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Preparation method for lithium iron phosphate precursor without wastewater discharge

A technology of lithium iron phosphate and precursors, which is applied in the field of preparation of precursors in the preparation process of lithium iron phosphate, the positive electrode material of lithium ion batteries, can solve the problems of increasing process flow, consuming energy, increasing costs, etc., to save water resources, Performance and quality improvement, short-term effect

Active Publication Date: 2019-03-12
SHENZHEN QINGYAN EQUIP TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in actual production, it was found that due to the introduction of SO 4 - Impurity ions and ammonium ions will be introduced when adjusting the pH, and ammonium ions are impurity ions that need further treatment. During the preparation process, washing is still required to remove impurities; the washing process will generate a large amount of waste water, and the treatment of waste water will increase the cost. It will also increase the process flow, increase the cost, and consume energy
[0004] Therefore, the current preparation process of lithium iron phosphate precursor has problems such as long process, high cost, large amount of waste water, and large energy consumption.

Method used

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  • Preparation method for lithium iron phosphate precursor without wastewater discharge
  • Preparation method for lithium iron phosphate precursor without wastewater discharge
  • Preparation method for lithium iron phosphate precursor without wastewater discharge

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preparation example Construction

[0031] The preparation method of the lithium iron phosphate precursor without waste water discharge provided by the invention comprises the following steps:

[0032] S1 pre-activates ferric oxide to obtain sub-micron ferric oxide powder, which is sieved (100 mesh) for subsequent use; then take concentrated phosphoric acid (85%) and gradually add it to deionized water for dilution to make the diluted Finally, the concentration of phosphoric acid in the solution is about 20%-30%, and then the submicron ferric oxide powder is mixed with the diluted phosphoric acid solution, so that the molar ratio of phosphorus and iron in the mixed solution is between 1.02-1.1.

[0033] In this step, the ferric oxide is mechanically preactivated, and the method is as follows: put the ferric oxide powder into a ball mill for dry grinding, and then use large-scale zirconia balls (2-3mm specification) at the speed of the ball mill. Under the condition of 2000-2500r / min, high-speed ball milling for ...

Embodiment 1

[0052] S1 Put 30g of ferric oxide powder into a ball mill jar, dry-mill it with large-scale zirconia balls (2mm size), mill it at high speed for 30 minutes, and pass it through a 100-mesh sieve at a speed of 2500r / min to obtain a pre-activated powder of ferric oxide , the next step is standby;

[0053] Take by weighing deionized water 75g, then take by weighing concentrated phosphoric acid (85%) 23.5g, concentrated phosphoric acid is added gradually in deionized water, dilute, the phosphoric acid concentration in the solution after dilution is about 20%, then takes by weighing 16g preactivated three Ferric oxide powder is mixed with the above-mentioned phosphoric acid solution, so that the molar ratio of phosphorus and iron in the mixed solution is about 1.05;

[0054] S2 Ultrasonic disperse the above mixed solution for 10 minutes, then transfer the mixed solution to a ball mill tank, use small-sized zirconia microspheres (0.2mm) to wet mill for 3 hours, and the ball mill tank...

Embodiment 2

[0062] S1 Put 50g of ferric oxide powder into a ball mill jar, dry-mill it with large-scale zirconia balls (2.5mm size), mill at a high speed for 40min, at a speed of 2000r / min, and pass through a 100-mesh sieve to obtain pre-activated ferric oxide powder, the next step for future use;

[0063] Take by weighing deionized water 70g, then take by weighing concentrated phosphoric acid (85%) 38g, concentrated phosphoric acid is added gradually in deionized water, dilute, the phosphoric acid concentration in the solution after dilution is about 30%, then takes by weighing 38g pre-activated dioxygen trioxide Iron powder, mixed with the above-mentioned phosphoric acid solution, so that the molar ratio of phosphorus and iron in the mixed solution is about 1.1;

[0064] S2 Ultrasonic disperse the above mixed solution for 15 minutes, then transfer the mixed solution to a ball mill tank, use small-sized zirconia microspheres (0.25mm) to wet mill for 4 hours, and the ball mill tank speed ...

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Abstract

The invention provides a preparation method for a lithium iron phosphate precursor without wastewater discharge. The preparation method comprises the steps of diluting concentrated phosphoric acid with deionized water, mixing with pre-activated Fe2O3, or further adding a carbon nanotube to obtain a mixed liquid; performing wet grinding after ultrasonic dispersion on the mixed liquid, performing sieving, and adding a dispersing agent for heating, stirring and dispersing; performing heating reaction on the dispersed paste under an N2 environment, and obtaining a precipitant and a solution aftercooling; and performing high-speed separation on the precipitant and the solution, and drying the precipitant, thereby obtaining an iron phosphate (or iron phosphate / carbon nanotube) precursor. The Fe2O3 and phosphoric acid are used as raw materials, the carbon nanotube can be combined, the lithium iron phosphate precursor is prepared by a hydrothermal method, the preparation process is simple, isshort in time and low in energy consumption and cost, no wastewater is discharged, no other side product and impurity ions are introduced, the iron phosphate product is pure, the product is high in purity, and the improvement of the performance and the quality of the lithium iron phosphate battery are facilitated.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a method for preparing a precursor in the preparation process of lithium iron phosphate, a cathode material of the lithium ion battery. Background technique [0002] Lithium iron phosphate battery refers to a lithium ion battery that uses lithium iron phosphate as the positive electrode material. Lithium iron phosphate material has good thermal stability, long cycle life, non-toxic material, and one of the main components is rich in iron element, the battery working platform is stable, and the specific capacity is considerable. In recent years, it has been put into commercial application in large quantities. Lithium iron phosphate cathode material is an important part of lithium iron phosphate battery, and its production process, cost and comprehensive performance are directly related to the cost and performance of lithium iron phosphate battery. [0003] At presen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525
CPCH01M4/5825H01M10/0525Y02E60/10
Inventor 陈建军李志文田勇符冬菊闵杰张维丽王晓伟郭震刘荣跃
Owner SHENZHEN QINGYAN EQUIP TECH CO LTD
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