Battery grade high-purity manganese sulfate monohydrate and preparation method thereof

A manganese sulfate, battery-grade technology, applied in the direction of manganese sulfate, etc., can solve the problems of inconvenient production and corrosion effects of equipment, and achieve the effects of reducing corrosion effects, low economic cost, and wide sources

Inactive Publication Date: 2013-02-13
HUNAN SPECIAL METAL MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the addition of fluoride will introduce fluorine impurities, if the fluorine content is too high, reaching the level of 1000ppm, it will have a corrosion effect on the equipment and

Method used

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  • Battery grade high-purity manganese sulfate monohydrate and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation method of battery grade high-purity manganese sulfate monohydrate of the present invention comprises the following steps, and its process flow chart is as follows figure 1 shown.

[0042] (1) Weigh 600g of pyrolusite containing 25% manganese, 200g of pyrolusite, and 4.0L of water, stir evenly, slowly add 200ml of industrial sulfuric acid, heat up to 100°C within 30min, react for 4h, pH is 2, slowly add 40g of CaCO 3 , the pH at the end of the reaction is 4, and the manganese sulfate filtrate 1 is obtained by filtration;

[0043] (2) Add 2ml of hydrogen peroxide to filtrate 1, control the temperature at 50°C, oxidize and hydrolyze for 2 hours, stand and filter to obtain filtrate 2;

[0044] (3) Weigh 5g of BaS, dissolve in 50ml of distilled water, boil and filter to obtain BaS hydrolysis filtrate, add this BaS hydrolysis filtrate to filtrate 2, control the temperature at 50°C, stir for 2 hours, and obtain filtrate 3 by filtration;

[0045] (4) Add 8ml o...

Embodiment 2

[0051] The preparation method of battery grade high-purity manganese sulfate monohydrate of the present invention comprises the following steps, and its process flow chart is as follows figure 1 shown.

[0052] (1) Weigh 640g of pyrolusite containing 25% manganese, 160g of pyrite, and 4.5L of water, stir evenly, slowly add 220ml of industrial sulfuric acid, heat up to 90°C within 35min, react for 6h, pH is 2.5, slowly add 50g of CaCO 3 , the pH at the end of the reaction is 4.5, and the manganese sulfate filtrate 1 is obtained by filtration;

[0053] (2) Add 6ml of hydrogen peroxide to the filtrate 1, control the temperature at 60°C, oxidize and hydrolyze for 2 hours, stand and filter to obtain the filtrate 2;

[0054] (3) Weigh 4g of BaS, dissolve in 60ml of distilled water, boil and filter to obtain the BaS hydrolysis filtrate, add the BaS hydrolysis filtrate to the filtrate 2 at a temperature of 45°C, stir for 1 hour, and filter to obtain the filtrate 3;

[0055] (4) Add ...

Embodiment 3

[0061] The preparation method of battery grade high-purity manganese sulfate monohydrate of the present invention comprises the following steps, and its process flow chart is as follows figure 1 shown.

[0062] (1) Weigh 1000g of pyrolusite containing 18% manganese, 200g of pyrolusite, and 4.5L of water, stir evenly, slowly add 280ml of industrial sulfuric acid, heat up to 95°C within 30min, react for 5h, pH is 2.2, slowly add 80g of CaCO 3 , the pH at the end of the reaction is 4, and the manganese sulfate filtrate 1 is obtained by filtration;

[0063] (2) Add 10ml of hydrogen peroxide to filtrate 1, control the temperature at 70°C, oxidize and hydrolyze for 1 hour, stand and filter to obtain filtrate 2;

[0064] (3) Weigh 5g of BaS, dissolve it in 60ml of distilled water, boil and filter to obtain the BaS hydrolysis filtrate, add the BaS hydrolysis filtrate to the filtrate 2, control the temperature at 30°C, stir for 1.5h, and filter to obtain the filtrate 3;

[0065] (4) ...

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Abstract

The invention relates to battery grade high-purity manganese sulfate monohydrate and a preparation method thereof. The content of the high-purity manganese sulfate monohydrate is over 32 percent, the contents of all impurities potassium, sodium, calcium and magnesium are less than 50 ppm, the content of heavy metal impurity is below 10 ppm, the content of impurity ferro is below 5 ppm, and the content of impurity fluorine is below 100 ppm. The preparation method comprises the following steps: gray manganese ore, manganese blende or sulfurous iron ore and industrial sulphuric acid are taken as the raw materials, hydrogen peroxide is added firstly, and the temperature is controlled within 50-70 DEG C; secondly, BaS is added, and the temperature is controlled within 30-50 DEG C; thirdly, hydrofluoric acid is added, and the pH is regulated to 5-6 by adding a neutralizing agent MnCO3; fourthly, polyaluminum sulfate and polyacrylamide solution are added to flocculate and deposit, activated carbon is added after filter, and standing and absorption are carried out; fifthly, polyaluminum sulfate and polyacrylamide solution are introduced into a circulation device equipped with an active alumina ball; and lastly, the high-impurity manganese sulfate is obtained via non-pressurized compaction and crystallization, washing and drying. The manganese content of the manganese sulfate monohydrate is high, the contents of each metal impurity and fluorine are lower, and the demand for the positive pole material of lithium ion batteries is completely satisfied.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a battery-grade high-purity manganese sulfate monohydrate and a preparation method thereof. Background technique [0002] As a new generation of environmentally friendly and high-performance batteries, lithium-ion batteries have become one of the key directions for the development of the battery industry. Lithium batteries are mainly composed of positive electrode materials, negative electrode materials, separators and electrolytes, and lithium battery positive electrode materials are its core key materials. In the cost of lithium battery raw materials, the positive electrode material accounts for more than 40% of the manufacturing cost, and the positive electrode material is the source of lithium ions in the battery, and its performance directly affects the various performance indicators of the lithium battery. Occupying the core position, it is the most critical functional m...

Claims

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Application Information

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IPC IPC(8): C01G45/10
Inventor 陈飞宇赵凯银瑰许定胜文平
Owner HUNAN SPECIAL METAL MATERIALS CO LTD
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