Preparation method of low-sulfur compact crystal form cobalt carbonate

A cobalt carbonate and cobalt sulfate solution technology, which is applied in the direction of cobalt carbonate, can solve the problems of production efficiency and other problems, and achieve the effect of dense crystal form and low specific surface area

Inactive Publication Date: 2020-07-17
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The "Preparation Method of Low Sodium Cobalt Tetroxide" disclosed by Jingmen GEM New Material Co., Ltd., and the "Preparation Method and Device of Low Sodium Cobalt Tetroxide" disclosed by Jiangsu Kailike Cobalt Industry Co., Ltd. reduce the sodium impurity in the product by backwashing the Cobalt Tetroxide system content, but the backwashing process will have a certain impact on production efficiency

Method used

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  • Preparation method of low-sulfur compact crystal form cobalt carbonate
  • Preparation method of low-sulfur compact crystal form cobalt carbonate
  • Preparation method of low-sulfur compact crystal form cobalt carbonate

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Experimental program
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Effect test

Embodiment 1

[0028] Step 1. Preparation of solutions: prepare a cobalt sulfate solution with a concentration of 1.2 mol / L, and prepare an ammonium bicarbonate solution with a concentration of 2.5 mol / L.

[0029] Step 2. Synthesis of seed crystals: inject the ammonium bicarbonate solution prepared in step 1 into the reactor as the bottom liquid, the volume of the bottom liquid accounts for 0.06% of the reactor, and the pH value of the bottom liquid is controlled to 8.3; 1. The prepared cobalt sulfate solution was pumped into the reaction kettle separately, the feeding time was 2 hours, the feeding flow rate was 20mL / min, the synthesis temperature was 38°C, and the final pH range was 7.9, and cobalt carbonate seeds were synthesized with a particle size of 2.5 μm;

[0030] Step 3. Growth and synthesis: the above-mentioned cobalt carbonate seed crystals are placed in the reactor to continue to grow, the stirring speed is 280rpm, the corresponding cobalt liquid flow rate of the 50L reactor is 10...

Embodiment 2

[0037] Step 1. Prepare the solution: prepare an aluminum-doped cobalt sulfate solution with a concentration of 2.2 mol / L, wherein the mass ratio of aluminum element to cobalt element in the cobalt liquid is 0.0125, and prepare an ammonium bicarbonate solution with a concentration of 2.9 mol / L.

[0038] Step 2, synthesis of seed crystals: inject the ammonium bicarbonate solution prepared in step 1 into the reactor as the bottom liquid, the volume of the bottom liquid accounts for 0.20% of the reactor, and the pH value of the bottom liquid is controlled to be 8.6; The cobalt sulfate solution prepared in step 1 was pumped into the reaction kettle separately, the feeding time was 2 hours, the feeding flow rate was 25mL / min, the synthesis temperature was 42°C, and the final pH range was 7.8, and cobalt carbonate seeds were synthesized with a particle size of 1.5 μm;

[0039] Step 3. Growth and synthesis: the above-mentioned cobalt carbonate seed crystals are placed in the reactor to...

Embodiment 3

[0047] Step 1, preparing the solution: preparing the cobalt sulfate solution with a concentration of 1.8 mol / L, and preparing the ammonium bicarbonate solution with a concentration of 2.8 mol / L.

[0048] Step 2, synthesis of seed crystals: inject the ammonium bicarbonate solution prepared in step 1 into the reactor as the bottom liquid, the volume of the bottom liquid accounts for 0.1% of the reactor, and the pH value of the bottom liquid is controlled to be 8.4; The cobalt sulfate solution prepared in step 1 was pumped into the reaction kettle separately, the feeding time was 2 hours, the feeding flow rate was 25mL / min, the synthesis temperature was 40°C, and the final pH range was 8.2, and cobalt carbonate seeds were synthesized with a particle size of 2.5 μm;

[0049] Step 3. Growth and synthesis: the above-mentioned cobalt carbonate seed crystals are placed in the reactor to continue to grow, the stirring speed is 300rpm, the corresponding cobalt liquid flow rate of the 50L...

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Abstract

The invention relates to the technical field of battery material preparation, in particular to a preparation method of low-sulfur compact crystal form cobalt carbonate. The compact crystal form cobaltcarbonate prepared by the method has a relatively low specific surface area, and the specific surface area of the particles is reduced and the quantity of impurity sulfur attachment sites is reducedby improving the crystal density of the particles and reducing the quantity of micropores or mesopores in the particles, so that the tap density of the cobalt carbonate particles is improved, and thecontent of impurities can be reduced; the proper feeding molar ratio of cobalt salt to ammonium bicarbonate in the synthesis process not only provides enough carbonate ions for precipitation reaction,but also avoids the increase of hydroxide radicals in the solution and the formation of sulfate radical-containing basic carbonate due to the decomposition of excessive ammonium bicarbonate at high temperature.

Description

technical field [0001] The invention relates to the technical field of battery material preparation, in particular to a method for preparing low-sulfur dense crystalline cobalt carbonate. Background technique [0002] With the upgrading of 3C products, the requirements for lithium-ion batteries are getting higher and higher, and the control of impurity content of cobalt tetroxide, which is the precursor of lithium batteries, is becoming increasingly strict. Cobalt tetroxide is an important raw material for the preparation of lithium cobalt oxide, the positive electrode material of lithium batteries, and its performance in various aspects determines the performance of lithium cobalt oxide positive electrode materials and downstream lithium ion batteries. The preparation of highly dense cobalt tetroxide has also become a research hotspot. Lithium cobalt oxide cathode material manufacturers have increasingly strict requirements on the sphericity and tap density of small-sized ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/06
CPCC01G51/06C01P2004/61C01P2006/12C01P2006/80C01P2006/11
Inventor 夏勇田礼平刘人生胡招文祝婷
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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