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Short-process low-consumption high-purity manganese sulfate solution preparing method

A manganese sulfate solution and low-consumption technology, applied in the direction of manganese sulfate, etc., can solve the problems of removing calcium and magnesium impurities, manganese loss, high content, and difficulty in removing, and achieve the effects of reducing production costs, shortening the process flow, and improving production efficiency

Active Publication Date: 2017-02-01
UNIV OF SCI & TECH BEIJING
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The process of directly preparing manganese sulfate solution from rhodochrosite is long, and the key problem is that the technical difficulty of deep removal of impurities is high. Considering the cost accounting and environmental protection, the feasibility of this technology is poor.
Especially for the current situation that the average grade of rhodochrosite in my country is less than or equal to 14%, it is a big challenge to directly prepare high-purity manganese sulfate solution from the sulfuric acid leaching solution of rhodochrosite: (1) due to the complex types of soluble impurities in low-grade manganese ore, High content and difficult to remove
(2) Precipitants commonly used to remove calcium and magnesium impurities mainly include ammonium fluoride, manganese fluoride, etc., but due to the small particles of the precipitated products magnesium fluoride and calcium fluoride, it is difficult to settle and filter, resulting in manganese sulfate solution Calcium and magnesium impurities are not easy to remove in depth, and the precipitated product will absorb more manganese ions due to its high specific surface area, resulting in the removal of calcium and magnesium impurities accompanied by the loss of manganese
(3) In the traditional preparation process, in order to cooperate with the impurity removal process, it is necessary to repeatedly adjust the pH value of the system, resulting in serious waste of medicaments, complex process operation, and long synthesis cycle

Method used

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  • Short-process low-consumption high-purity manganese sulfate solution preparing method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] (1) The rhodochrosite of grade 12% is ground, crosses 200 mesh sieves, obtains manganese ore powder; Manganese ore powder is joined in the sulfuric acid solution of 2mol / L, and the mass ratio of sulfuric acid solution and manganese ore powder is 3:1, stirs After being heated to 90°C under certain conditions, the reaction was continued for 4 hours, and the manganese ore leaching solution 1 was obtained by filtration, and the impurity content was analyzed by ICP;

[0020] (2) Add manganese ore powder to manganese ore leaching solution 1, the mass ratio of manganese ore leaching solution 1 to manganese ore powder is 3:1, heat to 90°C under agitation and continue to react for 4 hours, and filter to obtain manganese ore leaching solution 2 ;

[0021] (3) Regulate the pH of manganese ore leaching solution 2 to 4 with barium hydroxide, then add barium fluoride until no new precipitation occurs, then filter to obtain filtrate 1, wherein barium hydroxide is 100 mesh sieves with ...

Embodiment 2

[0029] (1) grind the rhodochrosite of grade 14%, cross 150 mesh sieves, obtain manganese ore powder; Manganese ore powder is joined in the sulfuric acid solution of 1.8mol / L, the mass ratio of sulfuric acid solution and manganese ore powder is 4:1, in Continue to react for 3 hours after heating to 85°C under stirring conditions, filter to obtain manganese ore leaching solution 1, and use ICP to analyze its impurity content;

[0030] (2) Add manganese ore powder to the manganese ore leaching solution 1, the mass ratio of the manganese ore leaching solution 1 and the manganese ore powder is 5:1, heat to 80° C. under agitation and continue to react for 3 hours, and filter to obtain the manganese ore leaching solution 2;

[0031] (3) Regulate the pH of manganese ore leaching solution 2 to 3 with barium hydroxide, add barium fluoride again, until no new precipitation produces, then filter, obtain filtrate 1, wherein barium hydroxide is that content 98% crosses 100 mesh sieves Bariu...

Embodiment 3

[0038] (1) The rhodochrosite of grade 11% is ground, crosses 100 mesh sieves, obtains manganese ore powder; Manganese ore powder is joined in the sulfuric acid solution of 1.5mol / L, and the mass ratio of sulfuric acid solution and manganese ore powder is 5:1, in Continue to react for 2 hours after heating to 80°C with stirring, and filter to obtain manganese ore leaching solution 1;

[0039](2) Add manganese ore powder to manganese ore leaching solution 1, the mass ratio of manganese ore leaching solution 1 and manganese ore powder is 4:1; continue to react for 2 hours after heating to 85°C under stirring conditions, and filter to obtain manganese ore leaching solution 2 ;

[0040] (3) Regulate the pH of manganese ore leaching solution 2 to 3 with barium hydroxide, add barium fluoride again, until no new precipitation produces, then filter, obtain filtrate 1, wherein barium hydroxide is that content 98% crosses 100 mesh sieves Barium hydroxide octahydrate solid powder, barium...

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Abstract

The invention relates to a method for directly preparing a high-purity manganese sulfate solution from low grade rhodochrosite sulfuric acid extraction liquid. The rule that the PH value of a system is changed from small to large is implemented, and an efficient chemical coupling mechanism is played. The method includes the steps that firstly, manganese mineral powder is continuously dissolved into low grade manganese ore sulfuric acid extraction liquid, the pH value of the extraction liquid is sequentially adjusted with barium hydroxide to reach 3 to 4, then barium fluoride is added, and filtering is carried out; secondly, the pH value of filter liquor is adjusted with barium hydroxide to reach 5 to 6, then barium sulfide is added, filtering is carried out, and new filter liquor is obtained; and finally, the PH value of the new filter liquor is adjusted with barium hydroxide to reach 8, and filtering is carried out to obtain the high-purity manganese sulfate solution. The method is simple in operation, medicament waste caused by operation for repeatedly adjusting the PH value of the system in an overlapped manner is avoided, the manganese content in the prepared high-purity manganese sulfate solution is larger than or equal to 80 g / L, the main impurity contents are all smaller than or equal to 10 ppm, the heavy metal content is smaller than or equal to 1 ppm, and the short-process low-consumption free-pollution high-purity manganese sulfate solution preparing method is provided.

Description

technical field [0001] The invention belongs to the field of chemical production, in particular to a method for directly preparing high-purity manganese sulfate solution from sulfuric acid leaching solution of low-grade rhodochrosite. Background technique [0002] At present, the demand for high-purity manganese sulfate is gradually increasing, but the production of high-purity manganese sulfate is subject to relatively large technical restrictions. At home and abroad, electrolytic metal manganese is commonly used to produce high-purity manganese sulfate, that is, electrolytic metal manganese is processed into powder and then dissolved in sulfuric acid. Because the production of these high-purity manganese sulfate has experienced ion manganese (manganese ore)-metal manganese (electrolysis)- The production cycle of ionic manganese (oxidation), so the product price is expensive, and the physical indicators such as particle size and morphology are difficult to control. Moreove...

Claims

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Application Information

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IPC IPC(8): C22B3/08C22B3/44C01G45/10
CPCC01G45/10C22B3/08C22B3/44
Inventor 连芳陈李泽方毛磊马来君
Owner UNIV OF SCI & TECH BEIJING
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