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A method for deep separation of molybdenum and vanadium in molybdenum-vanadium-containing solution

A separation method and solution technology are applied in the preparation of vanadium compounds, the preparation of molybdenum compounds, chemical instruments and methods, etc., which can solve the problems of large amount of waste water, high cost, long process flow, etc. The effect of convenience and short process flow

Inactive Publication Date: 2017-06-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ion exchange or extraction can carry out deep vanadium removal, but because the enrichment process of molybdenum already has a similar process, it leads to long process flow, large amount of waste water and high cost in the whole process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 20L heavy oil hydrogenation desulfurization waste catalyst alkaline leaching liquid and obtain V-containing 2 o 5 0.9g / L, Mo4.3g / L solution, adding sulfuric acid to the solution to adjust the solution [H + ] is 0.5mol / L, add the solution containing low-valent molybdenum according to the reduction of vanadium in the solution from V (V) to 1.1 times of the theoretical amount of V (IV), and react at 50 ° C for 1 hour. The solution containing low-valent molybdenum is obtained by dissolving ammonium molybdate into an acidic solution with a pH value of 0 and feeding sulfur dioxide under pressure for reduction. Add sodium carbonate to the solution after reduction to adjust the pH of the solution to 5.0, precipitate the oxides of tetravalent vanadium, filter the oxides of tetravalent vanadium and the solution after precipitation of vanadium, and calcinate the oxides of tetravalent vanadium at 500 ° C for 3 hours to obtain V 2 o 5 99.1% vanadium pentoxide product; addi...

Embodiment 2

[0026] Take 10L of vanadium-molybdenum-lead ore alkaline leaching solution and obtain V-containing 2 o 5 1.1g / L, Mo 9.1g / L solution, add hydrochloric acid to adjust solution [H + ] is 2mol / L, add MoO by 1.3 times of V(V) in the solution reduced to V(IV) theoretical amount 2 , reacted at 95°C for 3 hours; added sodium hydroxide to the solution after reduction to adjust the pH of the solution to 2.0, then used anion exchange resin D314 to enrich molybdenum, and analyzed with ammonia water to obtain molybdenum ammonium containing Mo 150g / L and V 1.1mg / L salt solution, then adjust the pH of the ammonium salt solution of molybdenum to 9.0, add magnesium chloride to react at 50°C for 1 hour, and filter to obtain the purified liquid; Ammonium molybdate, ammonium tetramolybdate is dried at 90°C to obtain ammonium tetramolybdate product, ammonium tetramolybdate contains V 0.0006%; add sodium hydroxide to the solution after molybdenum extraction by ion exchange to adjust the pH of th...

Embodiment 3

[0028] Get Mo 7.9g / L obtained by oxidizing and roasting 10L nickel-molybdenum ore, V 2 o 5 0.4g / L alkaline leaching solution, adding sulfuric acid to the solution to adjust the solution [H + ] is 1.5mol / L, according to the reduction of vanadium in the solution to 1.2 times of the theoretical amount of V(IV), add the solution containing low-valent molybdenum, and react at 60°C for 1 hour. The solution containing low-valent molybdenum is to dissolve ammonium molybdate into [H + ] is obtained by adding zinc to 1mol / L acidic solution for reduction. Add potassium carbonate to the solution after reduction to adjust the pH of the solution to 5.0, precipitate the oxides of tetravalent vanadium, filter the oxides of tetravalent vanadium and the solution after precipitation of vanadium, calcinate the oxides of tetravalent vanadium at 500 ° C for 3 hours, and obtain the oxides containing V 2 o 598.9% vanadium pentoxide product; add sulfuric acid to the solution after vanadium precip...

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Abstract

The invention relates to a method for deeply separating molybdenum and vanadium in a solution containing the molybdenum and the vanadium. The method includes: regulating the acidity [H<+>] of the solution containing the molybdenum and the vanadium to be 0.0003-10mol / L, and then using the compound of Mo(IV) or / and Mo(V) as the reducing agent to selectively reduce the vanadium in the solution to obtain liquid after reduction; regulating the pH of the liquid after reduction to be 4-7, settling the vanadium, and using an ion exchanging method or extraction method to enrich the molybdenum; or regulating the pH of the liquid after reduction to be 2-4, using an ion exchanging method or extraction method to enrich the molybdenum, then regulating the pH to 4-7, and settling the vanadium. The method has the advantages that the E<0>Mo(VI) / Mo(V) and E<0>V(V) / V(IV) potential differences under an acidic condition are utilized, the compound of Mo(IV) or / and Mo(V) as the reducing agent to selectively reduce the V(V) in the solution into V(IV), and the maximum differentiation of the properties of the molybdenum and the vanadium in the solution is achieved; the property that anion exchange resin or basic extractant can only selectively enrich the Mo(VI) in the solution and cannot absorb the V(IV) is utilized to deeply separate the molybdenum and the vanadium; the method is simple in process, short in process flow, convenient to operate, good in molybdenum-vanadium separation effect, low in treatment cost, environmental friendly, suitable for industrial application, and the like.

Description

technical field [0001] The invention relates to a deep separation method for molybdenum and vanadium in a molybdenum-vanadium-containing solution. Background technique [0002] Molybdenum and vanadium are diagonally adjacent to each other in the periodic table, and have similar properties. They often exist in minerals in a symbiotic manner in nature. Nickel-molybdenum ore, vanadium-molybdenum-lead ore, and stone coal are typical representatives of such minerals. During the alkaline leaching process of these minerals, molybdenum and vanadium enter the solution in the form of molybdate and vanadate, respectively. In addition, the process of extracting molybdenum from waste petroleum catalysts and high-impurity ferromolybdenum alloys formed by smelting nickel-molybdenum ores will also form alkaline leach solutions containing molybdenum and vanadium. The characteristics of this type of molybdenum-vanadium-containing solution are usually: the system is an alkaline system, the M...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02C01G39/00
CPCC01G31/003C01G31/02C01G39/00C01G39/003C01P2006/80
Inventor 王明玉王学文陈边防孟钰麒
Owner CENT SOUTH UNIV
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