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Method for preparing Mn(OH)2 by circularly using ammonia water

A technology of ammonia water and concentration, applied in the direction of manganese oxide/manganese hydroxide, etc., can solve the problems of less research, easy oxidation, instability, etc.

Inactive Publication Date: 2010-07-14
GUIZHOU REDSTAR DEVING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Mn(OH) 2 It is easy to oxidize and unstable. It is generally not used as a commodity. It is usually only used as an intermediate product in the preparation of manganese salts, so there are few studies on it.

Method used

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  • Method for preparing Mn(OH)2 by circularly using ammonia water
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  • Method for preparing Mn(OH)2 by circularly using ammonia water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Manganese oxide powder and Sr(HS) 2 The solution is reacted, and the MnSO obtained after washing, separating, and sulfuric acid compounding 4 The solution was precision filtered with a 0.5 μm filter membrane, and the measured concentration was 450g / L. Measure 3000mL into a 5000mL beaker, and add 10mol / L NH 4 OH 1790ml, measured solution pH = 8.0, maintained stirring for 30 minutes and suction filtered, rinsed the filter cake with a small amount of deionized water, combined the filtrate for recycling regeneration treatment, Mn(OH) 2 Dry in a vacuum oven under nitrogen protection at 60°C for 16 hours to obtain Mn(OH) 2 sample 1 # .

[0019] Take the above filtrate - the concentration is 1.76mol / L (NH4) 2 SO 4 Put 2500ml of the solution in a 5000mL three-neck flask, connect the second stage to a bubbling absorption device equipped with deionized water in a cold water bath, turn on the vacuum pump to form a slight negative pressure, and slowly add 1470mL of 3mol / L Ba(O...

Embodiment 2

[0021] Manganese oxide powder and Sr(HS) 2 The solution is reacted, and the MnSO obtained after washing, separating, and sulfuric acid compounding 4 The solution was precision filtered with a 0.5 μm filter membrane, and the measured concentration was 200g / L. Measure 2000mL into a 5000mL beaker, and add 2mol / L NH 4 OH 2650ml, measure the solution pH=7.5, keep stirring for 30 minutes and then suction filter, rinse the filter cake with a small amount of deionized water, combine the filtrate for recycling regeneration treatment, Mn(OH) 2 Dry in a vacuum oven under nitrogen protection at 60°C for 16 hours to obtain Mn(OH) 2 sample 2 # .

[0022] Get above-mentioned filtrate---concentration is 0.53mol / L (NH 4 ) 2 SO 4 Put 3000ml of the solution in a 5000mL three-neck flask, connect the second stage to a bubbling absorption device equipped with deionized water in a cold water bath, turn on the vacuum pump to form a slight negative pressure, and slowly add 795mL of 2mol / L Ba(OH)...

Embodiment 3

[0024] Commercially available feed grade MnSO 4 ·H 2 O was added to deionized water to prepare 450g / LMnSO 4 Solution, add MnS made by Guizhou Hongxing Development Co., Ltd. under stirring to remove impurities, and filter it with a 0.5 μm filter membrane to measure MnSO 4 447.5g / L, put 3000ml in a 5000mL beaker, add 10mol / L NH 4 OH1780ml, measure the solution pH=8.0, maintain stirring for 30 minutes, then suction filter, rinse the filter cake with a small amount of deionized water, and combine the filtrates for recycling regeneration treatment, Mn(OH) 2 Dry in a vacuum oven under nitrogen protection at 60°C for 16 hours to obtain Mn(OH) 2 sample 3 # .

[0025] Get the above-mentioned filtrate—concentration is 1.74mol / L (NH4) 2 SO 4 Put 3000ml of the solution in a 5000mL three-necked flask, connect the second stage to a bubbling absorption device equipped with deionized water in a cold water bath, turn on the vacuum pump to form a slight negative pressure, and slowly add ...

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Abstract

The invention relates to a method for preparing Mn(OH)2 by circularly using ammonia water, which comprises the following steps: making MnSO4 into a solution with the concentration of 100-450g / L, precisely filtering the solution, putting in a reaction vessel, adding ammonia water which is quantitatively prepared and has the concentration of 2-10mol / L while stirring at normal temperature, carrying out reaction, controlling pH of end point of the reaction to be 7-8, continuously stirring for 15-30 minutes, carrying out pressure filtration and separation to obtain a filtrate and Mn(OH)2 solid; reacting the filtrate in the step A with a Ba(OH)2 solution with the concentration of 0.5-3mol / L at the same molar weight in a closed container, turning on a heating device after the end point of the reaction is reached, raising temperature, stirring so that the solution is decomposed into ammonia gas, and finally absorbing by using deionized water to prepare the ammonia water.

Description

technical field [0001] The invention relates to a method for preparing Mn(OH) by recycling ammonia water 2 Methods. Background technique [0002] Mn(OH) 2 It is easy to oxidize and unstable, and it is generally not used as a commodity. It is usually only used as an intermediate product for the preparation of manganese salts, so there are few studies on it. [0003] With the development of lithium-ion secondary batteries, especially power batteries, lithium manganate and multi-component materials containing manganese have gained attention. On the other hand, due to the particularity of manganese ore resources, the ore powder raw materials are mixed with alkali metal and alkaline earth metal impurities. , K, Na, Ca, Mg, etc., separate these impurities to obtain high-purity Mn(OH) 2 , has become an urgent problem to be solved in the preparation process of lithium-manganese secondary battery materials. Contents of the invention [0004] In the present invention, manganese ...

Claims

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Application Information

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IPC IPC(8): C01G45/02
Inventor 姜志光华东罗建平都邦旭
Owner GUIZHOU REDSTAR DEVING
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