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Comprehensive recovery method for extracting ferrovanadium from stone coal acid immersion liquid

A recovery method, stone coal acid technology, applied in the direction of improving process efficiency, etc., can solve the problems of difficult liquid-solid separation, long process flow, difficult extraction and phase separation, etc., to reduce environmental pollution, avoid ammonia nitrogen wastewater, and facilitate liquid-solid separation effect

Inactive Publication Date: 2011-07-20
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, the leaching solution is reduced and extracted first, and then back-extracted and oxidized. The process is long, the consumption of reagents is large, and the production cost is high. Moreover, if the solution is recycled after vanadium extraction, a large amount of sulfate will accumulate, the viscosity of the solution will be high, and the extraction and phase separation will be difficult. , direct discharge of large environmental pollution
The stone coal sulfuric acid leaching solution is oxidized and ion exchanged after iron removal. Since a lot of reducing organic matter enters the solution during the stone coal acid leaching process, not only the amount of oxidant used in the vanadium oxidation process is large, but also the oxidation is not complete, which affects the exchange capacity of the resin.
Although the precipitation effect of iron and vanadium compounds in the sulfuric acid leaching solution of stone coal is good, the obtained iron hydroxide colloidal precipitate is difficult to separate liquid and solid, and there are many impurities entrained
In addition, no matter what kind of process the vanadium precipitation process will produce ammonia nitrogen wastewater, and the iron in the sulfuric acid leaching solution of stone coal cannot be comprehensively utilized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] with V 2 o 5Add 3000ml of stone coal acid leaching solution containing 3.83g / L vanadium, add ammonia water to adjust the pH value to 3.0 to remove aluminum by crystalline ammonium aluminum sulfate alum, and oxidize ferrous iron, ferric vanadium and tetravalent vanadium according to the oxidation of ferrous iron in the solution Add sodium chlorate to 1.5 times the stoichiometric amount of pentavalent vanadium, add jarosite as a seed crystal and stir at 85°C for 1 hour to precipitate a mixture of vanadium-containing jarosite and jarosite, a mixture of vanadium-containing jarosite and jarosite According to the solid-liquid ratio of 1:3g / ml, add NaOH to control the pH value of 13, 80°C, stir and leach for 1.5 hours and filter, the filter residue is calcined at 350°C for 2 hours to obtain iron red with a purity of 99.5%, and the filtrate is 85°C Add sulfuric acid to adjust the pH value 1.5 Precipitate vanadium, filter and wash to obtain red vanadium filter cake, red cake is...

Embodiment 2

[0032] with V 2 o 5 1000ml of stone coal acid leaching solution containing vanadium 9.31g / L, according to NH 4 Al(SO 4 ) 2 12H 2 1.5 times of the stoichiometric number of O crystal precipitation is added in the leaching solution (NH 4 ) SO 4 , to remove aluminum by crystallization, and add CaCO to the liquid after crystallization 3 Neutralize until the pH value is filtered to 2.0, and the filtrate is oxidized to ferric iron by ferrous iron and oxidized by trivalent vanadium and tetravalent vanadium to 1.5 times of the stoichiometric number of pentavalent vanadium. The mixture of vanadium jarosite and jarosite is used as the crystal seed and stirred and leached at 60°C for 2.0 hours, and the mixture of vanadium-containing jarosite and jarosite is precipitated, and the mixture of vanadium-containing jarosite and jarosite is at a solid-to-liquid ratio of 1:4.5g / ml, adding the mixed solution of sodium hydroxide and sodium carbonate obtained in Example 1, stirring and leach...

Embodiment 3

[0034] with V 2 o 5 Measure the stone coal pickling solution 500ml that contains vanadium 20.15g / L, add the ammonium sulfate regeneration solution that embodiment 2 obtains, crystallize out aluminum ammonium sulfate alum NH 4 Al(SO 4 ) 2 12H 2 O crystals were filtered, and CaCO was added to the solution after crystallization 3 Neutralize until the pH value is filtered to 1.8, and the filtrate is oxidized to ferric iron and trivalent vanadium and tetravalent vanadium to 1.5 times the stoichiometric number of pentavalent vanadium by ferrous iron and adds sodium persulfate, adding the obtained in Example 1 The mixture of vanadium-containing jarosite and jarosite is used as the crystal seed and stirred and leached at 95°C for 1 hour, and the mixture of vanadium-containing jarosite and jarosite is precipitated, and the precipitation mixture is at a solid-to-liquid ratio of 1:2.5g / ml, and potassium hydroxide is added Control the pH value at 12.5, 55°C, stir and leach for 3 hour...

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Abstract

The invention relates to a comprehensive recovery method for extracting ferrovanadium from stone coal acid leaching liquid. The process mainly comprises the following steps of: crystallizing a stone coal sulfuric acid leaching liquid into ammonium aluminum alum sulfate and adding a pH value regulator to the crystallized liquid at a room temperature; oxidizing, precipitating and separating out crystallized liquid into a mixture containing ammonium jarosite and ammoniojarosite, leaching the vanadium-contained mixture separated from the precipitate in alkaline to obtain alkaline leaching liquid and alkaline leaching slag; adding sulphuric acid to the alkaline leaching liquid to acidify and precipitate vanadium pentoxide, calcining, washing and drying the vanadium pentoxide to obtain a refined vanadium product, calcining the alkaline leaching slag to obtain ferric oxide or adding sulphuric acid to dissolve, concentrate and crystallize to obtain polymerase ferric sulfate; and transforming the ammonium aluminum alum sulfate and regenerating vanadium precipitation mother liquor alkali, and the like. The invention has the advantages of good product quality, less reagent amount, low production cost, environmental protection, and the like.

Description

technical field [0001] The invention relates to a comprehensive recovery method for extracting vanadium and iron from stone coal acid leaching solution. Background technique [0002] Stone coal is an important vanadium metallurgical mineral resource, and the common process for extracting vanadium from stone coal is sulfuric acid leaching. The current techniques for extracting vanadium from stone coal acid leaching solution include: [0003] 1) Stone coal sulfuric acid leaching solution → reduction → extraction → stripping → oxidation → ammonium salt precipitation of vanadium → calcination to obtain refined vanadium; [0004] 2) Stone coal sulfuric acid leaching solution → ammonium salt removal of aluminum → selective oxidation of iron removal → vanadium oxidation → ion exchange → desorption → ammonium salt precipitation of vanadium → calcination to obtain refined vanadium; [0005] Or stone coal sulfuric acid leaching solution → ammonium salt removal of aluminum → selectiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/22C22B3/44
CPCY02P10/20
Inventor 王学文王明玉
Owner CENT SOUTH UNIV
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