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Comprehensive recovery method of lithium iron phosphate waste powder

A lithium iron phosphate and recovery method technology, applied in the direction of phosphorus compounds, chemical instruments and methods, alkali metal compounds, etc., can solve the problems of not realizing effective recovery of lithium, achieve low production cost, eliminate pollution, and have broad application prospects

Active Publication Date: 2018-12-28
ZHUZHOU SMELTER GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the negative electrode of the lithium iron phosphate battery is removed first, and after being heated at a certain temperature for a period of time, it is dissolved and soaked in a mixed acid solution, the waste sheet of the negative electrode is separated from the copper foil, and the copper foil is separated by cleaning. This invention is a convenient, simple and effective method. method, and achieve acid-base recovery and reuse, avoiding the cumbersome recovery methods of conventional methods, but this invention does not realize the effective recovery of lithium

Method used

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  • Comprehensive recovery method of lithium iron phosphate waste powder
  • Comprehensive recovery method of lithium iron phosphate waste powder
  • Comprehensive recovery method of lithium iron phosphate waste powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Step A, oxidative roasting: put 15 kg of lithium iron phosphate waste powder into a roasting furnace, and roast in the air at a temperature of 150° C. for 150 minutes to obtain activated calcined sand.

[0052] Step B, acid back leaching: the liquid-solid ratio is 2.5:1, the temperature is 90°C, the time is 5 hours, the end point pH=4.0, sulfuric acid is added dropwise, the process pH=3, and the leaching residue is obtained, and the Li in the leaching solution is + The content is 21g / L.

[0053] Step C, purification and removal of phosphate: add 1.1 times Fe of the theoretical amount of ferric phosphate precipitation in the leachate 2+ , and slowly add an oxidizing agent at a temperature of 70°C for 3 hours, add a neutralizing agent during the process, and end at pH=5.0, and filter to obtain a purified solution. Among them, the oxidizing agent preferably adopts hydrogen peroxide that does not introduce new impurities, and the neutralizer preferably adopts sodium hydrox...

Embodiment 2

[0059] Step A, oxidative roasting: put 15 kg of lithium iron phosphate waste powder into a roasting furnace, and roast under oxygen condition, T=250°C, t=90 minutes, to obtain activated calcined sand.

[0060] Step B, acid back leaching: the liquid-solid ratio (by mass ratio) of acid back leaching solution to calcined sand is 4:1, T=75°C, t=3 hours, end point pH=2.5, process pH=4, The leaching end point was filtered and separated to obtain leaching residue and leaching solution; the leaching residue was obtained, and the Li content in the leaching solution was 16 g / L.

[0061] Step C, purification and removal of phosphate: add 1.2 times Fe of the theoretical amount of ferric phosphate precipitation in the leachate 2+ , and slowly add an oxidizing agent, T=55°C, t=5 hours, add a neutralizing agent during the purification process, the final pH=3.5, and filter to obtain a purified solution.

[0062] Step D, Calcium and magnesium removal: T=60°C, t=1 hour, first use neutralizer t...

Embodiment 3

[0067] Step A, oxidative roasting: put 15 kg of lithium iron phosphate waste powder into a roasting furnace, and roast under air condition, T=180°C, t=120 minutes, to obtain activated calcined sand.

[0068] Step B, acid back leaching: the liquid-solid ratio is 3:1, T=80°C, t=4 hours, the end point pH=3.0, slowly add sulfuric acid dropwise, the process pH=3.5, filter and separate at the end point of leaching to obtain leaching residue and leaching liquid ; Obtain the leaching residue, and the Li content in the leaching solution is 19g / L.

[0069] Step C, purification and removal of phosphate radicals: add Fe 1.15 times the theoretical amount of ferric phosphate precipitation in the leachate 2+ , and slowly add an oxidizing agent, T=60°C, t=4 hours, add a neutralizing agent during the process, the end point pH=4.0, and filter to obtain a purified solution.

[0070] Step D, Calcium and magnesium removal: T=55°C, t=1.5 hours, first use neutralizer to adjust pH=8, then add 4g / L s...

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Abstract

A comprehensive recovery method of lithium iron phosphate waste powder comprises the following steps that A, lithium iron phosphate waste powder is oxidized and roasted to obtain activated roasted sand; B, acid regurgitation and leaching are performed, wherein the Li in the activated roasted sand is leached out as much as possible, so that valuable elements phosphorus and iron form iron phosphate;C, a certain amount of precipitator is added, and impurities phosphate anions are removed; D, by means of regulation of a neutralizer and sodium carbonate, impurities such as calcium and magnesium inthe solution are removed; E, sodium carbonate is added under the high-temperature condition to obtain battery grade lithium carbonate; F, sodium sulfate is synthesized. The valuable elements phosphorus, iron and lithium in the lithium iron phosphate waste powder are recovered to the most degree, and the method has the advantages of being reasonable in process, low in manufacturing cost, free of pollution, nonhazardous and the like.

Description

technical field [0001] The invention relates to a comprehensive recovery method for lithium iron phosphate waste powder, in particular to a wet comprehensive recovery method for lithium iron phosphate waste powder. Background technique [0002] In recent years, China has become the largest producer of lithium batteries. Since 2012, with the outbreak of new energy vehicles, the demand for power batteries has exploded. Especially on January 14, 2017, the Ministry of Industry and Information Technology took the lead in compiling the "Medium and Long-term Development Plan for the Automobile Industry", which clarified that the annual output of new energy vehicles in my country will reach 2 million by 2020, and that the sales of new energy vehicles in my country will account for the total sales volume by 2025. At the same time, in September 2017, the person in charge of the Ministry of Industry and Information Technology stated that my country has started to study the launch timeta...

Claims

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Application Information

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IPC IPC(8): C01D15/08C01D5/00C01B25/37C22B7/00C22B1/02
CPCC01B25/375C01D5/00C01D15/08C01P2002/72C01P2004/03C22B1/02C22B7/007Y02P10/20
Inventor 廖贻鹏周玉琳张桂海林文军戴慧敏易鹏飞王勇刘敏
Owner ZHUZHOU SMELTER GRP
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