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Method for recycling waste lithium iron phosphate ion battery anode material

A technology for lithium iron phosphate and ion batteries, which is applied in the field of recycling of cathode materials of lithium iron phosphate batteries, can solve the problem that the electrode materials cannot be recycled and reused, and achieves the effects of protecting the environment, reducing costs, and simplifying the treatment process.

Inactive Publication Date: 2012-04-04
DALIAN JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The disadvantage of the above-mentioned recovery technology is that it can only mechanically recover lithium iron phosphate or other electrode materials, and the purpose of recycling and reusing the inactivated electrode materials cannot be achieved.

Method used

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  • Method for recycling waste lithium iron phosphate ion battery anode material
  • Method for recycling waste lithium iron phosphate ion battery anode material
  • Method for recycling waste lithium iron phosphate ion battery anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The first step pre-processing

[0029] Firstly, 4.1519 g of the obtained electrode material was weighed, and then it was dissolved in 10 ml of concentrated hydrochloric acid and left for 2 hours. Filter it and dilute it to 30ml, measure its content of lithium, iron, phosphorus, the measurement result of present embodiment is that the mass ratio of lithium, iron, phosphorus is 1:1:1, so need not add lithium source and iron source. Concentrate the above solution by evaporation to a volume of about 15ml, adjust its pH value to 5.3 with ammonia water, and name it as 1# sample. Add about 2 g of ascorbic acid thereto (based on the detection of potassium thiocyanate without discoloration and a slight excess of 1 wt%). The solution was diluted to 32ml, and then transferred to a polytetrafluoroethylene hydrothermal kettle with a volume of 80ml.

[0030] The second step of sample synthesis

[0031] After tightening the above-mentioned hydrothermal kettle, put it into an oven, ...

Embodiment 2

[0035] The first step pre-processing

[0036] Firstly, 4.0274 g of the obtained electrode material was weighed, and then dissolved in 5 ml of concentrated hydrochloric acid + 5 ml of deionized water, and left for 2 hours. Dilute to 30ml by filtration. Measure the content of its lithium, iron, phosphorus, the measurement result of present embodiment is lithium, iron, the mass ratio of phosphorus 0.5: 1: 1.4, then need to add lithium source---lithium hydroxide and iron source---subchlorite Iron, the mass ratio to lithium, iron, phosphorus is 3: 1: 1, evaporates and concentrates above-mentioned solution to volume and is about 15ml, adjusts pH with ammonia water to be 4.5, is named as 2# sample; Add about 1.8g of ascorbic acid to it, The detection of potassium thiocyanate does not change color and the excess is about 1% by weight; the solution is diluted to 32ml, and then transferred to a polytetrafluoroethylene hydrothermal kettle with a volume of 80ml.

[0037] The second step...

Embodiment 3

[0042] The first step pre-processing

[0043]Firstly, 4.2051 g of the obtained electrode material was weighed, then dissolved in 10 ml of concentrated hydrochloric acid, and left for 2 hours. Dilute to 30ml by filtration. Measure the content of its phosphorus, iron, lithium, the measurement result of present embodiment is that the mass ratio of lithium, iron, phosphorus is 0.5: 1: 1.4, then need to add lithium source---lithium chloride) and iron source---sulfuric acid The mass ratio of ferrous iron to lithium, iron and phosphorus is 1:1:1. Concentrate the above solution by evaporation to a volume of about 15ml, adjust the pH to 4.5 with ammonia water, and name it 3# sample. About 1.5ml of hydrazine hydrate was added dropwise thereto, based on the detection of potassium thiocyanate without discoloration and a slight excess of about 1 wt%. The solution was diluted to 32ml, and then transferred to a polytetrafluoroethylene hydrothermal kettle with a volume of 80ml.

[0044] T...

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Abstract

The invention discloses a method for recycling a waste lithium iron phosphate ion battery anode material, which comprises the steps of: dissolving collected waste lithium iron phosphate ion battery anode material with hydrochloric acid, measuring contents of phosphorus, iron and lithium; adding iron or / and lithium to prepare a lithium iron phosphorus solution with a certain mass ratio; regulating the pH value to be 2-9 by using ammonia water, then adding a reducing agent therein, finally adding water to be diluted to reach 1 / 3 of the volume of a hydrothermal reactor; reacting at a temperature of 140-180 DEG C for 6-12h in the hydrothermal reactor, filtering, washing and drying a product to obtain lithium iron phosphate powder; carrying out X-ray diffraction (XRD) test on the lithium iron phosphate powder to be lithium iron phosphate with an olivine structure, and displaying with a scanning electron microscope (SEM) as an integral crystal structure. The invention has the beneficial effects of simple processing process, remarkable effect, capabilities of batch processing and realizing recycling of the lithium battery electrode material, reduction in cost, energy source saving and environment protection.

Description

technical field [0001] The invention relates to the technical field of secondary batteries, in particular to the recycling of positive electrode materials of iron phosphate lithium ion batteries. Background technique [0002] Nowadays, lithium batteries have been widely used in various fields. Lithium-ion batteries are used in tens of thousands of applications. According to the survey data of Frost & Sullivan in the United States, the global supply of lithium batteries in 2007 was about 1.76 billion pieces, and it is expected to reach 3.99 billion pieces in 2013. With such a large number of lithium battery applications, the amount of waste generated by used batteries will also be staggering. At present, most of the waste materials of these used batteries are landfilled, and only a small amount is recycled. loss of useful substances. In the prior art, the recovery of lithium iron phosphate positive electrode materials in waste lithium iron phosphate batteries mainly has t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/54
CPCY02E60/12Y02W30/84
Inventor 赵红张大珉梁立君卢璐徐洪峰
Owner DALIAN JIAOTONG UNIVERSITY