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Method for preparing vanadium pentoxide through ammonium-free molybdenum precipitation

A technology of vanadium pentoxide and vanadium precipitation, which is applied in the field of ammonium-free vanadium precipitation to prepare vanadium pentoxide, can solve the problems of large consumption of sulfuric acid and ammonia water, etc., and achieve the effects of easy industrialization, simplified process and short process

Active Publication Date: 2020-04-17
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing vanadium pentoxide by precipitating vanadium without ammonium, so as to solve the problem of large consumption of sulfuric acid and ammonia water in the existing vanadium metallurgical process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Using the prepared loaded organic phase as raw material, carry out stripping with mass concentration of 3% hydrogen peroxide and 1.5mol / L sulfuric acid as stripping agent.

[0031] (2) Under the condition of O / A=5:1, carry out stripping of the obtained loaded organic phase: after two-stage cross-flow stripping with hydrogen peroxide, then single-stage stripping with sulfuric acid; the stripping time is 3min, 30s Internal phase separation; after 3 times of cross-flow stripping, the total stripping rate is above 97.77%.

[0032] (3) Mix the back-extraction solutions three times together, and after standing for 24 hours, the polyvanadic acid is precipitated from the solution with the decomposition of the peroxovanadium complex, and the crystallization rate is above 85%. The red-black solid was calcined in a muffle furnace for 4 hours at a temperature of 555°C to obtain red V 2 o 5 product.

Embodiment 2

[0034] (1) Using the prepared loaded organic phase as raw material, carry out stripping with mass concentration of 4% hydrogen peroxide and 1.3mol / L sulfuric acid as stripping agent.

[0035] (2) Back-extract the obtained loaded organic phase under the condition of O / A=8:1: three-stage cross-flow back-extraction with hydrogen peroxide, and then single-stage back-extraction with sulfuric acid; the back-extraction time is 3min, 30s Internal phase separation; after 4 times of cross-flow stripping, the total stripping rate is above 85.43%.

[0036] (3) Mix the back-extraction solutions three times together, and after standing for 30 hours, the polyvanadic acid is precipitated from the solution with the decomposition of the peroxovanadium complex, and the crystallization rate is above 92%. The red-black solid was calcined in a muffle furnace for 5 hours at a temperature of 550°C to obtain red V 2 o 5 product.

Embodiment 3

[0038] (1) Using the prepared loaded organic phase as a raw material, carry out stripping with a mass concentration of 6% hydrogen peroxide and 1mol / L sulfuric acid as a stripping agent.

[0039] (2) Under the condition of O / A=10:1, back-extract the obtained loaded organic phase: go through three-stage cross-flow back-extraction with hydrogen peroxide, and then perform single-stage back-extraction with sulfuric acid; the back-extraction time is 2.5min, Phase separation within 30s; after 4 times of cross-flow stripping, the total stripping rate is above 92.25%.

[0040] (3) Mix the back-extraction solutions three times together, and after standing for 28 hours, the polyvanadic acid is precipitated from the solution with the decomposition of the peroxovanadium complex, and the crystallization rate is above 94.3%. The red-black solid was calcined in a muffle furnace for 6 hours at a temperature of 545°C to obtain red V 2 o 5 product.

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Abstract

The invention discloses a method for preparing vanadium pentoxide through ammonium-free molybdenum precipitation. The method comprises the steps that a vanadium-containing acid leaching solution is reduced by a reduction agent, and then the pH of the solution is adjusted with ammonia liquor; cationic extraction agent is adopted for extraction, and a vanadium oxygen cation-supported organic phase and a raffinate are obtained; hydrogen peroxide and sulfuric acid are used as a stripping agent for stripping, and vanadium stripping liquor is obtained; after the stripping liquor is placed for a period of time, peroxy polyvanadate is unstable and is decomposed to generate polyvanadic acid to be gradually separated out in a water phase, and after calcination, the vanadium pentoxide product is obtained. According to the method for preparing the vanadium pentoxide through ammonium-free molybdenum precipitation, the vanadium smelting process is greatly simplified, the problems are thoroughly solved that in the stripping process, a lot of sulfuric acid and ammonia liquor is consumed and a lot of ammonia-nitrogen wastewater is produced, the method has the advantages of being short in process, environmentally friendly and efficient, and the method is easy to industrially popularize.

Description

technical field [0001] The invention relates to the technical field of nonferrous metal metallurgy, in particular to a method for preparing vanadium pentoxide by precipitating vanadium without ammonium. Background technique [0002] Vanadium is an important strategic metal, because vanadium has the properties of grain refinement and oxygen affinity, it is often widely used as a grain refiner and deoxidizer in the field of production of high-quality alloys, such as various iron alloys, titanium alloys Production; and in recent years, vanadium oxide is added to new materials, its electromagnetic properties can be expected, so the production of vanadium compounds has attracted much attention. [0003] In China, stone coal is an important vanadium storage resource, accounting for 87% of the total vanadium reserves. In recent years, the direct acid leaching method has gradually become the dominant method for extracting vanadium from stone coal due to its advantages of high leach...

Claims

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Application Information

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IPC IPC(8): C22B34/22C22B3/44
CPCC22B3/44C22B34/22Y02P10/20
Inventor 李青刚刘源张贵清曹佐英曾理关文娟巫圣喜
Owner CENT SOUTH UNIV
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