A kind of preparation method of aluminum-magnesium-nickel-manganese spherical cobalt tetroxide

A technology of tricobalt tetroxide and magnesium-nickel-manganese, which is applied in the direction of structural parts, electrical components, battery electrodes, etc., can solve the problem that the specific capacity and cycle retention rate of the battery cannot be kept in balance, the precipitation of doping elements is incomplete, and it is difficult to ensure the electrical performance of the battery To achieve excellent test results, avoid aggregation, and good sphericity

Active Publication Date: 2020-12-15
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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AI Technical Summary

Problems solved by technology

However, the existing chemical wet doping of cobalt tetroxide is prone to aggregation of doping elements when doping multiple elements, especially the problem of aggregation of doping elements such as aluminum flakes is prone to occur in aluminum doping, and there are also doping elements Incomplete precipitation, unstable content of doping elements in the product, etc.
When doping multiple elements, if the content of each doping element is unreasonable, it is difficult to ensure that lithium cobalt oxide and its battery prepared by doping tricobalt tetroxide have good electrical properties, in terms of battery specific capacity and cycle retention rate. unable to maintain balance

Method used

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  • A kind of preparation method of aluminum-magnesium-nickel-manganese spherical cobalt tetroxide
  • A kind of preparation method of aluminum-magnesium-nickel-manganese spherical cobalt tetroxide
  • A kind of preparation method of aluminum-magnesium-nickel-manganese spherical cobalt tetroxide

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Experimental program
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Effect test

Embodiment 1

[0025] 1. Prepare the solution: take the cobalt sulfate solution produced in the extraction process, dilute it to a concentration of 1.7mol / L with hot pure water; weigh 10g of the doping element aluminum sulfate octadecahydrate, heptahydrate Add 2g of magnesium sulfate, 0.8g of nickel sulfate hexahydrate, and 1.03g of manganese sulfate monohydrate into the prepared cobalt liquid, then add complexing agent EDTA into the cobalt liquid, and mix well, the molar ratio of complexing agent EDTA to Co ions 0.19%; prepare 9mol / L sodium hydroxide solution for subsequent use;

[0026] 2. Wet synthesis: add hot pure water to the reaction kettle in advance, adjust the pH to 11.5, then pump the cobalt liquid, sodium hydroxide solution and compressed air prepared in step 1 into the reaction kettle at the same time, and synthesize at a temperature of 78°C and The synthesis reaction is carried out at a stirring speed of 360r / min, and 100L / h of compressed air is introduced, and the pH of the sy...

Embodiment 2

[0030] 1. Prepare the solution: take the cobalt sulfate solution produced in the extraction process and dilute it to a concentration of 2mol / L with hot pure water; weigh 11.8g of the doping element aluminum sulfate octadecahydrate and heptahydrate for each liter of cobalt solution Add 2.36g of magnesium sulfate, 0.89g of nickel sulfate hexahydrate, and 1.2g of manganese sulfate monohydrate into the prepared cobalt liquid, then add complexing agent EDTA into the cobalt liquid, and mix well, the mole of complexing agent EDTA and Co ions The ratio is 0.3%; prepare 5mol / L sodium hydroxide solution for subsequent use;

[0031]2. Wet synthesis: add hot pure water to the reaction kettle in advance, adjust the pH to 11.5, then pump the cobalt liquid, sodium hydroxide solution and compressed air prepared in step 1 into the reaction kettle at the same time, and synthesize at a synthesis temperature of 78°C Carry out the synthesis reaction, the stirring speed is gradually reduced from 36...

Embodiment 3

[0035] 1. Prepare the solution: take the cobalt sulfate solution produced in the extraction process, dilute it to a concentration of 1.7mol / L with hot pure water; weigh 12.5g of doping element aluminum sulfate octadecahydrate, seven Add 1.9g of magnesium sulfate water, 0.75g of nickel sulfate hexahydrate, and 1g of manganese sulfate monohydrate into the prepared cobalt liquid, then add complexing agent EDTA into the cobalt liquid, mix well, and complex The molar ratio of agent EDTA and Co ion is 0.15%; Prepare 12mol / L sodium hydroxide solution for subsequent use;

[0036] 2. Wet synthesis: add hot pure water to the reaction kettle in advance, adjust the pH to 11.5, then pump the cobalt liquid, sodium hydroxide solution and compressed air prepared in step 1 into the reaction kettle at the same time, at a synthesis temperature of 62°C Carry out the synthesis reaction, the stirring speed is 380r / min, and the compressed air is 90L / h, and the pH of the synthesis process is controll...

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Abstract

The invention belongs to the technical field of preparing precursor of battery positive electrode material, in particular to a preparation method of doped cobalt tetroxide, and provides a preparationmethod of aluminum-magnesium-nickel-manganese doped spherical cobalt tetroxide. Cobalt liquid containing doped elements is prepared, EDTA is used as a complexing agent and synthesis is performed at acertain pH and temperature. Meanwhile, the doped elements are uniformly and fully precipitated, and finally the high-density spherical cobalt hydroxide with uniform doping is obtained and the doped cobalt tetroxide is obtained through centrifugation and calcination. The aluminum-magnesium-nickel-manganese doped spherical cobalt tetroxide prepared by the method has uniform particle size, good compactness, complete precipitation and uniform distribution of doped elements and stable and controllable process.

Description

technical field [0001] The invention relates to the technical field of battery material preparation, in particular to a method for preparing doped spherical tricobalt tetroxide. Background technique [0002] With the upgrading of products in the 3C field and the rapid development of various high-end smart devices, the requirements for thinner, lighter and higher capacity batteries are getting higher and higher. On the one hand, it is necessary to increase the compacted density of the material, and on the other hand, higher requirements are placed on the gram specific capacity of lithium cobalt oxide. Different elements play different roles on the structure of lithium cobaltate: Mg element is an element that was used earlier for doping improvement research. Tukamoto et al. pointed out that doping a small amount of divalent element Mg in lithium cobalt oxide can improve the electrical conductivity of the material without changing the crystal structure, and at the same time, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/46H01M4/505H01M4/525
CPCH01M4/364H01M4/463H01M4/505H01M4/525Y02E60/10
Inventor 夏勇田礼平刘人生张荣洲秦才胜
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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