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Method for preparing high-purity manganese sulfate through extracting low-grade pyrolusite by using rice straw

A technology of pyrolusite and straw straw, which is applied in the field of hydrometallurgy

Inactive Publication Date: 2014-12-10
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of rice is produced in southern China, and a large amount of rice straw is produced every year, but its comprehensive processing and utilization efficiency is very low, and most of it is left to rot or burn as organic fertilizer

Method used

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  • Method for preparing high-purity manganese sulfate through extracting low-grade pyrolusite by using rice straw

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 10g of pyrolusite (see Table 1 for its indicators) into the reaction vessel, then add 3 M sulfuric acid solution with a volume of 180ml, and then add 20g of crushed dry straw (length after crushing 2 to 4 mm). Since the crushed dry straw has a low density and cannot sink into the sulfuric acid solution, the reaction is carried out in a special straw leaching reaction device for pyrolusite. Such as figure 1 As shown, the reaction device has a cylindrical reaction vessel 1 with an upper opening. A gland 2 is arranged at the opening of the reaction vessel. There are many small holes 7 on the gland 2. There is a central hole 6 in the middle of the gland 2. The agitator 4 passes through the The central hole 6 protrudes into the reaction vessel. The diameter of gland 2 is slightly smaller than the internal diameter of reaction vessel, and gland 2 can all be pressed in the sulfuric acid with dry straw stalk 3;

[0023] (2) Turn on the stirrer and heat the solution ...

Embodiment 2

[0032] (1) Add 20g of pyrolusite into the reaction vessel, then add 3 M sulfuric acid solution with a volume of 320ml, and then add 35g of pulverized dry straw (length after pulverization is 2-4 mm). The reaction was carried out in the reaction device for leaching pyrolusite with straw straw as provided in the examples.

[0033] (2) Turn on the stirring device and heat the solution to 80 0 C, the reaction was continuously stirred at this temperature for 12 hours. After the reaction is completed, cool to room temperature, first remove the straw stalks on the surface, filter, then filter the remaining solution, wash the filter residue with water for 3 times, and combine the two filtrates. The leaching rate is greater than 97.1%.

[0034] (3) Use 10% ammonia solution to adjust the pH of the above-mentioned pyrolusite leachate to 5-6, so that the ferric iron is precipitated as ferric hydroxide; then add barium sulfide under constant stirring to make the Ni in the pyrolusite leac...

Embodiment 3

[0038] (1) Add 30g of pyrolusite into the reaction vessel, then add 3 M sulfuric acid solution with a volume of 450ml, and then add 50g of crushed dry straw (length after crushing is 2-4 mm). The reaction was carried out in the reaction device for leaching pyrolusite with straw straw as provided in the examples.

[0039] (2) Turn on the stirring device and heat the solution to 95 0 C, continuously stirring the reaction at this temperature for 15 hours. After the reaction is completed, cool to room temperature, first remove the straw stalks on the surface, filter, then filter the remaining solution, wash the filter residue with water for 3 times, and combine the two filtrates. The leaching rate is greater than 96.4%.

[0040] (3) Use 10% ammonia solution to adjust the pH of the above-mentioned pyrolusite leachate to 5-6, so that the ferric iron is precipitated as ferric hydroxide; then add barium sulfide under constant stirring to make the Ni in the pyrolusite leachate 2+ 、C...

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Abstract

The invention provides a method for preparing high-purity manganese sulfate through extracting low-grade pyrolusite by using rice straw. The method comprises the steps of adding a sulfuric acid solution and dry rice straw into pyrolusite, reacting at the temperature of 70-950 DEG C for 8-15h while continuously stirring, and filtering to obtain pyrolusite leachate; respectively removing heavy metal ions such as iron ions, Ni<2+> and Co<2+> as well as calcium and magnesium ions by using an ammonia solution, barium sulfide and ammonium fluoride to obtain an initial solution of manganese sulfate; adding ammonium carbonate to form a white sediment, filtering, mixing the obtained solid and 500-DEG C water, stirring for 10 minutes, filtering, mixing the obtained solid and 500-DEG C water, stirring for 10 minutes, and then, filtering to obtain solid manganese carbonate; and adding the sulfuric acid solution to completely dissolve the solid manganese carbonate, continuing to stir for 30 minutes, heating to concentrate the solution, crystallizing, centrifugally dehydrating, and drying in hot air to obtain high-purity solid manganese sulfate. By using the method, the process flow is simplified, the operation condition is improved, the energy consumption is greatly reduced, and the industrial application prospect is huge.

Description

technical field [0001] The invention relates to a process for leaching manganese from low-grade pyrolusite and finally obtaining high-purity manganese sulfate by using straw acid hydrolyzate as a reducing agent, belonging to the field of hydrometallurgy. Background technique [0002] Manganese ore resources are very rich in our country. At present, more than 20 provinces, municipalities and autonomous regions in our country have discovered and surveyed manganese ore. According to preliminary statistics, there are more than 200 manganese mines identified in mainland my country, and manganese mines are mainly distributed in the central-southern and southwestern regions. These two regions account for more than 80% of the country's total reserves, including Guangxi, Hunan, Guizhou, Sichuan, etc. Provinces are the main storage areas of manganese ore, forming a pattern dominated by Guangxi and Hunan provinces. Among manganese ore resources, the reserves of pyrolusite resources are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/08C22B47/00C01G45/10
CPCY02P10/20
Inventor 易清风
Owner HUNAN UNIV OF SCI & TECH
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