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Method for preparing high-purity vanadium from heteropolyacid impurity in amine extraction mode

A heteropoly acid and extraction technology, applied in the direction of improving process efficiency, can solve the problems of low purity and unsatisfactory vanadium products, and achieve significant economic benefits, low equipment requirements, and good thermal stability.

Active Publication Date: 2014-01-29
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

[0004] The technical problem to be solved by the present invention is: in view of the economic downturn of the current vanadium industry, the purity of vanadium products is not high, and cannot meet the requirements for the purity of vanadium products such as vanadium redox flow batteries, catalysts with higher requirements, medical raw materials, and certain luminescent materials at the present stage. To meet this reality, provide a method for preparing high-purity vanadium by extracting heteropolyacid impurities with amines, which can prepare high-purity vanadium pentoxide products through simple operations, with low equipment requirements and good thermal stability of key extraction agents , insensitive to acid and alkali, simple regeneration and recycling methods, easy to industrialize

Method used

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  • Method for preparing high-purity vanadium from heteropolyacid impurity in amine extraction mode

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Experimental program
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Effect test

Embodiment 1

[0021] The chromium-containing vanadium slag leaching liquid is used as the vanadium-containing solution after deep removal of impurities. The solution components are: 16 g / L vanadium, 0.5 g / L chromium, 0.5 g / L tungsten, 0.05 g / L silicon, 0.05 g / L Phosphorus, 0.5 g / L molybdenum, 0.1 g / L arsenic, primary amine N1923, oxime extractant LIX63, n-octanol and kerosene were used to form an organic phase for extraction and separation tests, and the pH value of the feed liquid was adjusted to 6.00. The volume percentage concentration of primary amine is selected as 3%, the volume percentage concentration of LIX63 is 0.8%, and the volume percentage concentration of n-octanol is 0.8%. Minutes, remove the oscillator and let the layers stand for 20 minutes, back-extract the loaded organic phase with 5% sodium hydroxide to regenerate the organic phase, heat the raffinate to 105 degrees, evaporate to about 40g / L, ammonium chloride The solid-to-liquid ratio of the dosing amount and the evapor...

Embodiment 2

[0023] The chromium-containing vanadium slag leaching liquid is used as the vanadium-containing solution after deep removal of impurities. The solution components are: 16 g / L vanadium, 0.5 g / L chromium, 0.5 g / L tungsten, 0.05 g / L silicon, 0.05 g / L Phosphorus, 0.5 g / L molybdenum, 0.1 g / L arsenic, quaternary ammonium salt N263, trialkylphosphorous oxide TRPO, n-hexanol and toluene are used to form an organic phase, and the extraction and separation test is carried out. The pH value of the feed solution is adjusted to 6.50, and the extraction The volume percentage concentration of primary amine is 4%, the volume percentage concentration of LIX63 is 1.0%, and the volume percentage concentration of n-octanol is 1.0%. The extraction temperature is room temperature 25°C. After 20 minutes, remove the shaker and let it stand for 10 minutes to separate the layers. The loaded organic phase is back-extracted with 5% potassium hydroxide to regenerate the organic phase. The raffinate is heat...

Embodiment 3

[0025] The chromium-containing vanadium slag leaching liquid is used as the vanadium-containing solution after deep removal of impurities. The solution components are: 16 g / L vanadium, 0.5 g / L chromium, 0.5 g / L tungsten, 0.05 g / L silicon, 0.05 g / L Phosphorus, 0.5 g / L molybdenum, 0.1 g / L arsenic, tertiary amine Alamine336, dioctyl sulfoxide, 4-methyl-1-pentanol and o-xylene were used to make the organic phase, and the extraction and separation test was carried out to adjust the pH value of the feed solution 4.5, the volume percentage concentration of the extraction agent primary amine is 3.0%, the volume percentage concentration of LIX63 is 0.3%, the volume percentage concentration of n-octanol is 0.3%, the extraction temperature is room temperature 25 ° C, and the aqueous phase and the organic phase are mixed in a stirring tank Mix, stir and extract for 20 minutes, remove the oscillator and let it stand for 10 minutes to separate the layers, back-extract the loaded organic phas...

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Abstract

The invention relates to a method for preparing high-purity vanadium from heteropolyacid impurities in an amine extraction mode. Generally an ordinary vanadium solution is doped with impurities such as chromium, silicon, phosphorus, tungsten, molybdenum and arsenic, if acid is added into the solution, heteropolyacids such as phosphorus tungsten, phosphorus vanadium tungsten, silicon tungsten, phosphorus molybdenum tungsten, silicon molybdenum tungsten, molybdenum vanadium arsenic and tungsten arsenic can be formed, the impurities in the solution are removed by carrying out compounding synergic extraction on the heteropolyacids in the ordinary vanadium solution by using amines and a synergist so as to obtain a purified vanadium-containing raffinate, subsequently the vanadium-containing raffinate is evaporated and concentrated to be the concentration that each liter of the solution contains 40g vanadium, ammonium salt is further added into the concentrated liquid to obtain ammonium metavanadate solid, vanadium pentoxide with the purity greater than 99.9% is obtained through washing in pure water, drying and calcining in an oxygen atmosphere, the organic phase after the heteropolyacid is extracted is subjected to reverse extraction by using an alkali solution so as to form a heteropolyacid water phase, and the organic phase is recycled and circulated. The method has low requirement on equipment, and is simple to operate, key extraction agents are good in thermal stability and not sensitive in acid and alkali, and a recycling and circulating method is simple and easy to be industrialized.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy and metallurgical material preparation, and specifically relates to a method for preparing high-purity vanadium by extracting heteropolyacid impurities with amines. Background technique [0002] Vanadium, rare earths, titanium, etc. are listed as the national first-level strategic reserve resources, which are widely used and are called "industrial monosodium glutamate". In recent years, the price of vanadium resources has fluctuated and declined due to the impact of the steel market, and related enterprises and manufacturers are suffering. In order to get out of the economic crisis, many manufacturers have turned their attention to the high-end product market, and intend to win market competitiveness by increasing the added value of products. At present, the market price of ordinary 98.5% vanadium pentoxide is 70,000-80,000 / ton, the price of 99.5% high-purity vanadium pentoxide is more than 160,000 / ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/28C22B34/22
CPCY02P10/20
Inventor 宁朋歌曹宏斌张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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