Method for preparing electronic-grade manganese sulfate by utilizing tungsten ore alkaline leaching slag

An alkali leaching, electronic-grade technology, applied in the direction of manganese sulfate, etc., can solve the problems of high cost and long impurity removal process, and achieve the effects of efficient recycling, simplified impurity removal process, and simple production process

Inactive Publication Date: 2014-12-10
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The preparation process of the above-mentioned high-purity manganese sulfate or high-purity manganese compound requires external agents to remove silicon impurities, and the impurity removal process is long and costly

Method used

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  • Method for preparing electronic-grade manganese sulfate by utilizing tungsten ore alkaline leaching slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Grind tungsten ore alkali leaching slag to a particle size of 75 Next, take 200g, put it into the leaching tank, slowly add 240g of sulfuric acid with a concentration of 70%, turn on the stirrer, react and leaching at 70°C for 1.5h, and then filter. Heat the filtrate to 60°C, add sodium carbonate to adjust the pH value of the solution to 4, hydrolyze the iron and aluminum ions in the solution to generate corresponding hydroxide colloids, cool the solution to 30°C, and stir for 3 hours to fully absorb the hydroxide colloids in the solution silicon, scandium and other impurities, and then stand and filter. The filtrate was heated to 80°C, the pH value was controlled to 4.5, 26g of manganese fluoride was added, and the reaction was stirred for 0.5h to make the Ca in the solution 2+ , Mg 2+ Wait for the impurity ions to form insoluble fluoride precipitates, then add 12g of sodium sulfide, stir for 2.5 hours to make the heavy metal impurity ions in the solution form insol...

Embodiment 2

[0026] Grind tungsten ore alkali leaching slag to a particle size of 105 Next, take 200g, put it into the leaching tank, slowly add 185g of sulfuric acid with a concentration of 80%, turn on the stirrer, react and leaching at 80°C for 2h, and then filter. Heat the filtrate to 70°C, add sodium carbonate to adjust the pH value to 5, hydrolyze the iron and aluminum ions in the solution to generate corresponding hydroxide colloids, cool the solution to 40°C, and stir for 2.5 hours to fully absorb the hydroxide colloids in the solution silicon, scandium and other impurities, and then stand and filter. The filtrate was heated to 90°C, the pH value was controlled to be 5, 28g of manganese fluoride was added, and the reaction was stirred for 1h to make the Ca in the solution 2+ , Mg 2+ Wait for the impurity ions to form insoluble fluoride precipitates, then add 15g of sodium sulfide, stir for 2 hours to make the heavy metal impurity ions in the solution form insoluble sulfide preci...

Embodiment 3

[0029] Grind tungsten ore alkali leaching slag to a particle size of 150 Next, take 200g, put it into the leaching tank, slowly add 145g of sulfuric acid with a concentration of 90%, turn on the stirrer, react and leaching at 90°C for 1.5h and then filter. Heat the filtrate to 80°C, add sodium carbonate to adjust the pH value of the solution to 6, hydrolyze the iron and aluminum ions in the solution to generate corresponding hydroxide colloids, cool the solution to 50°C, and stir for 2 hours to fully absorb the hydroxide colloids in the solution silicon, scandium and other impurities, and then stand and filter. The filtrate was heated to 95°C, the pH value was controlled to 6.5, 25g of manganese fluoride was added, and the reaction was stirred for 1.5h to make the Ca in the solution 2+ , Mg 2+ Wait for the impurity ions to form insoluble fluoride precipitates, then add 18g of sodium sulfide, stir for 1.5 hours to make the heavy metal impurity ions in the solution form insol...

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Abstract

A method for preparing electronic-grade manganese sulfate by utilizing tungsten ore alkaline leaching slag comprises steps as follows: the tungsten ore alkaline leaching slag is ground to particles with particle sizes smaller than 250 mu m, sulfuric acid with the mass fraction of 70%-90% is added, a solution is controlled to react for 1-3 hours at the temperature of 70 DEG C-90 DEG C and then filtered; the temperature of filtrate is controlled to be 70 DEG C-90 DEG C, sodium carbonate is added, the pH value of the solution is adjusted to be 4-6.5, so that iron ions and aluminum ions in the solution are hydrolyzed and generate corresponding hydroxide colloids; the solution is cooled to 30 DEG C-50 DEG C and stirred, so that the hydroxide colloids fully absorb silicon and scandium in the solution, and still standing and filtration are performed; manganese fluoride is added to the filtrate to remove calcium and magnesium in the solution, sodium sulphide is added to remove heavy metal impurity ions, and still standing and filtration are performed; the filtrate is concentrated, crystallized, washed, recrystallized, filtered and dried, so that the electronic-grade manganese sulfate is obtained. According to the method, tungsten ore alkaline leaching slag is taken as a raw material and used for preparing the electronic-grade manganese sulfate, so that the tungsten ore alkaline leaching slag can be recycled, pollution to the environment is reduced, and economic benefits can be obtained.

Description

technical field [0001] The invention relates to recycling and utilization of tungsten ore alkali leaching slag, in particular to a method for preparing electronic-grade manganese sulfate by using tungsten ore alkali leaching slag. Background technique [0002] As an important basic raw material of manganese-based materials, electronic-grade manganese sulfate is of great significance to the development of my country's new generation of environmental protection and high-energy battery industry. With the rapid development of some high-quality and high-purity electronic chemicals such as electrolytic manganese, chemical manganese dioxide, and magnetic manganese tetraoxide, especially the rapid development of lithium-ion batteries, the demand for electronic-grade manganese sulfate is increasing. Manganese ore is the main raw material of manganese sulfate products. Although my country has abundant reserves, manganese ore is poor, miscellaneous and fine, and the average grade of ra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/10
Inventor 邱运仁闫升
Owner CENT SOUTH UNIV
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