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Method for preparing high-purity manganous-manganic oxide and high-purity magnesium oxide

A technology of manganese tetroxide and magnesium oxide, applied in the directions of manganese oxide/manganese hydroxide, magnesium oxide, ammonium sulfate, etc., can solve the problems of waste of magnesium resources, poor quality stability, high energy consumption, and save reagent consumption. and energy consumption, reducing operation steps, and the effect of simple process

Active Publication Date: 2022-04-22
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]Because the manganese ore in our country is mainly low-grade ore, manganese ore is used to directly prepare manganese tetraoxide, but there are still manganese tetraoxides with low purity and poor quality stability and other shortcomings
On the other hand, although the existing precipitation and impurity removal process can effectively remove heavy metal ions, it fails to remove magnesium ions, which not only affects the quality of manganese tetraoxide, but also causes a waste of magnesium resources.
Therefore, there is an urgent need for a new process that is environmentally friendly and economically beneficial to solve the problems of high energy consumption, poor quality stability and unreasonable utilization of associated resources in the current high-purity manganese manganese tetraoxide production method

Method used

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  • Method for preparing high-purity manganous-manganic oxide and high-purity magnesium oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A kind of production method of electrolytic manganese

[0054] Including the processes of leaching, impurity removal, extraction, stripping and recovery of ammonia nitrogen and magnesium, the details are as follows:

[0055] S1. Leaching: Dilute 18.23g of concentrated sulfuric acid to 95mL with water, then add 30g of crushed manganese ore powder, stir and leaching at 90°C for 3 hours, and filter to obtain the leaching solution and leaching residue. The rate is 96.34%. In the leachate, the concentration of each element is: Mn 35.44g / L, Mg 9.14g / L, Fe 2.96g / L, Na 0.38g / L, Ca0.33g / L, Al 0.11g / L;

[0056] S2, impurity removal: add manganese dioxide to oxidize low-valent iron in the leaching solution obtained in step S1, the ratio of the amount of substance added by manganese dioxide to the amount of low-valent iron in the leaching solution is 0.5:1, then add sodium hydroxide Adjust the pH value to 5.47, precipitate Fe and Al ions, and then add SDD to react to form chelated...

Embodiment 2

[0063] A kind of production method of electrolytic manganese

[0064] Including the processes of leaching, impurity removal, extraction, stripping and recovery of ammonia nitrogen and magnesium, the details are as follows:

[0065] S1. Leaching: Dilute 18.19g of concentrated sulfuric acid to 130mL with water, then add 30g of crushed manganese ore powder, stir and leaching at 50°C for 5h, and filter to obtain the leaching solution and leaching residue. The rate is 97.41%. In the leach solution, the concentration of each element is: Mn 26.19g / L, Mg 6.83g / L, Fe 2.19g / L, Na 0.28g / L, Ca0.24g / L, Al 0.08g / L;

[0066] S2, impurity removal: add hydrogen peroxide to the leaching solution obtained in step S1 to oxidize the low-valent iron, the ratio of the amount of the substance added to the hydrogen peroxide to the amount of the low-valent iron in the leaching solution is 0.5:1, then add sodium hydroxide to adjust the pH value to 5.26. Precipitate Fe and Al ions, and then add SDD to r...

example 3

[0073] The production method of the electrolytic manganese of the present embodiment is the same as that of Example 1, the difference is that in step S3, neodecanoic acid is used as the extraction agent, aviation kerosene is the diluent, the concentration is 400g / L, and the mass fraction is 30%. Sodium hydroxide solution is saponified to a saponification rate of 20%, the pH of the purified solution is adjusted to be 4, and O:A=1:1 is controlled in the countercurrent extraction process, and the purified solution obtained in step S2 and the organic phase with a saponification rate of 20% are subjected to secondary The loaded organic phase and raffinate were obtained by countercurrent extraction. The manganese concentration in the organic phase was detected to be 8.79g / L, and the magnesium concentration was 0.73g / L. The loaded organic phase was washed with manganese sulfate solution at pH 5.0-5.5 to remove Impurity magnesium in the organic phase is loaded to obtain an organic phas...

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Abstract

The invention provides a method for preparing high-purity manganous-manganic oxide and high-purity magnesium oxide, which comprises the following steps: (1) leaching manganese ore to prepare a manganese-containing solution; (2) carrying out impurity removal treatment; (3) manganese and magnesium in the purified liquid are separated through extraction, manganese enters an organic phase, and magnesium remains in raffinate; (4) carrying out reverse extraction on the loaded organic phase by using alkali liquor to obtain a regenerated organic phase and reverse extraction liquor; (5) filtering the strip liquor to obtain manganese sulfate, and drying to obtain a high-purity manganese sulfate product; (6) adding ammonia water into the raffinate for precipitation to obtain magnesium hydroxide and an ammonium sulfate solution, washing the magnesium hydroxide, and calcining to obtain a high-purity magnesium oxide product; and (7) evaporating the ammonium sulfate solution to obtain an ammonium sulfate product. According to the method, efficient preparation of high-purity manganous-manganic oxide is achieved through alkali reverse extraction, high-added-value utilization of magnesium is achieved, and the method has the advantages of being high in resource utilization rate, low in cost, green, clean and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for preparing high-purity trimanganese tetraoxide and high-purity magnesium oxide. Background technique [0002] Trimanganese tetroxide, as an important inorganic functional material, is widely used in the fields of catalytic active components, electromagnetic materials, electrochemistry and air purification. In recent years, with the development of the new energy field, the demand for power lithium-ion batteries is also rising, as LiMn 2 o 4 Prepared high-quality raw materials, high-purity Mn 3 o 4 demand also increased. Currently, Mn 3 o 4 The preparation methods can be divided into several types according to the different raw materials: electrolytic metal manganese suspension catalytic oxidation method, reduction method, roasting method and manganese brine thermal oxidation method, etc., mainly using metal manganese, manganese dioxide, manganese sulfate ...

Claims

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Application Information

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IPC IPC(8): C22B47/00C22B26/22C22B3/38C22B3/32C22B3/44C01F5/02C01F5/06C01C1/24C01G45/02
CPCC22B47/00C22B26/22C22B3/44C01F5/02C01F5/06C01C1/24C01G45/02C01P2006/80C01P2002/72Y02P10/20
Inventor 钟宏王启任王帅马鑫
Owner CENT SOUTH UNIV
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