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Method for preparing vanadyl oxalate from vanadium slag through short process

A technology of vanadyl oxalate and vanadyl oxalate solid, which is applied in the direction of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., and can solve the problems of high production cost, long process flow, complex vanadyl oxalate process, etc. Achieve the effect of low production cost and short process

Active Publication Date: 2019-10-22
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To obtain vanadium pentoxide or other vanadium-containing intermediates, complex processes such as leaching-removing impurities-precipitating vanadium-calcining are required, resulting in a complex process for the production of vanadium oxalate, a long process flow, and high production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The vanadium slag comprising the composition listed in Table 1 is crushed to 0.074mm and accounts for 70%. 100g of vanadium slag is mixed with 10g of calcium carbonate. ℃, the roasting time is 60min; add 200ml pure water to the clinker obtained by roasting, add 40g oxalic acid to control the pH of the system to 3.7, control the leaching temperature at 90℃, stir and leaching for 60min, filter to obtain the vanadium-containing leaching solution and residue; the vanadium-containing solution Carry out concentrated crystallization, and obtain vanadyl oxalate solid after solid-liquid separation.

[0028] The vanadyl oxalate solid prepared in this embodiment is detected by ICP, and its purity is 99.13wt%.

Embodiment 2

[0030] The vanadium slag comprising the ingredients listed in Table 1 is crushed to 0.074mm and accounts for 80%, 100g of vanadium slag is mixed with 8g of calcium oxide, and then the resulting mixture is added to a muffle furnace and fed with air for high-temperature roasting, and the roasting temperature is controlled to be 950 ℃, the roasting time is 100min; add 300ml pure water to the clinker obtained by roasting, add 30g oxalic acid to control the pH of the system to 4.6, control the leaching temperature at 90℃, stir and leaching for 45min, filter to obtain the vanadium-containing leaching solution and residue; the vanadium-containing solution Carry out concentrated crystallization, and obtain vanadyl oxalate solid after solid-liquid separation.

[0031] The vanadyl oxalate solid prepared in this embodiment is detected by ICP, and its purity is 99.57wt%.

Embodiment 3

[0033] The vanadium slag containing the ingredients listed in Table 1 is crushed to 0.074mm, accounting for 85%. Take 100g of vanadium slag and put air into the muffle furnace for high-temperature roasting. The roasting temperature is controlled to be 900°C, and the roasting time is 120min; Add 400ml of pure water to the material, add 40g of oxalic acid to control the pH of the system to 3.1, control the leaching temperature at 60°C and stir for 30 minutes, filter to obtain the vanadium-containing leachate and residue; concentrate and crystallize the vanadium-containing solution, and obtain oxalic acid oxygen after solid-liquid separation. Vanadium solid

[0034] The vanadyl oxalate solid prepared in this embodiment is detected by ICP, and its purity is 99.82wt%.

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Abstract

The invention discloses a method for preparing vanadyl oxalate from vanadium slag through a short process, and belongs to the technical field of preparation for vanadyl oxalate. The method for preparing vanadyl oxalate from the vanadium slag through the short process comprises the following steps: roasting the vanadium slag to obtain roasted clinker; adding water and oxalic acid into the roasted clinker, and leaching and filtering; and concentrating and crystallizing a filtrate, and then carrying out solid-liquid separation to obtain vanadyl oxalate solid. According to the method for preparingvanadyl oxalate from the vanadium slag through the short process, oxalic acid is taken as a leaching agent, and on one hand, an acidic environment is provided for dissolving out vanadium from the clinker; and on the other hand, ferrous oxalate, calcium oxalate, manganese oxalate, magnesium oxalate and aluminum oxalate which have extremely low solubility are formed with iron, calcium, manganese, magnesium and aluminum in the clinker, and then the impurity elements are prevented from entering a leaching solution, so that one-step completion of leaching for vanadium and separation for the impurities is realized, and short process and low production cost are achieved.

Description

technical field [0001] The invention belongs to the technical field of vanadyl oxalate preparation, and in particular relates to a method for preparing vanadyl oxalate in a short process from vanadium slag. Background technique [0002] Vanadyl oxalate is a precursor for the preparation of various vanadium-based functional materials, and has a wide range of uses, such as the preparation of nano-vanadium nitride powder by aminolysis of vanadyl oxalate, and the preparation of nano-vanadium dioxide powder by thermal decomposition of vanadyl oxalate. At present, the raw materials used in the preparation of vanadyl oxalate are the end products of vanadium extraction, such as vanadium pentoxide and sodium vanadate. For example, CN104974028A uses vanadium pentoxide as raw material, and reacts with oxalic acid at 100-200°C to obtain vanadyl oxalate; CN106380389A uses sodium vanadate as raw material, and obtains vanadyl oxalate through precipitation-dissolution-crystallization proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/04C22B34/22C07C51/41C07C55/07
CPCC07C51/412C22B7/007C22B7/04C22B34/22C07C55/07Y02P10/20
Inventor 杨晓刘波姚洁
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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