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Method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore

A technology of vanadium pentoxide and leaching solution, applied in the direction of improving process efficiency, can solve the problems of ammonium salt or sodium salt pollution, excess impurities, ammonia pollution and other problems, and achieve the effect of ensuring purity

Inactive Publication Date: 2011-09-14
BEIJING GENERAL RES INST OF MINING & METALLURGY
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Problems solved by technology

[0006] At present, the low-vanadium solution containing impurities is basically treated by reduction-extraction-extraction-oxidation neutralization and precipitation of vanadium to obtain polyvanadate and then calcined to obtain vanadium pentoxide. The technology of vanadium stripping solution in the process of treatment involves ammonium oxide. Precipitate vanadium with salt, or use lye such as sodium carbonate and sodium hydroxide to deposit vanadium. The solution after vanadium precipitation must be reprocessed, and if acid is used as stripping agent, the pH needs to be neutralized to about 2.0 before vanadium precipitation. The process will produce pollution problems such as ammonium salt or sodium salt. During the calcination process, there will be ammonia pollution or other impurities in the product exceeding the standard, and the neutralization process will waste a lot of acid and alkali, which are not in line with green chemistry and process economy. in principle

Method used

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  • Method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore
  • Method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore

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Experimental program
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Effect test

Embodiment 1

[0045] The leaching solution obtained by directly acid leaching stone coal vanadium ore with sulfuric acid contains 1.69g / L of vanadium. The vanadium solution obtained after neutralization and reduction pretreatment contains vanadium 1.60g / L, pH is 1.5, solution potential is 180mV, 10% P204+90% sulfonated kerosene (volume ratio) is used as the extraction organic phase, and the temperature is 35°C Compared with O / A=1:2.5 countercurrent 6-stage extraction, the raffinate contains less than 0.02g / L of vanadium. The loaded organic phase is back-extracted with 150g / L of sulfuric acid, and the back-extraction condition is compared to O / A=10:1, 4 stages of countercurrent back-extraction, and the stripping solution obtained contains vanadium 33.20g / L (fold V 2 o 5 59.23g / L), H 2 SO 4 80.38g / L. Add hydrogen peroxide to the stripping solution to oxidize to a solution potential of 900mV, maintain at 60°C for 30 minutes, then raise the temperature to 100°C, and continue to hydrolyze ...

Embodiment 2

[0047] The leaching solution obtained by direct acid leaching stone coal vanadium ore with sulfuric acid contains 6.2g / L of vanadium. The solution treated by Zhonghe reduction contains 6.1g / L of vanadium, pH is 2.3, and solution potential is 310mV. Using 25% P204+75% sulfonated kerosene (volume ratio) as the extraction organic phase, at a constant temperature of 35°C, compared O / A=1:1 countercurrent 6-stage extraction, the raffinate contains less than 0.05g / L of vanadium. The loaded organic phase was supplemented with acid to 150g / L after oxidative hydrolysis, and the stripping conditions were 8:1, 5-stage countercurrent stripping, and the obtained stripping solution contained vanadium 52g / L and H2SO4 40.29g / L. Hydrogen peroxide was added to the stripping solution, and it was oxidized and hydrolyzed at 100°C, and the vanadium precipitation was continuously hydrolyzed for 3 hours to obtain the vanadium precipitation intermediate product and the vanadium precipitation solution. ...

Embodiment 3

[0049] The leaching solution obtained by directly acid leaching stone coal vanadium ore with sulfuric acid contains 3.89g / L of vanadium. The vanadium solution obtained after neutralization and reduction pretreatment contains vanadium 3.60g / L, pH is 2.1, solution potential is 250mV, 15%P204+85%sulfonated kerosene (volume ratio) is used as the extraction organic phase, and the temperature is constant at 35°C Compared with O / A=1:1 countercurrent 6-stage extraction, the raffinate contains 0.02g / L of vanadium. The acidity of the loaded organic phase after oxidative hydrolysis is 137.03g / L, containing 8.54g / L of vanadium, and the stripping conditions are 10:1, 5-stage countercurrent stripping, and the obtained stripping solution contains 42.1g / L of vanadium, H2SO4 74.65g / L. Add persulfation to the stripping solution until the potential of the solution is 900mV, maintain it at 60°C for 30 minutes, then raise the temperature to 80°C, and continue to hydrolyze the vanadium precipitati...

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Abstract

The invention relates to a method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore, particularly a method for preparing high-purity vanadium pentoxide from sulfuric acid leach liquor of low-impurity-content stone coal vanadium ore. The method is characterized by sequentially comprising the following steps: (1) extracting leach liquor, which is obtained by leaching stone coal vanadium ore with sulfuric acid, to remove impurities; (2) carrying out back extraction on sulfuric acid to carry an organic phase; (3) oxidizing the back extraction liquor; (4) carrying out hydrolysis to precipitate vanadium; and (5) calcining the vanadium precipitate slag to obtain the vanadium pentoxide. Compared with the traditional technique, by using oxydol, persulfuric acid and the like as oxidants in the oxidation process, the method provided by the invention can avoid introducing other impurity cations, thereby ensuring the purity of the product vanadium pentoxide. Compared with the traditional ammonium-salt vanadium-precipitation technique, the method provided by the invention saves the alkali consumption required by neutralization. The purity of the prepared vanadium pentoxide is up to 99.9%, and the recovery rate of vanadium is up to above 98%; and meanwhile, the invention can implement no pollution and cyclic utilization of the back extraction agent.

Description

technical field [0001] The invention discloses a method for preparing vanadium pentoxide from sulfuric acid leaching solution of stone coal vanadium ore, and relates to a method for preparing high-purity vanadium pentoxide from sulfuric acid leaching solution of stone coal vanadium ore containing low impurities. technical background [0002] Vanadium has a high melting point and is often called refractory metal together with niobium, tantalum, tungsten and molybdenum. It has good ductility, hard quality, resistance to hydrochloric acid and sulfuric acid, and better resistance to gas-salt-water corrosion than most stainless steels. Therefore, vanadium is widely used in metallurgy, chemical industry and steel industry. With the rapid development of my country's modernization, the demand for vanadium and its compounds is increasing. [0003] my country's vanadium resources are mainly stored in stone coal vanadium ore. It is estimated that the vanadium reserves in my country's...

Claims

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Application Information

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IPC IPC(8): C22B3/26C22B34/22
CPCY02P10/20
Inventor 王成彦尹飞居中军杨永强李强陈永强揭晓武阮书峰王振文
Owner BEIJING GENERAL RES INST OF MINING & METALLURGY
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