain lithium-containing solution 2 and filter residue, and return the filter residue to step A for acid-dissolved oxidation reaction;

[0064] C. Add 1.8kg of activated carbon to the lithium-containing solution 2 obtained in step B, control the temperature at 100°C, stir for 0.5h, and filter to obtain lithium-containing solution 3;

[0065...

Embodiment 3

[0070] A. Take 100kg of lithium iron phosphate waste (Li% is 3.9%), add 200L of washing water, and add 81kg of 65% (wt%) HNO 3 , then add the sodium hypochlorite of 100kg 10% (wt %), reaction times 1.5h, filter and obtain the volume that contains lithium solution 1 to be V 1 =350L;

[0071] Table 3 Chemical composition of lithium-containing solution 1

[0072] element

Li

Al

Fe

Na

Ca

pH

Contentg / L

11.2

3.8

8.5

0.3

0.6

1.8

[0073] B. Add 100 kg of lithium iron phosphate waste to the lithium-containing solution 1 obtained in step A, stir and react for 60 minutes, the end point pH is 3.0, filter to obtain lithium-containing solution 2 and filter residue, and return the filter residue to step A for acid-dissolved oxidation reaction;

[0074] C. Add 2.1 kg of activated carbon to the lithium-containing solution 2 obtained in step B, control the temperature at 80° C., stir for 1 hour, and filter to obtain lithium-conta...

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Abstract

The invention discloses a method for recovering lithium from lithium iron phosphate waste materials for preparing cell-level lithium carbonate. The method comprises the following steps: (1) acid soluble oxidation: adding water into the lithium iron phosphate waste materials to prepare pulp, then, adding inorganic acid for dissolving, then adding an oxidizing agent for oxidization, and filtering; (2) residual acid removal: adding lithium iron phosphate waste materials to remove excessive acid in the solution; (3) organic matter removal: adding activated carbon to remove organic matters in the solution; (4) aluminum and magnesium removal: adding calcium compound to regulate the pH (Potential of Hydrogen) of the solution to remove iron and aluminum; (5) evaporation and sodium precipitation: carrying out evaporation and concentration on the solution until Li<+> concentration is 25-35g/l for sodium precipitation; (6) rough removal of calcium: introducing carbon dioxide gas to remove calcium; (7) lithium precipitation: adding soluble carbonate to precipitate Li<+> into the lithium carbonate. The method for recovering lithium from the lithium iron phosphate waste materials for preparing the cell-level lithium carbonate has the advantages of high lithium recovery rate, environment protection, high product purity, simple technology and low production cost and is suitable for industrialproduction.

Description

technical field [0001] The invention relates to a method for preparing battery-grade lithium carbonate, in particular to a method for preparing battery-grade lithium carbonate by recovering lithium from lithium ferrous phosphate waste. Background technique [0002] Due to the advantages of high specific energy, long service life, high rated voltage, high power endurance, low self-discharge rate, light weight, and high and low temperature adaptability, lithium-ion batteries have become a popular choice for digital, communication, aviation, and portable electronic products. preferred power source. With its popularization and application in power vehicles and high-power energy storage facilities, its demand will grow explosively. In 2015, the global lithium-ion battery production reached 100.75GWh, of which small batteries accounted for 66.28%, power batteries accounted for 28.26%, and energy storage batteries accounted for 5.46%. In 2015, my country's lithium-ion battery out...

Claims

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Application Information

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IPC IPC(8): C01D15/08H01M10/54
CPCC01D15/08H01M10/54Y02W30/84
Inventor 李良彬谢绍忠熊训满章小明刘超白有仙胡冰彭爱平李芳芳李忠
Owner 江西赣锋循环科技有限公司
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