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A method for preparing high-purity manganese sulfate monohydrate by double washing method

A hydrated sulfuric acid, high-purity technology, applied in the field of electrochemistry, can solve the problems of cumbersome process, difficult operation, and unsuitable for large-scale industrial production.

Active Publication Date: 2017-02-22
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned purification method is cumbersome, complicated, difficult to operate, and a fluorinating agent is added in the middle, so it is not suitable for large-scale industrial production

Method used

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  • A method for preparing high-purity manganese sulfate monohydrate by double washing method

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Experimental program
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Effect test

Embodiment 1

[0034] Get the manganese sulfate solution that rhodochrosite is made, measure the Mg content wherein with inductively coupled plasma emission spectrometer to be 8140mg L -1 , Ca content 1700mg·L -1 , K content 835mg·L -1 , Na content 973mg·L -1 , Fe content 105mg·L -1 , Ni content 16mg·L -1 , Cu content 25mg·L -1 , Zn content 50mg·L -1 , Pb content 62mg·L -1 . Simultaneous determination of Mn 2+ The content is 35g·L -1 .

[0035] Accurately measure 1500mL of manganese sulfate solution and place it in a 2000mL volumetric flask, stir and heat to 60°C, then slowly add 38.2g of NaOH, and 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 60°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 0.2g of oxalic ...

Embodiment 2

[0037] Accurately measure 1500mL of the same manganese sulfate solution in Example 1 and place it in a 2000mL volumetric flask. After stirring and heating to 50°C, slowly add 25% to 28% ammonia 68mL (calculated by 14mol / L) in a mass percentage. Stir at temperature for 60 min. After separation by filtration, the solid was mixed at a material-to-water ratio of 1:6 and stirred and washed at 50°C for 60 minutes. After filtration, the filter cake was beaten with a small amount of water, and 6mol / 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 of oxalic acid was added to it, stirred and reacted at 50°C for 60 minutes, and then filtered. Under stirring condition, slowly add 100g NH to the filtrate 4 HCO 3 After the addition of ammonium bicarbonate, stir and react at 50°C for 60 minutes, then filter, beat the solid and water at a ratio of 1:4, stir and wash at 50°C for 60 minutes, and then filter. Add a smal...

Embodiment 3

[0039] Accurately measure 1500mL of the same manganese sulfate solution in Example 1 and place it in a 2000mL volumetric flask, stir and heat to 80°C, then slowly add 53.5g of KOH, and 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 filtering, the filter cake was beaten with a small amount of water, and concentrated sulfuric acid was slowly added to it, and the amount of sulfuric acid was controlled so that the pH was 4, and then 0.2g of oxalic acid was added to it, stirred at 80°C for 60 minutes, and then filtered. Under stirring condition, slowly add 100g NH to the filtrate 4 HCO 3 After the addition of ammonium bicarbonate, stir and react at 80°C for 60 minutes, then filter, beat the solid and water at a ratio of 1:4, stir and wash at 80°C for 60 minutes, and then filter. Add a small amount of water to the obtained manganese carbonate solid, the...

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Abstract

The invention discloses a method for preparing high-purity hydrated manganese sulfate employing a dual washing method, and belongs to the technical field of electrochemistry. The method comprises the following steps: 1) reacting a manganese sulfate solution with aqueous alkali at the molar ratio of Mn<2+> to OH<-> being 1 to 2, so as to prepare manganese hydroxide sediments; 2) washing the manganese hydroxide sediments with water, reacting manganese hydroxide with sulfuric acid at the equal molar ratio, and generating manganese sulfate; and 3) reacting manganese sulfate with ammonium bicarbonate to generate manganese carbonate sediments, washing the manganese carbonate sediments with water, reacting the washed manganese carbonate sediments with sulfuric acid, filtering, evaporating, concentrating and drying, so as to prepare the high-purity hydrated manganese sulfate. Separation of different ions and purification of manganese sulfate are achieved by using different solubility of different metal ion salts and a plurality of times of precipitation and washing treatment.

Description

technical field [0001] The invention belongs to the technical field of electrochemistry 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 adopting a double washing method. Background technique [0002] High-purity manganese sulfate (battery-grade manganese sulfate) is mainly used in the synthesis of nickel-cobalt lithium manganese oxide ternary positive electrode materials and lithium manganese oxide positive electrode materials. It is a hot research topic in the domestic manganese industry in recent years. Although my country's manganese resources are very rich, the manganese sulfate products in my country are currently mainly low-purity products, with a general purity of about 98%. The current main uses include: 1) It is used as base fertilizer, seed soaking, fertilizer mixing, topdressing and foliar spraying to promote crop production and increase yield; 2) ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/10
CPCC01G45/10
Inventor 冯江涛刘建伟徐浩延卫
Owner XI AN JIAOTONG UNIV