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Manufacturing method of ultra-pure battery-grade manganese chloride for battery material

A battery material and manufacturing method technology, applied in the direction of manganese halide, etc., can solve the problems that manganese lithium batteries cannot be used, the purity of manganese chloride products is not high, and the product quality cannot meet the requirements of battery-grade products, and achieve high purity and appearance. The effect of bright colors and high cycle performance

Active Publication Date: 2012-07-18
HUBEI HAOYUAN MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even if the content of Ca, Mg impurities and heavy metal impurities (Co, Ni, Pb, etc.) can be reduced with general impurity removers, the purity of the prepared manganese chloride product is still not high, and the product quality cannot reach that of battery-grade products. requirements, so it cannot be used as raw material for manganese-lithium batteries

Method used

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  • Manufacturing method of ultra-pure battery-grade manganese chloride for battery material
  • Manufacturing method of ultra-pure battery-grade manganese chloride for battery material

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 500gMnCO 3 Add 800~1000ml of 30% hydrochloric acid to dissolve, heat and stir to raise the temperature to 80°C, add 20g of hydrofluoric acid or fluoride or phosphoric acid or phosphate or polyphosphoric compounds to remove Ca and Mg, keep the pH value of the solution at 2.0~5.0, and keep warm under stirring React for 1 hour, then add sulfide or polysulfide to remove Co, Ni, Pb, Cd, Cr heavy metal impurities, keep the pH value at 4.5~5.5, stir and keep warm for 0.5 hour, filter. Return the filtrate to the iron removal reactor, control the Baume degree at 30~53 °Be', control the temperature at 30~120°C, add peroxide or hydrogen peroxide and 10 g of activated carbon, control the pH at 2.5~5.5, and react 1 hour, filtered, and the filtrate was concentrated, crystallized, and dehydrated to obtain 560g of a high-purity manganese chloride product. According to ICP detection, calcium in the obtained manganese chloride is 20.79 ppm, magnesium is 13.74 ppm, nickel is less than 20...

Embodiment 2

[0030] Add 1500~2000ml of 30% hydrochloric acid to 500g of manganese metal, heat and stir to raise the temperature to 80°C, add 20g of hydrofluoric acid or fluoride or phosphoric acid or phosphate or polyphosphorus compound to remove Ca and Mg, keep the pH value of the solution at 2.0~5.0, stir Under heat preservation reaction for 1 hour, then add sulfide or polysulfide to remove Co, Ni, Pb, Cd, Cr heavy metal impurities, keep the pH value at 4.5~5.5, stir and heat preservation reaction for 0.5 hour, and filter. Return the filtrate to the iron removal reactor, control the Baume degree at 30-53 °Be', control the temperature at 30-120 °C, add activated carbon and peroxide or hydrogen peroxide, control the pH at 2.5-5.5, and react for 1 hour , filtered, and the filtrate was concentrated, crystallized, and dehydrated to obtain 1560 g of a high-purity manganese chloride product. According to ICP detection, calcium in the obtained manganese chloride is 10.63 ppm, magnesium is 5.59 p...

Embodiment 3

[0036]Add 3000~4000ml of 30% hydrochloric acid to 1000g manganese metal, heat and stir to raise the temperature to 80°C, add 40g of hydrofluoric acid or fluoride or phosphoric acid or phosphate or polyphosphorus compound to remove Ca and Mg, keep the pH value of the solution at 2.0~5.0, stir Under heat preservation reaction for 1 hour, then add sulfide or polysulfide to remove Co, Ni, Pb, Cd, Cr heavy metal impurities, keep the pH value at 4.5~5.5, stir and heat preservation reaction for 0.5 hour, and filter. Return the filtrate to the iron removal reactor, control the Baume degree at 30-53 °Be', control the temperature at 30-120 °C, add activated carbon and peroxide or hydrogen peroxide, control the pH at 2.5-5.5, and react for 1 hour , filtered, and the filtrate was concentrated, crystallized, and dehydrated to obtain 3047g of a high-purity manganese chloride product. According to ICP detection, calcium in the obtained manganese chloride is 10.63 ppm, magnesium is 5.59 ppm, ...

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Abstract

The invention relates to a manufacturing method of ultra-pure battery-grade manganese chloride for a battery material, which comprises the following steps that: manganese chloride solution which is prepared by leaching ordinary manganese carbonate or metal manganese with high impurity content through hydrochloric acid is added with hydrofluoric acid, fluoride, phosphoric acid, phosphate salt or polyphosphoric compound to remove calcium (Ca) and magnesium (Mg), sulfide, polysulfide or sulfuric organic sodium salt is used for removing heavy metal impurities, the pH value of the solution is maintained at 2.5 to 6.0, the solution is filtered after the reaction, filtered liquid enters an iron-removing reactor, the reaction temperature is controlled at 30 to 120 DEG C, the Baume degree is 30 to56 degrees Be, industrial peroxide or hydrogen peroxide is added under the pH value of 2.5 to 6.0 to remove the iron, organic matters can be removed by adding particle or powder active carbon under the temperature of 30 to 120 DEG C, filter liquid after the reaction and filter is pumped into a concentrator to be concentrated, crystallized and dripped at a normal pressure or a negative pressure, so an ultra-pure battery-grade manganese chloride product is obtained. For the manganese chloride product prepared through the method, the content of the manganese chloride product can reach more than 99 percent.

Description

technical field [0001] The invention relates to a method for preparing ultra-high-purity battery-grade manganese chloride used in manganese-lithium batteries or nickel-cobalt-manganese battery materials, in particular to a manganese chloride solution leached directly with ordinary manganese carbonate or metallic manganese with hydrochloric acid A method for the preparation of ultra-high purity battery-grade manganese chloride for use in battery materials. Background technique [0002] Manganese chloride solids (including reagent grade manganese chloride solids) prepared by ordinary methods or manganese chloride solids prepared by ordinary methods using manganese chloride solution leached with high-purity metal manganese and hydrochloric acid, its Ca, Mg impurities and heavy metals The content of impurities (Co, Ni, Pb, etc.) is very high. Among them, the content of Ca and Mg can reach about 1000ppm, and the content of heavy metal impurities (Fe, Co, Ni, Pb, Cd, Cr, etc.) ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/06
Inventor 常开军杨晓平
Owner HUBEI HAOYUAN MATERIAL TECH
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