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Method for preparing vanadium oxide

A technology of vanadium oxide and vanadium slag, applied in the field of preparation of vanadium oxide, can solve the problems of increased control difficulty, difficult handling, inconvenient stacking, etc., and achieve the effect of reducing production cost and reducing reagent consumption

Inactive Publication Date: 2013-06-12
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent documents CN85102378, CN201110082443.6, CN201110197357.X, CN86108218 and CN200810001589.1 provide methods for producing vanadium oxide by sodium roasting of vanadium slag, and the residue obtained after sodium roasting-water immersion contains pentavalent vanadium and six Valence chromium, which is hazardous waste residue, is not easy to handle; the residue cannot be returned to the ironmaking blast furnace for secondary use because it contains about 6% sodium oxide; the by-product sodium sulfate produced in the wastewater treatment process contains vanadium, chromium and ammonium sulfate and is easily Soluble in water, inconvenient to stack, the above problems have greatly affected the application of vanadium slag sodiumization vanadium extraction process
[0004] Patent documents CN200710202445.8, CN200810305602.2, CN200810305603.7, CN200810305601.8 provide a method for producing vanadium oxide by calcification roasting of vanadium slag-sulfuric acid leaching. High-phosphorus vanadium slag; leaching with sulfuric acid requires very low metal iron content in the fine powder vanadium slag, which increases the difficulty of control; the residue needs to be re-used after calcium sulfate is removed
[0005] Patent document CN201210066735 provides a vanadium extraction method for ammonium carbonate leaching vanadium slag clinker, that is, using 200-800g / L ammonium carbonate solution according to the liquid-solid ratio (mL:g) 5:1-30:1 at 60-98 ℃ for leaching, this method has the problem of large consumption of leaching agent, and the large amount of ammonium carbonate decomposition will affect the operating environment

Method used

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preparation example Construction

[0011] The method for preparing vanadium oxide according to the present invention comprises the following steps carried out in sequence: vanadium slag is mixed with calcium oxide or limestone to form a mixed material, so that the CaO / V in the mixed material 2 o 5 The weight ratio is 0.25 to 0.65, which can control the vanadium in the calcified roasting clinker, with calcium metavanadate as the main form, because the solubility of calcium metavanadate in water is larger than that of calcium pyrovanadate and calcium orthovanadate, which is conducive to leaching ; Roast the mixed material to obtain calcified clinker; use C at 80-95°C 2 o 4 2- The oxalate solution with a concentration of 35-70g / L is used to leach the calcified clinker; after the leaching reaction is completed, the solid-liquid separation is carried out to obtain the vanadium-containing leaching solution and residue; the vanadium-containing leaching solution is desiliconized so that the Silicon concentration 4 ...

example 1

[0032] Ordinary vanadium slag (containing V 2 o 5 17.2%, CaO1.84%, P0.04%) 100g mixed with calcium oxide 5g evenly, the mixture CaO / V 2 o 5 0.4; the mixture is roasted in a muffle furnace for 180 minutes at a roasting temperature of 850°C and air ventilated; the roasted clinker is crushed to a particle size of no more than 0.1mm and then added to 400mL of sodium oxalate 35g / L+ammonium oxalate 40g / L In the oxalate solution, stirring and leaching at a slurry temperature of 90°C for 120 minutes; after the leaching reaction, solid-liquid separation to obtain a vanadium-containing leaching solution and residue, the residue TV is 0.95wt%, and the vanadium transfer leaching rate is 89.8%; Add 0.8g of sodium aluminate, stir for 20min and then filter to obtain the filtrate; add 10g of ammonium oxalate to the filtrate and stir for 1h, cool to room temperature and let stand for 12h before filtering to obtain ammonium metavanadate and vanadium precipitation wastewater, vanadium precipit...

example 2

[0035] Ordinary vanadium slag (containing V 2 o 5 17.2%, CaO1.84%, P0.04%) 100g mixed with calcium oxide 3g evenly, the mixture CaO / V 2 o 5 0.28; the mixture is roasted in a muffle furnace for 60 minutes at a roasting temperature of 900°C and air ventilated; the roasted clinker is crushed to a particle size of no more than 0.1mm and then added to 600mL of sodium oxalate 30g / L+ammonium oxalate 25g / L In the oxalate solution, stirring and leaching at a slurry temperature of 95°C for 120 minutes; after the leaching reaction, solid-liquid separation to obtain a vanadium-containing leaching solution and residue, the residue TV 1.01wt%, vanadium transfer leaching rate 89.5%; into the leaching solution Add 0.8g of sodium aluminate, stir for 20min and then filter to obtain the filtrate; add 18g of ammonium oxalate to the filtrate and stir for 1h, cool to room temperature and let stand for 12h before filtering to obtain ammonium metavanadate and vanadium precipitation wastewater, vana...

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Abstract

The invention provides a method for preparing vanadium oxide, which comprises the following steps of: mixing vanadium slag with calcium oxide or limestone to form a mixed material; roasting the mixed material to obtain calcified clinker; leaching the calcified clinker by using C2O4<2-> and 35-70 g / L of oxalate solution at 80-95 DEG C; after leaching, carrying out solid-liquid separation to obtain vanadium-containing leachate and residues; removing silicon from the vanadium-containing leachate, so that the silicon concentration in the vanadium-containing leachate is less than 0.1 g / L, then adding ammonium oxalate into the vanadium-containing leachate, adjusting the mol ratio of NH4<+> to TV to 2-3.5, precipitating ammonium metavanadate, and filtering to obtain ammonium metavanadate and vanadium precipitation wastewater; and oxidizing, roasting and deaminizing ammonium metavanadate to prepare vanadium pentoxide or reducing to prepare vanadium trioxide. According to the invention, on the premise of satisfying environment-friendly requirements, preparation of vanadium oxide from ordinary vanadium slag and high-calcium and high-phosphate vanadium slag is realized; furthermore, consumption of reagents can also be reduced; and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of vanadium oxide production, in particular to a method for preparing vanadium oxide. Background technique [0002] Usually, vanadium slag is the main raw material for producing vanadium oxide. At present, the vanadium slag used in industrial production is mainly ordinary vanadium slag, which is characterized by low CaO content, and the general CaO / V 2 o 5 ≤0.15; however, for CaO / V 2 o 5 ≥0.16, P≥0.06% high-calcium and high-phosphorus vanadium slag, because of the high content of CaO, it is not suitable to adopt the process of sodium roasting-water leaching to extract vanadium, and because of the high content of phosphorus, it is not suitable to adopt the process of calcification roasting-sulfuric acid leaching to extract vanadium, so However, the process of extracting vanadium from high-calcium and high-phosphorus vanadium slag has not yet been industrialized. [0003] There are two main industrialized...

Claims

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Application Information

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IPC IPC(8): C22B7/04C22B3/16C22B3/44C22B34/22
CPCY02P10/20
Inventor 付自碧孙朝晖王彬彬张林何文艺申彪
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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