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Manganese sesquioxide micro powder and preparation method and application thereof

A technology of manganese trioxide micropowder and divalent manganese salt, which is applied in the direction of manganese oxide/manganese hydroxide, electrical components, battery electrodes, etc., and can solve the problems of negative impact on the safety performance of lithium-ion battery products, waste of raw materials, high impurity content, etc. , to achieve the effect of uniform and controllable product particle size, full utilization of resources, and low impurity content

Active Publication Date: 2014-04-02
贵州大龙汇成新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Accordingly, when electrolytic manganese dioxide is used as a precursor to prepare lithium manganate, there will be the following three problems: 1) The cost is high, for example, the electricity consumption in the electrolysis process needs to be 8000 kWh / ton, and the crushed The selection will result in a large proportion of waste of raw materials; 2) The morphology, specific surface area, particle size and distribution of powder materials cannot be effectively controlled, which will further affect the electrochemical performance of lithium manganate materials; 3) High impurity content , for example, the sulfate radical content contained in the product is generally as high as 1.3%, and elemental iron will be brought in during the crushing process, which will have a negative impact on the safety performance of lithium-ion battery products
[0006] Most of the existing manganese trioxide is prepared by roasting manganese salts such as manganese oxalate and manganese carbonate, but the commercially available manganese oxalate is generally prepared by the reaction of manganese salt and sodium oxalate, which has high sodium content and many impurities; Manganese is generally produced by the direct reaction of manganese sulfate and ammonium bicarbonate, etc., but the obtained manganese carbonate product has fluffy and relatively coarse particles, is not easy to rinse clean, and contains more sulfate radicals; it can be seen that the manganese salt roasted by the above Manganese cannot meet the requirements of modern lithium-ion battery materials and magnetic materials

Method used

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  • Manganese sesquioxide micro powder and preparation method and application thereof
  • Manganese sesquioxide micro powder and preparation method and application thereof
  • Manganese sesquioxide micro powder and preparation method and application thereof

Examples

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Embodiment 1

[0044] A kind of manganese trioxide micropowder of the present invention, the particle size index D50 of manganese trioxide micropowder is 9.2 μm, bulk density is 0.6g / mL, tap density is 1.2g / mL, Mn content is 69.2%, Ca element The content is 52ppm, the Mg element content is 48ppm, and the sulfate content is 236ppm.

[0045] The preparation method of above-mentioned manganese trioxide micropowder in the present embodiment specifically comprises the following steps:

[0046] (1) Prepare 1L of manganese sulfate solution with a metal manganese content of 145g / L, prepare 1L of oxalic acid solution with a concentration of 332g / L; prepare ammonia water with a mass fraction of 15%;

[0047] (2) Add 1L of pure water into an 8L reactor as the reaction bottom liquid, stir and heat up to 60°C, and at a temperature of 60°C and under stirring conditions, add the above-mentioned preparation at the same time continuously and at a uniform speed according to the stoichiometric ratio of 1:1. M...

Embodiment 2

[0052] A kind of manganese trioxide micropowder of the present invention, the particle size index D50 of manganese trioxide micropowder is 20.3 μm, bulk density is 0.8g / mL, tap density is 1.3g / mL, Mn content is 68.9%, Ca element The content is 39ppm, the Mg element content is 43ppm, and the sulfate content is 218ppm.

[0053] The preparation method of above-mentioned manganese trioxide micropowder in the present embodiment specifically comprises the following steps:

[0054] (1) Prepare 1L of manganese sulfate solution with a metal manganese content of 55g / L, prepare 1L of oxalic acid solution with a concentration of 126g / L; prepare 200g / L ammonium bicarbonate solution;

[0055] (2) Add 1L of pure water into the 8L reactor as the reaction bottom liquid, stir and heat up to 40°C, at the temperature of 40°C and under stirring conditions, add the above-mentioned preparation at the same time continuously and at a uniform speed according to the stoichiometric ratio of 1:1 Manganes...

Embodiment 3

[0060] A kind of manganese trioxide micropowder of the present invention, the particle size index D50 of manganese trioxide micropowder is 13.2 μm, bulk density is 1.0g / mL, tap density is 1.4g / mL, Mn content is 69.4%, Ca element The content is 47ppm, the Mg element content is 42ppm, and the sulfate content is 208ppm.

[0061] The preparation method of above-mentioned manganese trioxide micropowder in the present embodiment specifically comprises the following steps:

[0062] (1) Prepare a manganese sulfate solution with a metal manganese content of 110g / L, prepare an oxalic acid solution with a concentration of 250g / L (preheated to 60°C); prepare a 240g / L ammonium bicarbonate solution;

[0063] (2) Add about 30L of pure water into a 200L reactor as the reaction bottom liquid, stir and heat up to 60°C, at a temperature of 60°C and under stirring conditions, add the above preparation at the same time continuously and at a uniform speed according to the stoichiometric ratio of 1:...

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Abstract

The invention discloses manganese sesquioxide micro powder of which the D50 is 3-30 micrometer, the apparent density is 0.5-1.5 g / mL, the tap density is 1.0-2.5 g / mL, content of Mn is higher than 68%, contents of Ca and Mg are both lower than 100ppm, and content of sulfate radical is less than 500ppm. A preparation method comprises continuously adding a divalent manganese salt solution and oxalic acid at the same time at certain temperature under a stirring condition, then continuously adding ammonium hydroxide or ammonium bicarbonate when the pH value is lower than 5.0, to maintain a reaction system to be faintly acid, preserving heat and stirring until the reaction is finished after the reaction liquid is finished adding and the pH value is raised to about neutral, finally conducting solid liquid separation on a product, rinsing for multiple times, then roasting, cooling, crushing and sieving to obtain the product. The manganese sesquioxide micro powder is small and even, controllable in granularity, low in content of impurities and high in purity, and can be used as a precursor to prepare lithium manganate or soft magnetic ferrite for a lithium battery.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to an oxide micropowder material and a preparation method thereof, in particular to a manganese trioxide micropowder for lithium ion batteries or soft magnetic ferrite and a preparation method thereof. Background technique [0002] Manganese oxide has many uses, among which, the preparation of lithium-ion battery materials and magnetic materials is an important application in the field of modern new energy and new electronic materials. [0003] Lithium manganese oxide is one of the candidate materials for power batteries for new energy vehicles due to its abundant resources and low price. At present, the production of lithium manganese oxide is generally made of electrolytic manganese dioxide as raw material, which is mixed with lithium carbonate and then roasted. However, the production of electrolytic manganese dioxide is to obtain a block on the anode by electrolyzing mangane...

Claims

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Application Information

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IPC IPC(8): H01M4/50C01G45/02
CPCC01G45/02H01M4/502Y02E60/10
Inventor 周婷婷刘务华彭天剑
Owner 贵州大龙汇成新材料有限公司
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