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Preparation method of manganese sulfate monohydrate

A technology for hydrating sulfuric acid and manganese sulfate, applied in the field of chemistry, can solve problems such as difficulty and complicated operation

Active Publication Date: 2015-09-09
SHAANXI ZIYANG XIANGGUI MANGANESE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Although the above methods can obtain higher quality manganese sulfate products, some methods have limitations in use, for example, some are only effective for raw materials containing trace amounts of sodium ions; some methods are more complicated to operate, such as using ferric iron The process of removing sodium ions requires precise control of the pH value between 1.6-1.8, which is difficult in practical applications

Method used

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  • Preparation method of manganese sulfate monohydrate

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Effect test

Embodiment 1

[0035] Get the manganese sulfate solution that rhodochrosite is made, measure the Mg content wherein with inductively coupled plasma emission spectrometer to be 8473mg L -1 , Ca content 2150mg·L -1 , K content 1073mg·L -1 , Na content 1235mg·L -1 , Fe content 151mg·L -1 , Ni content 26mg·L -1 , Cu content 37mg·L -1 , Zn content 63mg·L -1 , Pb content 50mg·L -1 . Simultaneous determination of Mn 2+ The content is 42.5g·L -1 .

[0036] Accurately measure 1000mL of manganese sulfate solution and place it in a 2000mL volumetric flask, stir and heat to 60°C, then slowly add 64.13g of NaCO 3 and 50 mL of ammonia water (25% to 28%), and stirred at this temperature for 60 min. After separation by filtration, the solid was mixed at a material-to-water ratio of 1:5 and stirred and washed at 60°C for 60 minutes. After filtration, the filter cake was beaten with a small amount of water, and then 12mol / L sulfuric acid was slowly added to it, and the amount of sulfuric acid was ...

Embodiment 2

[0038] Accurately measure 1000mL of manganese sulfate solution and place it in a 2000mL volumetric flask, stir and heat to 60°C, then slowly add 61.1g of NH 4 HCO 3 and 68mL of ammonia water (25wt%-28wt%), stirred at this temperature for 60min. After separation by filtration, the solid was mixed at a material-to-water ratio of 1:5 and stirred and washed at 50°C for 60 minutes. After filtration, the filter cake was beaten with a small amount of water, and 12mol / L sulfuric acid was slowly added to it, and the amount of sulfuric acid was controlled so that the pH was 4, and then 1mL hydrogen peroxide was added to it, stirred at 50°C for 60min, and then mixed with MnCO 3 After adjusting pH=5-6, filter. Add 0.75g MnF to the filtrate with stirring at 50°C 2 Stir and react for 120 minutes, filter, discard the filter cake, follow the recrystallization process of the filtrate, and dry the obtained solid at 80°C for 24 hours to obtain a high-purity manganese sulfate solid, which is r...

Embodiment 3

[0040] Accurately measure 1000mL of manganese sulfate solution and place it in a 2000mL volumetric flask, stir and heat to 80°C, then slowly add 72.7g of (NH 4 ) 2 CO 3 In a mixed solution formed with 75mL of ammonia water (25%-28%), stir at this temperature for 60min. After separation by filtration, the solid was mixed at a material-to-water ratio of 1:6 and stirred and washed at 80°C for 60 minutes. After filtration, the filter cake was beaten with a small amount of water, and 12mol / L sulfuric acid was slowly added to it, and the amount of sulfuric acid was controlled so that the pH was 4, and then 0.3g oxalic acid was added to it, stirred at 80°C for 60min, and then mixed with MnCO 3 After adjusting pH=5-6, filter. Add 0.3g MnF to the filtrate under stirring at 40°C 2 Stir and react for 120 minutes, filter, discard the filter cake, follow the recrystallization process of the filtrate, and dry the obtained solid at 80°C for 24 hours to obtain a high-purity manganese sulf...

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Abstract

The invention discloses a preparation method of manganese sulfate monohydrate, which is characterized in that a manganese sulfate solution prepared by rhodochrosite is reacted with soluble carbonate under alkalescence environment at 30-80 DEG C to generate MnCO3 deposition, sodion in the manganese sulfate solution prepared by rhodochrosite is removed, and most calcium ion, magnesium ion and other heavy metal ions are removed; sulfuric acid and MnCO3 are reacted to generate manganese sulfate, calcium ion and magnesium ion in manganese sulfate are deposited and removed by fluorinion, and finally, the manganese sulfate solution is filtered, recrystallized and dried to obtain the product. By using solubility difference of different metal ionic salt, through multitime deposition and washing process, by controlling the acid-base value of a system during a deposition washing process, impurity ion of calcium, magnesium and sodium can be removed at maximum degree, microscale Ca<2+> and Mg<2+> in the product can be removed by introducing F ion, product purity is increased by recrystallization, and manganese sulfate purification can be realized. The method has the advantages of simple and easy operation and friendly environment, and is suitable for industrial large scale production.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a method for preparing high-purity manganese sulfate monohydrate, in particular to a method for preparing high-purity manganese sulfate monohydrate by combining transformation-washing-precipitation-recrystallization. Background technique [0002] High-purity manganese sulfate (battery-grade manganese sulfate) is valued by the domestic manganese industry as a nickel-cobalt lithium manganate ternary cathode material and a lithium manganese oxide cathode material. my country is very rich in manganese resources, but the manganese sulfate products currently on the market are mainly low-purity, and the general purity is about 98%. The main uses include: 1) It is used for base fertilizer, seed soaking, fertilizer mixing, topdressing and foliar spraying to promote crop production and increase yield; 2) It is used as feed additive in animal husbandry and feed industry to make poultry grow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/10
Inventor 王天雄延卫董平安冯江涛刘京李习
Owner SHAANXI ZIYANG XIANGGUI MANGANESE IND CO LTD
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