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Methods for preparing iron phosphate precursor and lithium iron phosphate positive electrode material

A technology of lithium iron phosphate and positive electrode materials, which is applied in the direction of carbon preparation/purification, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of tight supply of upstream raw material resources, rising prices, and resource shortages, and achieve low prices and low emissions. less, high recycling efficiency

Pending Publication Date: 2022-01-18
骆驼集团资源循环襄阳有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The increase in demand for lithium iron phosphate batteries will inevitably bring about the following two problems: (1) The shortage of resources. On the one hand, the installed capacity of power batteries has increased due to the continuous growth in the production and sales of 3C, electric tools, new energy vehicles, and electric boats. On the one hand, due to the impact of international political relations, the supply of upstream raw material resources is tight and prices are rising
Taking lithium carbonate as an example, the price of lithium carbonate in March 2021 has doubled compared to November 2020; (2) Environmental pollution, lithium-ion batteries have a life cycle, and the average life of lithium iron phosphate power batteries is 4-6 years, exceeding the life cycle Retirement treatment is required, and the decommissioning of a large number of used batteries has caused great pressure on the environment

Method used

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  • Methods for preparing iron phosphate precursor and lithium iron phosphate positive electrode material
  • Methods for preparing iron phosphate precursor and lithium iron phosphate positive electrode material
  • Methods for preparing iron phosphate precursor and lithium iron phosphate positive electrode material

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A method for preparing an iron phosphate precursor, the preparation process is as follows:

[0032] S1 Discharge the lithium iron phosphate battery in a sodium chloride solution, crush it, and dry it at 200°C to obtain black powder through airflow separation and gravity separation. The content of lithium iron phosphate in the sorted copper foil is less than 0.5%. The lithium iron phosphate content in the aluminum foil is less than 1%, the copper content in the black powder is less than 2%, and the aluminum content is less than 4%.

[0033] S2 According to the ratio of m (phosphoric acid): m (black powder): m (hydrogen peroxide) = 0.4:1:0.3, add phosphoric acid, black powder, hydrogen peroxide in sequence, leaching at 80°C for 12 hours, press filter, separate the carbon material, and obtain the filtrate .

[0034] S3 adds excessive Fe powder to step S2 filtrate, presses filtration after reacting for 5h, detects Cu content in the filtrate, the copper content in the solut...

Embodiment 2

[0038] A method for preparing lithium phosphate, the preparation process is as follows:

[0039] S1 Discharge the lithium iron phosphate battery in sodium chloride solution, crush it, and dry it at 200°C to obtain black powder through airflow separation and gravity separation. The content of lithium iron phosphate in the sorted copper foil is less than 0.5% , The lithium iron phosphate content in the aluminum foil is less than 1%, the copper content in the black powder is less than 2%, and the aluminum content is less than 4%.

[0040] S2 According to the ratio of m (phosphoric acid): m (black powder): m (hydrogen peroxide) = 0.5:1:0.3, add phosphoric acid, black powder, hydrogen peroxide in sequence, leaching at 80°C for 12 hours, press filter, separate the carbon material, and obtain the filtrate ;

[0041]S3 adds excessive Fe powder to step S2 filtrate, presses filtration after reacting for 5h, detects Cu content in the filtrate, the copper content in the solution after ir...

Embodiment 3

[0047] A method for preparing lithium iron phosphate cathode material, the preparation process is as follows:

[0048] S8, weigh lithium carbonate and iron phosphate prepared in Example 1 according to the molar ratio of lithium and iron being 1.01:1, add 10wt% glucose; add ultrapure water, control the solid content to 50%, and then perform ball milling, ball milling time 3h, ball milling The particle size D50 of the final material is 0.5-3μm; the material after ball milling is spray-dried at a temperature of 200°C, and the D50 of the material after spray drying is 5-20μm; the dried material is calcined at a temperature of 780°C, and the calcined The time is 8h, the calcining atmosphere is a nitrogen atmosphere, and the lithium iron phosphate cathode material is obtained, and the appearance is as follows Figure 5 shown.

[0049] The lithium iron phosphate prepared in this example, polyvinylidene fluoride, and acetylene black were mixed in a mass ratio of 8:1:1, uniformly coat...

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Abstract

The invention relates to methods for preparing an iron phosphate precursor and a lithium iron phosphate positive electrode material. The method for preparing the iron phosphate precursor comprises the following steps of: (1) performing discharging, crushing, drying and sorting on a battery containing lithium iron phosphate to obtain black powder; (2) leaching black powder by using phosphoric acid and hydrogen peroxide, and separating out a carbon material after performing filter pressing; (3) adding iron powder and sodium thiosulfate into a filtrate to remove copper; (4) adding an oxidizing agent into the copper-removed filtrate; (5) adding a LiOH solution to adjust the pH value to 1.5-2, and carrying out filter pressing to obtain iron phosphate; (6) adding the LiOH solution to adjust the pH value to 5, and carrying out filter pressing to obtain an Al (OH) 3 byproduct; (7) adding the LiOH solution to adjust the pH value to 6-7, and carrying out filter pressing to obtain lithium phosphate; (8) adding a lithium source and a carbon source into the iron phosphate to prepare lithium iron phosphate; and (9) adding an iron source and a carbon source into the lithium phosphate to prepare the lithium iron phosphate. The raw materials are common, easy to obtain and low in price, the process is simple, the requirement for equipment is low, and thus, the method is suitable for large-scale production; and the utilization rate of the raw material is high, emission is low, environmental protection and low pollution are realized.

Description

technical field [0001] The invention relates to the technical field of lithium battery recycling, in particular to a method for preparing an iron phosphate precursor and a lithium iron phosphate cathode material. Background technique [0002] Lithium-ion batteries have the advantages of high energy density, long service life, high safety, and low environmental pollution. Since the commercialization of lithium-ion batteries, after 30 years of development, lithium-ion batteries have been widely used in 3C, energy storage, electric vehicles and other fields. Compared with ternary batteries, phosphoric acid phosphoric acid batteries have outstanding safety performance, cycle life and cost advantages. BYD will launch blade batteries in 2020, and the shortcomings of low energy density of lithium iron phosphate batteries will be further improved. The installed capacity of lithium iron phosphate batteries will continue to rise. The annual market share of lithium iron phosphate batt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37C01B25/30C01B25/45C01B32/05C01F7/02H01M10/54H01M4/58C22B7/00C22B21/00C22B15/00C22B26/12
CPCC01B25/375C01B25/306C01B25/45C01B32/05C01F7/02H01M10/54H01M4/5825C22B7/007C22B7/006C22B21/0023C22B15/0067C22B15/0091C22B26/12C01P2006/40Y02E60/10Y02P10/20Y02W30/84
Inventor 刘长来夏诗忠王飞陈琳雷青国汪杰
Owner 骆驼集团资源循环襄阳有限公司