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High-purity manganous nitrate and preparation method thereof

A technology of manganese nitrate and manganese sulfate solution, applied in the direction of manganese nitrate, etc., can solve the problem of high content of heavy metals

Inactive Publication Date: 2013-12-11
GUIZHOU REDSTAR DEVING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is: to overcome the defect of high heavy metal content in the existing high-purity manganese nitrate, provide a kind of high-purity manganese nitrate and its preparation method, adopt manganese sulfide-nitric acid process route, obtain the low heavy metal content High-purity liquid manganese nitrate product reduces process cost

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  • High-purity manganous nitrate and preparation method thereof

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preparation example Construction

[0021] A preparation method of manganese nitrate, the method comprising:

[0022] (1) Vulcanization

[0023] Sulfurize the mixed gas containing ammonia and hydrogen sulfide gas with 150-300g / L (preferably 200-250g / L) manganese sulfate solution until the Mn in the solution 2+ When the concentration is less than 500ppm, stop the reaction, separate the solid from the liquid (preferably press filter), and then wash the obtained manganese sulfide filter cake for use. The filtrate obtained by solid-liquid separation is used to recover ammonium sulfate.

[0024] The manganese sulfate solution above can be made from commercially available manganese sulfate, or from flue gas desulfurization.

[0025] In a specific embodiment, ammonia gas and hydrogen sulfide gas (preferably in molar ratio of reaction) are passed into the absorption tower, and the manganese sulfate solution is sprayed to absorb the above-mentioned gases to carry out sulfidation reaction. The injection speed of the so...

Embodiment 1

[0048] (1) Vulcanization

[0049] The reaction molar ratio of ammonia gas and hydrogen sulfide gas is passed into the absorption tower, and then a manganese sulfate solution with a concentration of 150g / L is sprayed to absorb the above-mentioned gas for sulfidation reaction. When Mn 2+ When the concentration is less than 500ppm, the reaction is stopped, separated by pressure filtration, and the filtrate is recovered after treatment (NH 4 ) 2 SO 4 , The filter cake (manganese sulfide) is washed twice with 60°C deionized water according to the weight ratio of feed to water 1:4, each time for 3 hours, separated by pressing and filtering, and the water content of the filter cake is controlled to be less than 25% for later use.

[0050] (2) Acidification

[0051] Put the above filter cake in a glass-lined reaction pot, replace the air in the pot with nitrogen, then add 98% industrial grade nitric acid under airtight conditions, keep the temperature of the reaction system under ...

Embodiment 2

[0056] The reaction molar ratio of ammonia gas and hydrogen sulfide gas is passed into the absorption tower, and then a manganese sulfate solution with a concentration of 214g / L is sprayed to absorb the above-mentioned gas for sulfidation reaction. When Mn 2+ When the concentration is less than 500ppm, the reaction is stopped, separated by pressure filtration, and the filtrate is recovered after treatment (NH 4 ) 2 SO 4 , The filter cake (manganese sulfide) is washed twice with 62°C deionized water according to the weight ratio of feed to water 1:4, each time for 3 hours, separated by pressing and filtration, and the moisture content of the filter cake is controlled to be less than 25% for later use.

[0057] (2) Acidification

[0058] Put the above filter cake in a glass-lined reaction pot, replace the air in the pot with nitrogen, then add 98% industrial grade nitric acid under airtight conditions, keep the temperature of the reaction system under jacket cooling, stir the...

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Abstract

The invention provides a high-purity manganous nitrate and a preparation method thereof. The method comprises the following steps: (1) sulfuration, adding the mixed gas containing ammonia gas and hydrogen sulfide into a manganese sulfate solution of 150-300g / L to conduct a sulfuration reaction until the concentration of Mn<2+> in the solution is less than 500ppm, then stopping the reaction, conducting solid-liquid separation, and then washing an obtained manganese sulfate filter cake for later use; (2) acidification, adding nitric acid into the manganese sulfate filter cake obtained in the sulfuration step (1) at the nitrogen atmosphere, keeping the temperature of a reaction system to be less than 50 DEG C, and using hydrogen sulfide produced in a nitrogen displacement reaction in the reaction process; stirring, reacting until the pH value is 3.5-4.0, stopping adding acid, then conducting solid-liquid separation, and the obtained filtrate is a manganous nitrate product. The preparation method adopts a manganese sulfide-nitric acid process route to obtain the high-purity manganous nitrate product with low content of heavy metals, and the process cost is lowered.

Description

technical field [0001] The invention relates to the field of inorganic chemistry, in particular to a high-purity manganese nitrate and a preparation method thereof. Background technique [0002] High-purity manganese nitrate is mainly used in the preparation of precursors of ternary cathode materials for lithium-ion secondary batteries and the production of high-purity manganese oxides. The traditional production method of manganese nitrate is mainly metal manganese-nitric acid method. The defect of this method is that the heavy metal content in the obtained product is high, the production energy consumption is large, and the cost is high. Contents of the invention [0003] The technical problem to be solved by the present invention is: to overcome the defect of high heavy metal content in the existing high-purity manganese nitrate, provide a kind of high-purity manganese nitrate and its preparation method, adopt manganese sulfide-nitric acid process route, obtain the low ...

Claims

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Application Information

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IPC IPC(8): C01G45/08
Inventor 姜志光华东高月飞马新宏
Owner GUIZHOU REDSTAR DEVING
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