Preparation method of high-density granulated nickel-cobalt-manganese hydroxide

A technology of hydroxide and nickel-cobalt-manganese, applied in nickel compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as poor sphericity, difficulty in preparation, poor particle sphericity, etc., to reduce production costs and process flow The effect of simplicity and good crystallization properties

Active Publication Date: 2018-07-10
BEIJING EASPRING MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Due to the small particle size, easy agglomeration, and poor sphericity of small particle nickel cobalt manganese hydroxide, it brings great difficulties to the preparation
Chinese patent CN103253717A adds the surfactant trisodium citrate or citric acid into the salt solution, and at the same time adds the dispersant polyethylene glycol or polyvinyl alcohol into the alkali solution to prepare small particles with a median particle size of 1.0-5.0 μm Nickel-cobalt-manganese hydroxide, but the sphericity of the particles is slightly poor and the particles are relatively loose from the electron microscope image, which is not suitable for the preparation of high-density nickel-cobalt lithium manganate cathode materials
In addition, this method is a typical batch production process, each time all the materials in the kettle are discharged, and the bottom liquid is added again for synthesis, and the product reproducibility is poor
In addition, in order to obtain crystal nuclei with small particle sizes, a higher stirring speed is used in the production of crystal nuclei, and a lower stirring speed is used in the particle size growth stage, which may lead to stratification or faults inside the particles.
In addition, this method uses a low temperature of 30-45°C in the stage of producing crystal nuclei and particle size growth, which is not conducive to improving the crystallization performance of nickel-cobalt-manganese hydroxide, and the obtained product contains high impurities such as S and Na, which will affect the prepared nickel. Processability and Electrical Properties of Cobalt Lithium Manganese Oxide Cathode Material

Method used

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  • Preparation method of high-density granulated nickel-cobalt-manganese hydroxide
  • Preparation method of high-density granulated nickel-cobalt-manganese hydroxide
  • Preparation method of high-density granulated nickel-cobalt-manganese hydroxide

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Embodiment 1

[0031] Using nickel sulfate, cobalt sulfate, and manganese sulfate as raw materials, configure a 2mol / L uniform nickel, cobalt, and manganese salt mixed solution in a molar ratio of 4:3:3. The liquid caustic soda with a mass fraction of 32% is configured into 5 mol / L lye as a precipitant, and the ammonia water with a mass fraction of 25% is configured into 5 mol / L as a complexing agent for use.

[0032]Add pure water to the reactor to the position of the overflow pipe to make the bottom liquid, stir at 500rpm, after the temperature in the reactor rises to 50°C, under the condition of feeding nitrogen, the mixed salt Solution, alkaline solution, and ammonia solution are fed into the reactor in parallel for reaction. During the reaction, the slurry was taken to test the reaction pH value, ammonia content and particle size. During the reaction process, the pH value was controlled to be 11.6, the ammonia content was 0.7 g / L, and nickel-cobalt-manganese hydroxide with a thickness ...

Embodiment 2

[0034] Using nickel sulfate, cobalt sulfate, and manganese sulfate as raw materials, it is configured into a 1.7mol / L uniform nickel, cobalt, and manganese salt mixed solution at a molar ratio of 5:2:3. The liquid caustic soda with a mass fraction of 32% is configured into 8 mol / L lye as a precipitating agent, and the ammonia water with a mass fraction of 25% is configured into 8 mol / L as a complexing agent for use.

[0035] Add pure water to the reactor to the position of the overflow pipe to make the bottom liquid, the stirring speed is 600rpm, after the temperature in the reactor rises to 55°C, under the condition of feeding nitrogen, the mixed salt Solution, alkaline solution, and ammonia solution are fed into the reactor in parallel for reaction. During the reaction, the slurry was taken to test the reaction pH value, ammonia content and particle size. During the reaction process, the pH value was controlled to be 11.9, the ammonia content was 1.3 g / L, and nickel-cobalt-...

Embodiment 3

[0037] Using nickel sulfate, cobalt sulfate, and manganese sulfate as raw materials, it is configured into a 1.7mol / L uniform nickel, cobalt, and manganese salt mixed solution at a molar ratio of 6:2:2. The liquid caustic soda with a mass fraction of 32% is configured into 10 mol / L lye as a precipitating agent, and the ammonia water with a mass fraction of 25% is configured into 8 mol / L as a complexing agent for use.

[0038] Add pure water to the reactor to the position of the overflow pipe to make the bottom liquid, the stirring speed is 600rpm, after the temperature in the reactor rises to 60°C, under the condition of feeding nitrogen, the mixed salt Solution, alkaline solution, and ammonia solution are fed into the reactor in parallel for reaction, and the slurry is taken during the reaction to test the reaction pH value, ammonia content and particle size. During the reaction process, the pH value was controlled to be 12.2, the ammonia content was 2.2 g / L, and nickel-cobal...

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Abstract

The invention relates to a method for continuously preparing high-density granulated nickel-cobalt-manganese hydroxide. Technological parameters are optimized, proper conditions such as liquid feedingtime, ammonia content, temperature, pH (potential of hydrogen) and stirring speed are selected, liquid is continuously fed, deposition is performed, and overflowing liquid is filtered, washed and dried to prepare the nickel-cobalt-manganese hydroxide which is spherical or near-spherical single particles. D50 is 3.0-5.0 micrometers, apparent density (AD) is higher than or equal to 1.2g / cm<3>, tapdensity (TD) is higher than or equal to 1.8g / cm<3>, S<=1200ppm, and Na<=200ppm. According to the method, surface active agents and dispersing agents are not added in the preparation process, crystal nucleuses do not need to be manufactured in advance, production efficiency and product consistency are improved, and the prepared product is good in crystallization property and low in impurity content.

Description

technical field [0001] The invention belongs to the technical field of precursors for positive electrode materials of lithium ion batteries, and in particular relates to a method for continuously preparing high-density small-particle nickel-cobalt-manganese hydroxides. Background technique [0002] Lithium-ion batteries have outstanding advantages such as high energy density, long cycle life, low self-discharge rate, no memory effect, and environmental protection. They are new green secondary batteries successfully developed in the 1990s. Lithium-ion batteries are mainly composed of positive electrode materials, negative electrode materials, electrolytes, diaphragms, etc. The positive electrode material is the most expensive part of lithium-ion batteries, and it is also a key factor that restricts the development of batteries to higher performance. [0003] At present, the main positive electrode materials on the market include lithium cobalt oxide, lithium manganese oxide, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/50H01M4/52
CPCC01G53/006C01P2002/72C01P2004/03C01P2004/51C01P2004/61C01P2006/11C01P2006/80H01M4/50H01M4/52Y02E60/10
Inventor 张朋立宋顺林姚静郑长春
Owner BEIJING EASPRING MATERIAL TECH CO LTD
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