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Method for preparing battery-grade lithium carbonate and battery-grade iron phosphate by using lithium iron phosphate battery positive and negative electrode waste powder

A lithium iron phosphate battery, lithium iron phosphate technology, applied in lithium carbonate;/acid carbonate, chemical instruments and methods, phosphorus compounds, etc., can solve the problem of low lithium ion concentration, low lithium recovery rate, Alkali metal high problems, to achieve the effect of strong operability, solving environmental problems and improving economic benefits

Active Publication Date: 2021-09-28
CHANGSHA RES INST OF MINING & METALLURGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The biggest problem of this type of process is that the concentration of lithium ions in the lithium-rich solution after the preparation of iron phosphate is not high, and the concentration of alkali metal (such as sodium) ions is extremely high. Before further preparation of lithium carbonate, it needs to be concentrated and desodiumized. The form of a large amount of loss in the sulfate, the recovery rate of lithium in the actual product lithium carbonate is less than 75%

Method used

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  • Method for preparing battery-grade lithium carbonate and battery-grade iron phosphate by using lithium iron phosphate battery positive and negative electrode waste powder

Examples

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Effect test

Embodiment 1

[0032] A method of preparing a cell grade carbonate and battery-grade phosphate using a phosphate-based lithium phosphate battery, and a process flow thereof, such as figure 1 As shown, including the following steps:

[0033] (1) 1 kg of lithium iron phosphate positive and negative waste powder (main components and content: Li 3.5%, Fe 27.1%, P15.1%) and water mixed were made into a slurry of 1: 3, and the material The slurry was heated to 80 ° C, and the concentration of 98% sulfuric acid, 450 g sulfate and 10 g of calcium chloride were slowly added. The pH of the control reaction system was 1.8-1.9. After 4 hours, filtration was carried out after completion of the reaction. Get a lithium-containing solution and phosphate slag;

[0034] (2) The lithium-containing solution after the step (1) is added to the depth, obtain a high concentration of lithium solution, and prepare a cell-grade carbonate product with a high concentration of lithium solution.

[0035] (3) The phosphotum an...

Embodiment 2

[0047] A method of preparing a cell grade carbonate and a battery-level phosphate using a phosphate-based lithium phosphate battery is preparing a cell-based carbonate and a battery-level phosphate, including the following steps:

[0048] (1) 1 kg of lithium iron phosphate positive and negative powder (main components and content: Li4.0%, Fe28.1%, P16.5%) and water mixed were mixed into slurry of 1: 4, Heat the slurry to 95 ° C, slowly added sulfuric acid with 98% by stirring while stirring, 50m 3 Pure oxygen and 25.2 g of magnesium sulfate, the pH of the control reaction system was 1.6-1.9, and the reaction was 8 hours, and the reaction was filtered after completion, and the lithium-containing solution and phosphot residue were obtained.

[0049] (2) The lithium-containing solution after the step (1) is added to the depth, obtain a high concentration of lithium solution, and prepare a cell-grade carbonate product with a high concentration of lithium solution.

[0050] (3) Mix the...

Embodiment 3

[0062] A method of preparing a cell grade carbonate and a battery-level phosphate using a phosphate-based lithium phosphate battery is preparing a cell-based carbonate and a battery-level phosphate, including the following steps:

[0063] (1) 1 kg of lithium iron phosphate positive and negative waste powder (main components and content: Li 4.1%, Fe 27.5%, P16.3%) and water mixed were made into a slurry of 1: 2.5, and the material The slurry was heated to 95 ° C, and the concentration of 98% sulfate was slowly added while stirring, 500 g of sodium sulfate, the pH of the control reaction system was 1.8-1.95, and the reaction was 3 hours, and the reaction was filtered, and the lithium-containing solution was obtained. Phosphorus iron slag;

[0064] (2) The lithium-containing solution after step (1) is induced, resulting in a high concentration of lithium solution, preparing a cell-grade carbonate product in a high concentration of lithium solution;

[0065] (3) The phosphotum and wat...

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Abstract

The invention provides a method for preparing battery-grade lithium carbonate and battery-grade iron phosphate by using lithium iron phosphate battery positive and negative electrode waste powder, the method specifically comprises the following steps: mixing the lithium iron phosphate positive and negative electrode waste powder with water to prepare slurry, heating, adding inorganic acid, an oxidizing agent and a regulator A, reacting, filtering and washing to obtain a lithium-containing solution and ferrophosphorus slag; carrying out deep impurity removal on the lithium-containing solution, and preparing a battery-grade lithium carbonate product by taking the obtained high-concentration lithium solution as a raw material; mixing ferrophosphorus slag and water to prepare slurry, heating, adding inorganic acid, an oxidizing agent and a regulator B, reacting, filtering and washing to obtain a ferrophosphorus solution; and carrying out deep impurity removal on the ferrophosphorus solution, and preparing a battery-grade iron phosphate product by taking the obtained high-purity ferrophosphorus solution as a raw material. According to the method, the aim of efficiently and comprehensively recycling lithium, iron and phosphorus is achieved, the operability is high, the economic benefit of recycling the lithium iron phosphate battery waste powder can be improved, the environmental protection problem can be solved, and the method is suitable for large-scale production.

Description

Technical field [0001] The present invention belongs to the technical field of secondary resource integrated utilization, and more particularly to a method of preparing battery-grade carbonate and battery-grade phosphite using a positive and negative precursor waste powder of lithium iron phosphate cells. Background technique [0002] In recent years, with the continuous deterioration of the world's energy tensions, domestic and foreign countries have passed policy guidance and distribution to support the development of new energy auto industry, especially in my country's support policies for new energy automotive industries, aimed at new energy vehicles. Realize the improvement of the corner of the car manufacturing industry, so in recent years, my country's new energy vehicle sales have been greatly improved. In 2017, my country's new energy vehicles had a total of 777,000 vehicles throughout the year, an increase of 53% year-on-year; in which pure electric movements were 652,0...

Claims

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Application Information

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IPC IPC(8): C01D15/08C01B25/37
CPCC01D15/08C01B25/375C01P2006/80C01P2006/11C01P2004/61Y02W30/84
Inventor 王奉刚陈坚谢美求
Owner CHANGSHA RES INST OF MINING & METALLURGY