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Preparation method of niobium, tungsten and tantalum-doped cobalt trioxide

A technology of cobalt tetroxide and cobalt hydroxide, applied in the direction of cobalt oxide/cobalt hydroxide, can solve the problems of uneven precipitation, low production efficiency, easy hydrolysis, etc., and achieve the effect of promoting rapid growth and improving production efficiency

Active Publication Date: 2018-08-28
LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when this method is used to prepare niobium, tungsten, and tantalum tricobalt tetroxide doped with high-valence and large atomic weight elements, there is the problem that niobium, tungsten, and tantalum chloride are easily hydrolyzed as wet dopants, resulting in the formation of niobium, tungsten, and tantalum elements. The precipitation is not uniform, which leads to the problem of uneven distribution of doping elements in cobalt tetroxide
In addition, the cobalt compound is very easy to oxidize, and the oxidized cobalt compound will hinder the rapid growth of the synthetic product. Therefore, this method also has the problem of low production efficiency.

Method used

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  • Preparation method of niobium, tungsten and tantalum-doped cobalt trioxide
  • Preparation method of niobium, tungsten and tantalum-doped cobalt trioxide

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Effect test

Embodiment 1

[0032] Prepare a cobalt chloride solution with a concentration of 1mol / L as solution A; prepare a sodium hydroxide solution with a concentration of 2mol / L as solution B; prepare an ammonia solution with a concentration of 5mol / L, and add 5mL volume fraction per liter of ammonia solution The 30% hydrazine hydrate solution is the C solution; the hydrogen peroxide solution with a concentration of 5mol / L is prepared as the D solution; the niobium pentachloride absolute ethanol solution with a concentration of 4g / L is prepared as the E solution.

[0033] At the beginning of the synthesis reaction, the A solution, the B solution and the C solution flow into the reactor simultaneously, and at the same time, the E solution feeding pipe is divided into 6-9 small pipes, and the liquid outlet of each fine feeding pipe is fixed to the reactor for stirring Add E solution to the middle or tail of the paddle, and react under the stirring state of 500r / min. Adjustment, the flow rate of soluti...

Embodiment 2

[0038] Prepare a cobalt sulfate solution with a concentration of 1.5mol / L as solution A; prepare a sodium hydroxide solution with a concentration of 4mol / L as solution B; prepare an ammonia solution with a concentration of 8mol / L, and add 15mL volume fraction per liter of ammonia solution A 30% hydrazine hydrate solution is solution C; a hydrogen peroxide solution with a concentration of 6mol / L is prepared as solution D; a tungsten hexachloride absolute ethanol solution with a concentration of 6g / L is prepared as solution E.

[0039]At the beginning of the synthesis reaction, the A solution, the B solution and the C solution flow into the reactor simultaneously, and at the same time, the E solution feeding pipe is divided into 6-9 small pipes, and the liquid outlet of each fine feeding pipe is fixed to the reactor for stirring Add E solution to the middle or tail of the paddle, and react under the stirring state of 400r / min. The pH value of the reaction was adjusted, the flow ...

Embodiment 3

[0044] Prepare the cobalt nitrate solution with a concentration of 2mol / L as solution A; prepare the sodium hydroxide solution with a concentration of 6mol / L as solution B; The 30% hydrazine hydrate solution is solution C; the hydrogen peroxide solution with a concentration of 8 mol / L is prepared as solution D; the tantalum pentachloride absolute ethanol solution with a concentration of 8 g / L is prepared as solution E.

[0045] At the beginning of the synthesis reaction, the A solution, the B solution and the C solution flow into the reactor simultaneously, and at the same time, the E solution feeding pipe is divided into 6-9 small pipes, and the liquid outlet of each fine feeding pipe is fixed to the reactor for stirring Add E solution to the middle or tail of the paddle, and react under the stirring state of 300r / min. The pH value of the reaction was adjusted, the flow rate of solution C was 60 L / h, the flow rate of solution E was 30 L / h, and the reaction time was 20 h to ob...

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Abstract

The invention discloses a preparation method of niobium, tungsten and tantalum-doped cobalt trioxide and belongs to the technical field of lithium ion batteries. The preparation method is characterized in that the synthetic reaction is performed by taking a certain concentration of cobalt solution as a cobalt source, a sodium hydroxide solution as a precipitating agent, an ammonia aqueous solutionas a complexing agent, a hydrazine hydrate solution as a reducing agent and a niobium, tungsten and tantalum chloride anhydrous alcohol solution as a doping agent; in the reaction process, the niobium, tungsten and tantalum chloride anhydrous alcohol solution is added in a reaction kettle in a dispersive liquid adding manner to participate in the reaction; after the end of the synthetic reaction,a synthetic product is oxidized into hydroxyl cobalt oxide by utilizing a hydrogen peroxide solution under the condition of a certain pH value, and then a mixture is washed, dried and calcined to obtain a niobium, tungsten and tantalum-doped cobalt trioxide product with uniformly-distributed doped elements; the production efficiency is high. The niobium, tungsten and tantalum-doped cobalt trioxide product prepared by the preparation method disclosed by the invention has a doping amount of 0.5-1 percent, has the uniformly-distributed doped elements, has a laser particle size of 15-20 mum, a tap density of more than or equal to 2.5 g / cm<3> and a specific surface area of 1.0-3.0 m<2> / g and has a massive or nearly-spherical appearance.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a method for preparing niobium-doped tungsten-tantalum tricobalt tetroxide used for preparing lithium cobalt oxide, a cathode material of lithium-ion batteries. Background technique [0002] The lithium-ion battery prepared with lithium cobaltate as the positive electrode material has the characteristics of light weight, large capacity, high specific energy, high working voltage, stable discharge, suitable for high current discharge, good cycle performance, and long life. It is mainly used in 3C digital field. [0003] Lithium cobalt oxide is developing in the direction of high voltage, high compaction, and high cycle performance. Therefore, the requirements for the raw material cobalt tetroxide are getting higher and higher. co 3 o 4 It is a functional material with special structure and properties, conventional Co 3 o 4 The market is already facing the status...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
CPCC01G51/04C01P2004/30C01P2004/32C01P2004/61C01P2006/11C01P2006/12C01P2006/80
Inventor 王树亮陈晓闯王红忠刘世红吴来红赵宗明李俊杰杜江何艳
Owner LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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