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Method for circularly purifying manganese sulfate and manganese carbonate

A purification method, manganese carbonate technology, applied in the direction of manganese sulfate, chemical instruments and methods, manganese compounds, etc., can solve the problem that the content of calcium and magnesium ions cannot meet the needs of development, etc.

Inactive Publication Date: 2010-05-12
GUIZHOU REDSTAR DEVING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of alkaline earth metals and alkali metals, especially calcium and magnesium ions in the manganese carbonate and manganese sulfate materials provided by the prior art cannot meet the current development needs of lithium manganate secondary batteries

Method used

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  • Method for circularly purifying manganese sulfate and manganese carbonate
  • Method for circularly purifying manganese sulfate and manganese carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 354g / L MnSO 4 Put 4000ml of the solution in a 5000ml beaker, control the temperature at 50°C, and slowly add food-grade NH under stirring 4 HCO 3 1514g, separated by suction filtration, filtrate recovery (NH 4 ) 2 SO 4 , the solid was washed twice at 80°C with a material-to-water ratio of 1:5, and part of it was dried into MnCO 3 1 # .

[0015] The manganese carbonate after above-mentioned washing is placed in the beaker of 5000ml, adds a small amount of deionized water to make a slurry, with 6mol / L H 2 SO 4 React until the pH value is 1, heat and boil with washed MnCO 3 Adjust the pH value to 4, filter with slow qualitative filter paper, discard the filter residue, evaporate the filtrate to crystallize, and dry the crystallization in an oven at 80-85°C for 20 hours to obtain MnSO 4 ·H 2 O sample 1 # .

Embodiment 2

[0017] 354g / L MnSO 4 Place the solution in a 5000ml beaker, control the temperature at 55°C, and slowly add food-grade NH under stirring 4 HCO 3 1514g, separated by suction filtration, filtrate recovery (NH 4 ) 2 SO 4 , The solid was washed twice at 100°C with a material-to-water ratio of 1:5.

[0018] The above washed MnCO 3 Add a small amount of deionized water for beating, and use 9mol / L H 2 SO 4 React to a pH of 2, heat and boil with washed MnCO 3 Return to pH 5, filter with slow qualitative filter paper, discard the filter residue, put the filtrate in a 5000ml beaker, control the temperature within 55°C, and slowly add equimolar NH 4 HCO 3 Synthesis, solid-liquid separation, liquid recovery (NH 4 ) 2 SO 4 , the solid was washed twice at 100°C with a material-to-water ratio of 1:5, dehydrated and dried in a vacuum oven at 85°C for 16 hours to obtain MnCO 3 sample 2 # .

Embodiment 3

[0020] Repeat Example 1, the difference is that the 12mol / L H that adds 2 SO 4 , slowly add food-grade NH to the manganese sulfate solution with stirring at a temperature of 60 4 HCO 3 , get MnCO 3 sample 3 # and MnSO 4 ·H 2 O sample 3 # .

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Abstract

The invention relates to a method for circularly purifying manganese sulfate and manganese carbonate. The method comprises the following steps: A, stirring manganese sulfate solution at the temperature of between 40 and 80 DEG C, and adding ammonium bicarbonate into the solution for synthesis, controlling the synthesis end point to be an equimolar reaction, separating solid, and washing the solid with hot water to prepare manganese carbonate; B, adding the prepared manganese carbonate into 6 to 12mol / L H2SO4 for reaction, controlling the pH value of the reaction solution to be between 1 and 2, and heating and boiling the solution; C, adding the manganese carbonate prepared in the step A into the reaction solution in the step B, and adjusting the pH value of the solution back to be 4 to 5; and D, performing solid-liquid separation on the reaction solution, distilling and crystallizing the prepared filtrate, and drying the crystal to prepare the manganese sulfate. The circularly purifying method can prepare high-purity manganese sulfate and manganese carbonate with low calcium magnesium and low potassium and sodium.

Description

technical field [0001] The invention relates to a purification process of manganese sulfate and manganese carbonate, in particular to a circulation purification process of manganese sulfate and manganese carbonate. Background technique [0002] With the development of lithium manganese oxide secondary batteries, the requirements for manganese sulfate and manganese carbonate materials are also exceedingly high. In addition to the high requirements for particle size distribution and heavy metal content, there are also high requirements for alkali metals and alkaline earth metals in materials, especially for power batteries. The requirements for such materials are more stringent. The contents of alkaline earth metals and alkali metals, especially calcium and magnesium ions in the manganese carbonate and manganese sulfate materials provided by the prior art cannot meet the current development needs of lithium manganate secondary batteries. [0003] For the preparation of mangan...

Claims

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Application Information

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IPC IPC(8): C01G45/10C01G45/00
CPCC01G45/00C01G45/10
Inventor 姜志光华东
Owner GUIZHOU REDSTAR DEVING
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