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Spray pyrolysis device with microwave heating and method for preparing ternary precursor thereof

A technology of spray pyrolysis and microwave heating, which is applied in chemical instruments and methods, electrical components, chemical/physical/physicochemical processes of energy application, etc. It can solve the problem of ternary oxide powder without cost-effective advantages. Physical and chemical indicators, large amount of additives and other problems, to achieve the effect of accelerating thermal decomposition rate, avoiding poor appearance, and excellent product performance

Active Publication Date: 2019-04-19
HENGDIAN GRP DMEGC MAGNETICS CO LTD
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Using the above methods 1-3 can only obtain spherical solid secondary particles with an average particle size of less than 3 μm, and cannot produce solid secondary particle ternary material precursors with an average particle size of 3 to 15 μm, and the amount of additives added is generally Larger, not only increases the cost of raw materials, but also needs to consume more heat to complete the thermal decomposition reaction, and the subsequent high-temperature calcination to prepare the secondary particle shape of the spherical ternary material no longer maintains, resulting in a decrease in the tap density of the product. Increased chloride content (generally Cl>2000ppm)
However, the precursor material prepared by the second spray pyrolysis method in method 4 needs to add a spray pyrolysis process, which has high energy consumption and low output. Compared with the liquid deposition method, it does not have a cost-effective advantage.
[0013] Reference 8 (CN106587172A) discloses a production process and production device for a positive electrode ternary oxide of a power battery. The positive electrode ternary oxide of a lithium battery is prepared by spraying and pyrolyzing a chloride salt raw material solution, and the atomizer adopts a two-fluid (i.e. Two-fluid) aerosol nozzle or pressure nozzle, liquefied gas is used as heating fuel, and the droplets pass through the evaporation zone and drying zone from top to bottom in the spray pyrolysis tower, and then enter the roasting zone with a temperature of 780℃~1100℃ for decomposition. into ternary oxide and hydrogen chloride, the top pressure of the furnace is controlled at -200Pa, and the positive electrode ternary oxide is prepared, and then discharged through the discharge equipment at the bottom of the roasting area, and then dechlorinated by the dechlorinator to obtain the ternary oxide powder. The patent does not mention the physical and chemical indicators of the prepared ternary oxide powder, such as particle shape, particle size and distribution, tap density and Cl root content, etc.

Method used

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  • Spray pyrolysis device with microwave heating and method for preparing ternary precursor thereof
  • Spray pyrolysis device with microwave heating and method for preparing ternary precursor thereof
  • Spray pyrolysis device with microwave heating and method for preparing ternary precursor thereof

Examples

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Embodiment 1

[0126] This embodiment provides a spray pyrolysis device with microwave heating, the tower height of the spray pyrolysis device is 18.6m, the inner diameter is 5.5m, and the vertical distance between the bottom end of the two-fluid nozzle and the initial position of the evaporation zone is 30cm , the ratio of the cavity height in the microwave heating zone to the cavity height in the sintering zone is 1:2, and the number of microwave generator components set in each zone of the microwave heating unit is: 5 groups in the evaporation zone, 3 groups in the drying zone and 2 groups in the thermal decomposition zone, Each group of microwave heaters is arranged with 10 microwave heaters every 1m along the circumference of the spray pyrolysis tower cavity.

[0127] This example also provides a method for preparing a ternary precursor, which is carried out in the spray pyrolysis device with microwave heating provided in this example, and prepared by secondary high-temperature calcinati...

Embodiment 2

[0142] This example provides a method for preparing the ternary 811 precursor, which is carried out in the spray pyrolysis device provided in Example 1, and the prepared ternary 811 precursor is used for secondary high-temperature calcination to prepare ternary 811 Positive electrode material, described method comprises the following steps:

[0143] (1) Configuration of ternary 811 precursor mixed solution

[0144] Accurately weigh a certain mass of LiCl and NiCl according to the molar ratio Li:(Ni+Co+Mn)=1:1, Ni:Co:Mn=0.8:0.1:0.1 2 ·6H 2 O, CoCl 2 ·6H 2 O and MnCl 2 4H 2 O, add deionized water to dissolve and configure a mixed solution with a total metal ion concentration of 0.5M.

[0145] (2) Preparation of ternary 811 precursor

[0146] Start the smoke exhaust fan, the PLC control automatically adjusts the frequency of the smoke exhaust fan, so that the pressure in the furnace reaches the set value -150Pa, then sprays deionized water into the spray pyrolysis device t...

Embodiment 3

[0152] This example provides a method for preparing a Zr-doped ternary precursor. The method is carried out in the spray pyrolysis device provided in Example 1, and the prepared Zr-doped ternary precursor is used for secondary The ternary 811 cathode material doped with Zr is prepared by high-temperature calcination, and the method comprises the following steps:

[0153] (1) Configuration of Zr-doped ternary 811 precursor mixed solution

[0154] Accurately weigh a certain amount of LiCl and NiCl according to the molar ratio Li:(Ni+Co+Mn+Zr)=1.03:1, Ni:Co:Mn:Zr=0.8:0.1:0.095:0.005 2 ·6H 2 O, CoCl 2 ·6H 2 O, MnCl 2 4H 2 O and ZrOCl 2 ·8H 2 O, add deionized water to dissolve and configure a mixed solution with a total metal ion concentration of 1.0M.

[0155] (2) Preparation of Zr-doped ternary 811 precursor

[0156] The difference from Example 1 is that the control operation parameters are as follows: liquid inlet pressure 1.8bar, liquid inlet speed 0.6m 3 / h, the carr...

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Abstract

The invention provides a spray pyrolysis device with microwave heating and a method for preparing a ternary precursor thereof. The spray pyrolysis device comprises a microwave heating unit and a sintering unit from top to bottom; wherein the cavity of the microwave heating unit is provided with at least one set of microwave generator module. The method comprises the following steps: spraying ionized water into the spray pyrolysis device through an atomizing device, sequentially starting microwave generators of an evaporation zone, a drying zone and a thermal decomposition zone, switching the deionized water to a ternary precursor mixed solution after the temperature of the midpoint in the horizontal direction of each zone reaches a set value, and carrying out spray pyrolysis to obtain theternary precursor powder. By microwave heating for the evaporation zone, the drying zone and the thermal decomposition zone of the spray pyrolysis device, the problems of hollowing and breaking of secondary particles of the precursor prepared by spray pyrolysis are fundamentally solved, and favorable conditions are created for the preparation of the ternary precursor having high tap density, smallspecific surface area and low chloride content.

Description

technical field [0001] The invention belongs to the technical field of lithium battery materials, in particular to the field of preparation of lithium-ion battery anode material precursors, and relates to a spray pyrolysis device and a method for preparing a ternary precursor using the spray pyrolysis device, in particular to a spray pyrolysis with microwave heating The device and the method for preparing the ternary precursor by using the same can also be used for preparing other spherical solid secondary particle materials. Background technique [0002] Compared with the liquid phase precipitation method to prepare ternary material precursors, the spray pyrolysis method has the advantages of short preparation time, large output, low cost, no pollution, adjustable particle size, narrow particle size distribution, easy doping and uniform element distribution Easy to control and other advantages, it is a lithium-ion battery precursor preparation technology with great developm...

Claims

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Application Information

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IPC IPC(8): B01J19/12H01M4/505H01M4/525H01M10/0525
CPCB01J19/126H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 龚金保黄明张章明
Owner HENGDIAN GRP DMEGC MAGNETICS CO LTD
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