Recycling method of waste lithium iron phosphate positive electrode material

A technology for lithium iron phosphate and positive electrode materials, which is applied in the field of recycling waste lithium iron phosphate positive electrode materials, and can solve the problems of large waste water discharge, complicated recycling process, and high impurity content of lithium iron phosphate

Active Publication Date: 2020-07-10
GUANGDONG GUANGHUA SCI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, patent CN104953200A discloses using acid solution to dissolve waste lithium iron phosphate powder, adding a surfactant to the acid solution after dissolving, adjusting the pH value, filtering the precipitate and obtaining battery grade iron phosphate, mixing iron phosphate with lithium carbonate and carbon source Lithium iron phosphate is obtained by calcining. This technical solution fails to fully recover the electrolyte remaining on the waste lithium iron phosphate electrode. At the same time, an acid solution is used to dissolve the waste lithium iron phosphate when preparing iron phosphate. This method still needs to use the waste iron phosphate Different metal elements in lithium materials are extracted and recovered separately. The recovery process is complicated, the process is long, the waste water d

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Take the waste lithium iron phosphate positive electrode sheet and grind it for 3 hours at a speed of 400 r / min to obtain the positive electrode sheet powder. Take 3 kg of positive electrode powder, add 6 kg of diethyl phosphate, transfer it to a supercritical extraction tank, fill it with carbon dioxide to a pressure of 7.5MPa, keep the temperature at 38°C, extract for 60 minutes, and the obtained positive electrode material powder is filtered The net is isolated and left in the extraction tank, the supercritical carbon dioxide and diethyl phosphate mixture carrying the electrolyte is transferred to the liquid separation tank, and the liquid separation tank is allowed to stand for stratification, and most of the diethyl phosphate is recovered, and then the carried electrolytic The liquid supercritical carbon dioxide is transferred to the carbon dioxide storage tank, the pressure of the storage tank is reduced to normal pressure, the electrolyte is recovered, and the...

Embodiment 2

[0042] (1) Take the waste lithium iron phosphate positive electrode sheet and grind it for 3 hours at a speed of 400 r / min to obtain the positive electrode sheet powder. Take 3.1 kg of positive electrode powder, add 4.5 kg of diethyl phosphate, transfer it to a supercritical extraction tank, fill it with carbon dioxide to a pressure of 11MPa, keep the temperature at 42°C, extract for 45 minutes, and the obtained positive electrode material powder is filtered Isolated and left in the extraction tank, the mixture of supercritical carbon dioxide and diethyl phosphate carrying the electrolyte is transferred to the liquid separation tank, where it is left to stand for stratification, and most of the diethyl phosphate is recovered, and then the electrolyte is carried The supercritical carbon dioxide is transferred to the carbon dioxide storage tank, the storage tank pressure is reduced to normal pressure, the electrolyte is recovered, and the positive electrode material powder left i...

Embodiment 3

[0049] (1) Take the waste lithium iron phosphate positive electrode sheet and grind it for 2 hours at a speed of 300 r / min to obtain the positive electrode sheet powder. Take 3 kg of positive electrode powder, add 15 kg of tributyl phosphate, transfer to a supercritical extraction tank, fill with carbon dioxide to a pressure of 23MPa, keep the temperature at 70°C, extract for 15 minutes, and the obtained positive electrode material powder is filtered Isolated and left in the extraction tank, the mixture of supercritical carbon dioxide and tributyl phosphate carrying the electrolyte is transferred to the liquid separation tank, where it is left to stand for stratification, and most of the tributyl phosphate is recovered, and then the electrolyte is carried The supercritical carbon dioxide is transferred to the carbon dioxide storage tank, the storage tank pressure is reduced to normal pressure, the electrolyte is recovered, and the positive electrode material powder left in the ...

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Abstract

The invention relates to a recycling method of a waste lithium iron phosphate positive electrode material. The method comprises the following steps: adding phosphate into the waste lithium iron phosphate positive electrode material, then carrying out supercritical carbon dioxide extraction, and filtering to obtain a solid intermediate A; heating the solid intermediate A to obtain a solid intermediate B; and adding a polymer containing a benzene ring into the solid intermediate B, and calcining to obtain regenerated lithium iron phosphate. The method is simple in process, low in environmental pressure, low in manufacturing cost, good in atom economy, controllable in quality and easy to industrialize, and the final product is good in performance.

Description

technical field [0001] The invention relates to the technical field of battery material recycling, in particular to a method for recycling waste lithium iron phosphate cathode materials. Background technique [0002] Lithium iron phosphate is an important cathode material for lithium batteries. It has an orthorhombic olivine structure. Lithium ions can move and intercalate in the crystal, and has electrochemical activity. In a certain voltage range, the olivine structure of lithium iron phosphate is stable. It is not easy to transform into a spinel structure. The actual specific capacity of lithium iron phosphate can reach 140mAh / g, the discharge voltage is 2.0-4.0V, and the charge and discharge times can reach 2000 times. Compared with lithium-ion battery cathode materials such as lithium manganese oxide and ternary materials, lithium iron phosphate batteries have high safety performance and do not contain highly toxic heavy metal ions. In addition, lithium iron phosphate...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M10/54
CPCC01B25/45C01P2006/40C01P2006/80H01M10/54H01M2004/028Y02E60/10Y02W30/84Y02P20/54
Inventor 李立平李煜乾卢超黄永润
Owner GUANGDONG GUANGHUA SCI TECH
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