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Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon

A silicon solution, vanadium-chromium technology, applied in the field of preparing low-silicon and high-purity V2O5, and preparing low-silicon V2O5, can solve the problems of vanadate reaching 99.5%, repeated and complicated operations, unfavorable popularization and application, etc., and achieves clear oil-water interface and separation. Good effect and good removal efficiency

Active Publication Date: 2014-07-23
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Related technologies such as CN101121962 adopt operations such as extraction, stripping, and precipitation of vanadium to fully reclaim the vanadium chromium in the vanadium chromium solution, but the purity of its product vanadate can only reach 99.5%
CN103540745A uses amines to extract the heteropolyacid in the vanadium solution to purify the vanadium solution, add ammonium salt to precipitate vanadium and calcined to obtain vanadium pentoxide with a purity greater than 99.9%, but the raw material liquid requires the formation of phosphorus molybdenum tungsten, silicon molybdenum tungsten and other heteropolyacids for impurity removal, but it is no longer suitable for other vanadium-chromium solutions that are difficult to form heteropolyacids
[0006] CN102849795A uses crude ammonium metavanadate as raw material to produce high-purity V 2 o 5 , not only the raw materials are limited, but also the operation is repetitive and complicated, which is not conducive to popularization and application
CN102923776A also uses crude ammonium metavanadate as raw material, and obtains 99.95% V 2 o 5 , but its requirements for equipment are relatively high, and the initial investment is relatively large
[0008] In the current reports, there are few low-silicon and high-purity V 2 o 5 process, so find a suitable process flow, low-cost preparation of low-silicon high-purity V 2 o 5 Urgent need to solve

Method used

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  • Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon
  • Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon

Examples

Experimental program
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Embodiment 1

[0049] A kind of preparation high-purity V from vanadium-chromium-silicon solution 2 o 5 method, including the following steps:

[0050] 1) Put 250ml of a solution containing pentavalent vanadium and hexavalent chromium in a beaker, heat it with a water bath to 90°C and then add 5.86g of AlCl 3 , 1.547g CaO, stirring the reaction for 30min with a stirring paddle, cooling to room temperature and adjusting the pH value to 8.8 with sulfuric acid, stirring for 5 minutes, and centrifuging to separate the solid and liquid;

[0051] 2) Adjust the collected silicon removal solution to 4.2 with sulfuric acid, then mix it with primary amine extractant (containing 10% JMT, 5% hexyl acetate and 85% kerosene) at a ratio of 1:1, and stir at 30°C 5min, stand until the oil and water are completely separated;

[0052] 3) Add sulfuric acid to the raffinate (water phase) to adjust the pH value to 3, then add 1 times the theoretical amount of anhydrous sodium sulfite to the solution, adjust th...

Embodiment 2

[0057] A kind of preparation high-purity V from vanadium-chromium-silicon solution 2 o 5 method, including the following steps:

[0058] 1) Put 500ml of a solution containing pentavalent vanadium and hexavalent chromium in a beaker, heat it with a water bath to 60°C and add 5.86g of Al 2 (SO 4 ) 3 and 0.751g CaCl 2 , after stirring and reacting with a stirring paddle for 40 minutes, cool to room temperature and adjust the pH value to 7.7 with sulfuric acid, and then stir for 10 minutes, then centrifuge to separate the solid and liquid;

[0059] 2) Adjust the collected desiliconization solution to 3.6 with sulfuric acid, and then mix it with primary amine extractant (containing 15% JMT, 5% ethyl p-methylparaformate and 80% kerosene) in a ratio of 2:1, at 25 Stir at ℃ for 20 minutes, and let it stand until the oil and water are completely separated;

[0060] 3) Add sulfuric acid to the raffinate (water phase) to adjust the pH to 3.4, then add 1.03 times the theoretical amo...

Embodiment 3

[0065] A kind of preparation high-purity V from vanadium-chromium-silicon solution 2 o 5 method, including the following steps:

[0066] 1) Put 1000ml of solution containing pentavalent vanadium and hexavalent chromium in a beaker, heat it with a water bath to 70°C and then add 1.056g of Al(OH) 3 and 0.7g CaCl 2 , after stirring and reacting with a stirring paddle for 50 minutes, cool to room temperature and adjust the pH value to 8.0 with sulfuric acid, stir for another 10 minutes, and centrifuge to separate the solid and liquid;

[0067] 2) Adjust the collected desiliconization solution to 3.4 with sulfuric acid, and then mix it with primary amine extractant (containing 15% N1923, 6% ethyl p-methylparaformate and 79% kerosene) in a ratio of 3:1, at 20 Stir at ℃ for 30 minutes, and let it stand until the oil and water are completely separated;

[0068] 3) Add sulfuric acid to the raffinate (water phase) to adjust the pH value to 2.5, then add 1.2 times the theoretical amo...

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Abstract

The invention discloses a method for preparing high-purity low-silicon vanadium pentoxide (V2O5) from a mixed solution containing vanadium, chromium and silicon. The method mainly comprises the following steps: firstly removing the silicon from the solution containing the vanadium, the chromium and the silicon by utilizing amphoteric metal salt and / or alkali metal salt, then also removing other introduced impurities by regulating the pH value of the solution and performing solid and liquid separation; afterwards, selectively extracting most of the vanadium into an organic phase according to a certain phase ratio by use of a primary amine extraction system, then also reversely extracting the vanadium in the organic phase rich in the vanadium by use of an alkaline solution containing ammonium salt, precipitating ammonium metavanadate, filtering or centrifuging the reversely-extracted water phase to obtain a high-purity ammonium metavanadate solid, washing, drying and calcining under a certain temperature to obtain a brick-red substance V2O5, wherein the purity of the V2O5 is above 99.9%, the content of silicon is smaller than 0.007% and no interlayer is formed during the extraction-reverse extraction process. The method disclosed by the invention is used for preparing the high-purity low-silicon V2O5 through processes of intensified silicon removal, extraction, reverse extraction and vanadium precipitation.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy or wastewater treatment, and relates to a method for preparing low-silicon V 2 o 5 The method, especially relates to a kind of preparation low silicon high purity V from vanadium chromium silicon solution 2 o 5 process flow. Background technique [0002] Vanadium is a non-ferrous metal and a very important strategic resource. Vanadium pentoxide (V 2 o 5 ) is an important oxide of vanadium and is also the most widely used oxide. The scope of application has expanded from metallurgy, chemical industry and other industries to aerospace, electronics industry, electrochemistry, etc. 2 o 5 The market demand is increasing, the V 2 o 5 The purity requirements of vanadium are also getting higher and higher, especially the development of vanadium redox flow batteries and vanadium aluminum alloys, which put forward higher requirements for the purity of vanadium and the content of impurity silicon in h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/22C22B3/26C22B3/44
CPCC22B3/44C22B34/22Y02P10/20C01G31/02
Inventor 宁朋歌曹宏斌张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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