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Preparation method of ultra-pure vanadium pentoxide

A technology for vanadium pentoxide and vanadium precipitation is applied in the field of preparation of vanadium pentoxide, which can solve problems such as unfavorable industrial production, difficult and unsatisfactory control of product impurities, simplification of operation flow and technological difficulty, and stable product index. Good sex, the effect of reducing the dosage of medicine

Inactive Publication Date: 2016-07-27
HEBEI IRON AND STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, the pH value is strictly required in this method, the pH value needs to be adjusted many times, the operation is cumbersome, and it is not conducive to industrial production.
[0014] The above method, the highest purity of the obtained high-purity vanadium pentoxide product is still lower than 99.92%, and the product impurities are difficult to control stably. The above method cannot simultaneously remove iron ions, chromium ions, manganese ions, silicate ions, phosphate ions , calcium ions, sodium ions, magnesium ions, potassium ions and aluminum ions to make their content less than 0.005%. High requirements, unable to fully meet the demand for high-end vanadium products

Method used

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  • Preparation method of ultra-pure vanadium pentoxide

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Effect test

Embodiment 1

[0090] 1) Pre-removal of impurities: the vanadium-containing solution obtained by extracting vanadium from vanadium slag by sodium roasting method is used as a vanadium-containing solution (containing 24.8g / L of vanadium, 92ppm of iron, 351ppm of chromium, 25ppm of manganese, 264ppm of phosphorus, and 650ppm of calcium calcium 59ppm, magnesium 33ppm, aluminum 21ppm, sodium 19.8g / L, potassium 1.5g / L), the dosage of soluble calcium salt is added with the molar ratio=1.1:1 of phosphorus element in its calcium-containing element and vanadium-containing solution, soluble aluminum salt The amount of feed is added according to the molar ratio of the aluminum-containing element to the silicon element in the vanadium-containing solution = 1.2:1, stirred and reacted at 70°C for 30 minutes, and filtered to obtain the pre-removed impurity liquid and the impurity-removed mud;

[0091] 2) Precipitation of vanadium by calcification: add calcium oxide to the pre-removed liquid obtained in step...

Embodiment 2

[0100] 1) Pre-removal of impurities: use the vanadium-containing solution obtained by extracting vanadium from stone coal as the vanadium-containing solution (containing 50.4g / L of vanadium, 25ppm of iron, 110ppm of chromium, 115ppm of manganese, 363ppm of phosphorus, 1521ppm of silicon, 26ppm of calcium, 32ppm of magnesium, aluminum 7ppm, sodium 135ppm, potassium 15ppm), the soluble calcium salt dosage is added with the mol ratio=1.2:1 of phosphorus element in its calcium-containing element and vanadium-containing solution, and the soluble aluminum salt dosage is added with its aluminum-containing element and vanadium-containing solution The molar ratio of silicon element = 1.3:1 was added, stirred and reacted at 80°C for 40 minutes, and filtered to obtain the pre-removed impurity liquid and impurity-removed mud;

[0101] 2) calcification vanadium precipitation: to step 1) add calcium hydroxide in the liquid dissolving liquid after pre-removal of impurities, the charging capac...

Embodiment 3

[0110] 1) Pre-removal of impurities: the vanadium-containing solution obtained by the secondary vanadium-containing waste extraction vanadium is used as the vanadium-containing solution (containing 28.51g / L of vanadium, 33ppm of iron, 28ppm of chromium, 285ppm of manganese, 465ppm of phosphorus, 121ppm of silicon, 16ppm of calcium, magnesium 76ppm, aluminum 33ppm, sodium 16.35g / L, potassium 933ppm), the mol ratio of soluble calcium salt to the phosphorus element in the solution containing calcium and vanadium=1.35:1 is added, and the soluble aluminum salt is charged according to its aluminum content The molar ratio of the element to the silicon element in the vanadium-containing solution = 1.4:1 was added, stirred and reacted at 100°C for 15 minutes, and filtered to obtain the pre-removed impurity liquid and the impurity-removed mud;

[0111] 2) Calcification of vanadium precipitation: add calcium oxide to the pre-removed liquid obtained in step 1), the feeding amount of calciu...

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Abstract

The invention discloses a preparation method of ultra-pure vanadium pentoxide. The preparation method comprises the following steps of: removing impurities in advance; transferring phosphorus and silicon in a vanadium-containing solution into a solid phase for removal; performing calcification and vanadium precipitation; transferring vanadium in a liquid phase into a calcium vanadate phase; leaving the impurities such as chromium, manganese, potassium and sodium in the liquid phase for removal; performing solubilization reaction of vanadium in the calcium vanadate into the liquid phase through ammonium bicarbonate and / or ammonium carbonate; leaving the calcium, phosphorus, silicon, iron and magnesium in the solid phase for removal; replacing residual trace cations of the liquid phase with ammonium ions by an ammonium type cation exchange system to realize deep purification; and performing cooling vanadium precipitation and deamination calcination to obtain vanadium pentoxide. In the invention, the process route is simple, the drug consumption is low, the vanadium pentoxide with purity of over 99.95% can be stably obtained, and the content of main impurities such as iron, chromium, manganese, silicon, phosphorus, calcium, sodium, magnesium, potassium and aluminum is all lower than 0.002%.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy, and relates to a preparation method of vanadium pentoxide, in particular to a preparation method of vanadium pentoxide with a purity ≥ 99.95%. Background technique [0002] With the advancement of science and technology, the application fields and scope of vanadium continue to expand, and some downstream high-end, high-tech, and deep-processed products of vanadium have put forward higher requirements for the grade of their raw material vanadium oxides, especially vanadium pentoxide. The existing national standard purity, especially the specific element index, has been difficult to meet the requirements of these high-end products. At present, the most important high-end products in the vanadium application field include aerospace-grade vanadium-aluminum alloys, electrolytes for all-vanadium redox flow batteries, nano-scale vanadium functional materials, series of vanadium catalysts and vanadium lumi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2006/80
Inventor 祁健陈东辉李兰杰高明磊常福增刘静
Owner HEBEI IRON AND STEEL
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