Method for recycling battery-grade lithium carbonate from anode powder of waste lithium iron phosphate battery

A lithium iron phosphate battery, lithium carbonate technology, applied in lithium carbonate; / acid carbonate and other directions, can solve the trouble of toxic and harmful gas and waste solid recovery, lithium carbonate products have high sodium ion content, can not reach the battery grading and other issues, to achieve the effect of large added value of products, improved lithium leaching rate, and strong social value

Active Publication Date: 2018-01-05
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of them use the method of carbonization of carbon dioxide under normal pressure or the method of hydrogenation decomposition to prepare battery-grade lithium carbonate, but the reaction is difficult to control, and the recovery rate is poor, the production cycle is long, the output is low, and the cost is high in the preparation process.
[0004] At present, there are many researches on the recycling of waste lithium iron phosphate batteries at home and abroad. Chinese patents such as application numbers 201610728143.3, 201610723286.5, and 201110065079.2 all disclose a method for recycling industrial lithium carbonate from lithium iron phosphate batteries. The way of precipitation, on the one hand, alkali washing will take away part of the lithium, resulting in a decrease in lithium recovery; on the other hand, the sodium carbonate precipitation method will make the sodium ion content of lithium carbonate products too high to reach the battery level.
The Chinese patent application number 201410443005.1 discloses a method for recycling and preparing battery-grade lithium carbonate from lithium-ion batteries, including the steps of preparing lithium-fluorine-containing slag, acid leaching, alkali-adjusted pH removal, carbonate precipitation, and washing. This method introduces fluorine, which brings troubles to the subsequent recovery of toxic and harmful gases and waste solids. At the same time, the introduction of sodium during precipitation will cause difficulties in subsequent washing

Method used

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  • Method for recycling battery-grade lithium carbonate from anode powder of waste lithium iron phosphate battery
  • Method for recycling battery-grade lithium carbonate from anode powder of waste lithium iron phosphate battery
  • Method for recycling battery-grade lithium carbonate from anode powder of waste lithium iron phosphate battery

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for reclaiming battery-grade lithium carbonate from waste lithium iron phosphate battery cathode powder, comprising the steps of:

[0026] S1. The positive electrode powder of the waste lithium iron phosphate battery is subjected to high temperature and high pressure alkali boiling, and the first material is obtained by filtering;

[0027] S2. Purifying and removing impurities from the first material to obtain the second material;

[0028] S3, adding ammonium carbonate to the second material, filling with carbon dioxide, performing high temperature and high pressure reaction, and filtering to obtain the third material;

[0029] S4, washing the third material to obtain battery grade lithium carbonate.

[0030] After the waste lithium iron phosphate battery was disassembled and crushed, positive electrode powder 1# and 2# were obtained after screening. The main element analysis is as follows:

[0031] content / %

Embodiment 2

[0033] A method for reclaiming battery-grade lithium carbonate from waste lithium iron phosphate battery cathode powder, comprising the steps of:

[0034] Put 500g of waste lithium iron phosphate battery cathode powder (1#) in an autoclave, add water according to the solid-to-liquid ratio of 1:3, add 75g of NaOH, heat up to 120°C and stir at a stirring speed of 600r / min, react for 5h, and filter to obtain The first material, its main element analysis is as follows (concentrations of metal ions such as Mg, Co, Ni, Fe are all less than 0.001g / L):

[0035] meal

[0036] Adjust the pH of the first material to 6 with sulfuric acid, add a flocculant obtained by mixing polyacrylamide and polyacrylic acid, the mass ratio of the flocculant to the aluminum element in the first material is 5:1000, and filter to remove aluminum to obtain the second material;

[0037] Put the second material in an autoclave, add ammonium carbonate according to 2.5 times the theoretical amount of ...

Embodiment 3

[0042] refer to figure 1 A method for reclaiming battery-grade lithium carbonate from waste lithium iron phosphate battery cathode powder, comprising the steps of:

[0043] Put 500g of waste lithium iron phosphate battery positive electrode powder (2#) in an autoclave, add water according to the solid-to-liquid ratio of 1:5, add 40g of NaOH, heat up to 150°C and stir at a stirring speed of 300r / min, react for 2h, and filter to obtain The first material, its main element analysis is as follows (Mg, Ca, Co, Cl and other ions are not detected in the raw material and the first material, and the concentrations of metal ions such as Ni and Fe are all less than 0.001g / L):

[0044] meal

F

Na

Al

S

K

Li

The first material, g / L

0.7

8.78

0.29

0.04

0.015

8.724

[0045] Adjust the pH of the first material to 4.5 with sulfuric acid, add methacrylic acid as a flocculant, the mass ratio of the flocculant to the aluminum element in the...

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PUM

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Abstract

The invention discloses a method for recycling battery-grade lithium carbonate from anode powder of a waste lithium iron phosphate battery. According to the method, anode powder of the waste lithium iron phosphate battery is studied, a vacuum boiling leaching mode is adopted, the leaching rate of lithium is greatly increased, influence of impurity metals is greatly reduced, and convenience is brought to later decontamination; in the presence of CO2, lithium carbonate is prepared from ammonium carbonate through vacuum precipitation, influence of sodium ions to impurity is avoided, the recyclingeffect of lithium is improved, thermal washing is implemented with RO (Reverse Osmosis) pure water, and the battery-grade lithium carbonate can be prepared. The method is a novel process route whichis short in process, high in lithium recycling rate, high in lithium carbonate purity, large in product additional value and capable of recycling waste lithium iron phosphate anode powder, and has great social values and considerable economic benefits.

Description

technical field [0001] The invention relates to the technical field of lithium battery recycling, in particular to a method for recycling battery-grade lithium carbonate from waste lithium iron phosphate battery positive electrode powder. Background technique [0002] Lithium-ion batteries have little pollution to the environment, no memory effect and excellent electrochemical performance. They have been widely used in portable appliances such as mobile phones, notebook computers, and cameras. They are also the main source of power batteries for electric bicycles and electric vehicles. There are many types of lithium-ion batteries, which can generally be distinguished according to their positive electrode materials. Among them, the lithium iron phosphate positive electrode material has the advantages of stable structure, long cycle life, environmental friendliness, excellent safety and overcharge resistance, making it a One of the most important power lithium-ion batteries. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
Inventor 徐懋刘春丽张宏立
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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