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Method for recycling lithium iron phosphate in waste lithium ion batteries

A lithium-ion battery and lithium iron phosphate technology, which is applied in the field of waste power lithium-ion battery recycling and recycling, can solve problems such as increased costs and secondary pollution, and achieve the effects of reducing overall production costs, low cost, and convenient implementation

Active Publication Date: 2017-01-04
BEIJING BEIDA MINGDE CHEM PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional lithium iron phosphate regeneration process often involves the use of a large amount of inorganic acid, resulting in a large amount of inorganic waste liquid, causing secondary pollution to the environment and increasing the cost of recycling

Method used

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  • Method for recycling lithium iron phosphate in waste lithium ion batteries
  • Method for recycling lithium iron phosphate in waste lithium ion batteries
  • Method for recycling lithium iron phosphate in waste lithium ion batteries

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Add 50 g of dried waste lithium iron phosphate power battery positive electrode material to 1.0 L of mixed acid solution of citric acid and oxalic acid (concentration 1.1 mol / L), then add 10.0 mL of 30 wt % hydrogen peroxide aqueous solution, and put it in a water bath Heat to near boiling, then cool down to 85°C and maintain the reaction for 150 minutes.

[0029] (2) After cooling down to room temperature, measure the ratio of lithium, iron and phosphorus in the solution, and add an appropriate amount of lithium dihydrogen phosphate to make the molar ratio of Li, Fe and P in the solution reach 1.05:1:1.05.

[0030] (3) A mixed solvent of ethanol and propanol (volume ratio to the mother liquor is 3:2) was added to the mother liquor to obtain a coarse precipitate of the lithium iron phosphate precursor. Disperse the coarse precipitate of lithium iron phosphate together with sucrose in ethanol (the amount of sucrose added is 7.5wt%, the solid-to-liquid ratio is 1:2), ...

Embodiment 2

[0034] (1) Add 50 g of dry waste lithium iron phosphate power battery positive electrode material to 500 mL of mixed acid solution of citric acid and oxalic acid (concentration 1.1 mol / L), then add 5.0 mL of 30 wt % hydrogen peroxide aqueous solution, and heat in a water bath After boiling, the temperature was lowered to 85°C and the reaction was maintained for 15 minutes.

[0035] (2) Add ethanol to the mother liquor (the volume ratio of the mother liquor is 4:1) to obtain a coarse precipitate of the lithium iron phosphate precursor.

[0036] (3) Disperse the coarse precipitate of lithium iron phosphate together with sucrose in ethanol (5wt% sucrose addition, solid-to-liquid ratio 1:2), high-energy ball milling for 6 hours according to our company's electrode material production process, and the obtained slurry After filtering and drying to remove the solvent, it was calcined at 800° C. for 10 hours in a nitrogen:hydrogen (95:5) mixed atmosphere to obtain a regenerated lithiu...

Embodiment 3

[0040] (1) Add 50 g of dry waste lithium iron phosphate power battery positive electrode material to 800 mL of mixed acid solution of citric acid and oxalic acid (concentration 1.2 mol / L), then add 5.0 mL of 30 wt % hydrogen peroxide aqueous solution, and heat in a water bath The reaction was maintained for 120 minutes until near boiling.

[0041] (2) After cooling down to room temperature, measure the ratio of lithium, iron and phosphorus in the solution, and add an appropriate amount of lithium dihydrogen phosphate to make the molar ratio of Li, Fe, and P in the solution reach 1.1:1:1. Ethanol was added to the mother liquor (the volume ratio to the mother liquor was 2:1) to obtain a rough precipitate of the lithium iron phosphate precursor.

[0042] (3) Disperse the coarse precipitate of lithium iron phosphate together with sucrose in ethanol (the addition of sucrose is 2 wt%, and the solid-to-liquid ratio is 1:2). The difference from Example 1 is that according to our comp...

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Abstract

The invention belongs to the technical field of recycling and cyclic utilization of waste power lithium ion batteries, and particularly relates to a method for recycling lithium iron phosphate in waste lithium ion batteries. The method includes the following steps that firstly, dried waste lithium iron phosphate powder is added into a 0.1-5 mol / L aqueous solution mainly containing organic acid to be processed, and an acidic solution containing Li+, Fe2+ and PO43- is obtained after filtering; secondly, an organic solvent is added into mother liquor to obtain lithium iron phosphate precursor coarse precipitate; thirdly, the lithium iron phosphate precursor coarse precipitate is filtered and collected and dispersed in an organic dispersing agent to be subjected to high-energy ball milling for 0.5-8 hours, the obtained slurry is dried to remove the solvent and then forged for 2-8 hours in atmosphere at 600-800 DEG C, and a recycled lithium iron phosphate cathode material is obtained; fourthly, filtrate obtained in the third step is recycled and used for dissolving of lithium iron phosphate in the first step again in the concentrated mixed organic acid with the organic solvent / dispersing agent separated out.

Description

technical field [0001] The invention belongs to the technical field of recovery and recycling of waste power lithium-ion batteries, and in particular relates to a recovery and regeneration method of waste power lithium iron phosphate. Background technique [0002] With the gradual industrialization and scale of pure electric vehicles and plug-in hybrid electric vehicles, power batteries, one of the most important components of new energy vehicles, will gradually enter the stage of mass scrapping in the next few years. On the one hand, scrapped lithium-ion batteries are toxic and harmful, such as flammability, leaching toxicity, corrosion, and reactivity. Market prices, the contradictions between the development of the new energy automobile industry and the environment and resources brought about by it will become more and more prominent. Therefore, recycling and regenerating lithium iron phosphate electrode materials in power lithium-ion batteries is of great significance f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M10/54
CPCY02W30/84C01B25/45C01P2006/40H01M10/54
Inventor 张冬柏孙晓陈继涛
Owner BEIJING BEIDA MINGDE CHEM PHARMA
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