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Preparation method of solid vanadyl sulfate

A technology of solid sulfuric acid and vanadyl, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of polluting the environment, excessive ammonia nitrogen in extraction wastewater, etc., achieving low cost, preventing overflow, and realizing large-scale industrial production Effect

Active Publication Date: 2019-11-01
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the first stage of the method, the alkaline extraction, impurity removal and purification process needs to introduce ammonium chloride as a stripping agent, which will cause the environmental problem of excessive ammonia nitrogen pollution in the extraction wastewater.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method of solid vanadyl sulfate, said method comprising the steps of:

[0035] (1) Take 1000ml vanadium concentration as 30g / L, pH value is 3.1 converter steelmaking vanadium slag calcification roasting, the obtained vanadium leaching solution after leaching carries out extraction and clarification treatment, wherein oil-water ratio O / A=1:2, extraction time 10min, clarification 10min extracts and removes iron, obtains the raffinate containing vanadium, and the extraction system used for extraction is N235 (trioctylamino ammonium), TBP (tributyl phosphate) and sulfonated kerosene, and the volume ratio of the three is 30: 10:60; after the separation of the two phases, use 2M sulfuric acid solution to back-extract the organic phase for regeneration, wherein the oil-water ratio O / A=3:1, the back-extraction time is 10min, and the clarification treatment after back-extraction is 3min;

[0036] (2) Add sulfuric acid to the vanadium-containing raffinate after iron...

Embodiment 2

[0042] A preparation method of solid vanadyl sulfate, said method comprising the steps of:

[0043] (1) Take 1000ml of converter steelmaking vanadium slag with a vanadium concentration of 25g / L and a pH value of 9.1 for sodium roasting and leaching to extract and clarify the vanadium leaching solution, wherein the oil-water ratio O / A=1:5, extract Time 10min, clarification 10min extraction and iron removal, obtain raffinate containing vanadium, the extraction system used for extraction is N235 (trioctylamino ammonium), TBP (tributyl phosphate) and sulfonated kerosene, the volume ratio of the three is 30 :10:60; after the two phases are separated, use 2M sulfuric acid solution to back-extract the organic phase for regeneration, wherein the oil-water ratio O / A=4:1, the back-extraction time is 10min, and the clarification treatment after back-extraction is 3min;

[0044] (2) Add sulfuric acid to the vanadium-containing raffinate after iron removal to adjust the pH of the solution ...

Embodiment 3

[0050] A preparation method of solid vanadyl sulfate, said method comprising the steps of:

[0051] (1) Take 1000ml vanadium concentration as 20g / L, pH value is 2.5 converter steelmaking vanadium slag calcification roasting, the obtained vanadium leaching solution after leaching carries out extraction and clarification treatment, and wherein oil-water ratio O / A=1:3, extraction time 10min, clarification 10min extracts and removes iron, obtains the raffinate containing vanadium, and the extraction system used for extraction is N235 (trioctylamino ammonium), TBP (tributyl phosphate) and sulfonated kerosene, and the volume ratio of the three is 30: 10:60; after the separation of the two phases, use 2M sulfuric acid solution to back-extract the organic phase for regeneration, wherein the oil-water ratio O / A=3:1, the back-extraction time is 10min, and the clarification treatment after back-extraction is 3min;

[0052] (2) Add sulfuric acid to the vanadium-containing raffinate after ...

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PUM

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Abstract

The invention relates to a preparation method of solid vanadyl sulfate. The preparation method comprises the following steps: roasting and leaching steelmaking converter vanadium slag to obtain a vanadium-containing solution; carrying out targeted iron removal and vanadium valence conversion, carrying out impurity removal and purification by using a solvent extraction method, and carrying out mixed acid back extraction to obtain a high-purity vanadyl sulfate solution; and finally, carrying out direct negative pressure distillation crystallization to obtain the solid vanadyl sulfate. The methodis simple in technological process and low in cost, and large-scale industrial preparation can be achieved. A tetravalent vanadium solution is purified by adopting a solvent extraction method for impurity removal and purification, and impurity elements such as iron, manganese, chromium, zinc, calcium and magnesium can be effectively removed by controlling proper technical parameter conditions.

Description

technical field [0001] The invention belongs to the technical field of impurity removal and purification of inorganic compound materials, and in particular relates to a preparation method of solid vanadyl sulfate. Background technique [0002] Vanadium is a rare metal that can store sunlight. All-vanadium redox flow battery is recognized as the preferred technology for large-scale grid energy storage and a reliable solution for efficient solar energy storage. Solar energy has the characteristics of volatility and dispersion, and it is necessary to develop an efficient energy storage system to deal with the unbalanced grid connection of solar power generation and the time difference between supply and demand. [0003] All-vanadium redox flow battery (VRB) is an excellent energy storage device, and the battery capacity depends on the amount of electrolyte. VRB batteries have no solid-state reaction, no change in the structure and form of electrode materials, and the electroly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/00C01P2006/80
Inventor 郭秋松杨莉花曹洪杨戴子林饶帅刘志强李伟高远陶进长张魁芳
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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