Preparation method for high-purity vanadyl sulfate solution

The technology of vanadyl sulfate solution and vanadyl sulfate, which is applied in the field of hydrometallurgy, can solve the problems of expensive reagents, long process flow and high cost, and achieve the effects of improving safety and reliability, simplifying process flow and good economic benefits.

Active Publication Date: 2016-02-24
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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Problems solved by technology

The main reason restricting the development of vanadium battery at present is that its cost remains high, and the root cause is that the preparation cost of electrolyte is too high. The method of high-purity vanadium oxide and high-concentration electrolyte for vanadium battery), prepare battery-grade vanadyl sulfate based on high-purity vanadium pentoxide, and the process of preparing high-purity vanadium pentoxide often involves remelting, separation and purification , precipitation, calcination and other steps, the process is complicated, the process is long and the effect of impurity removal is not ideal. The main impurities such as chromium and iron are high in content. The existence of iron and chromium will seriously reduce the energy efficiency of vanadium batteries and corrode electrode materials. , which seriously affects the operation of the vanadium battery system
[0003] At present, the impurity removal of vanadyl sulfate is mainly divided into two types, one is to remove impurities in raw materials (including qualified liquid of vanadium pentoxide and vanadium), and the main step is to return vanadium pentoxide to the qualified liquid or directly to the qualified liquid Add precipitant, such as magnesium salt, aluminum salt and calcium salt, etc. to remove anionic impurities such as silicate, chromate, phosphate in the solution, and then remove most of cationic impurities, such as

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preparation example Construction

[0027] Since the preparation of vanadyl sulfate needs to go through a reduction process, the impurity elements iron and chromium exist in the form of low price in the solution. In the acidic solution system, iron ions and chromium ions will enter the solution together with vanadium ions, so that the removal of Complexity becomes difficult. The invention mainly further removes impurity iron and chromium in the crude vanadyl sulfate solution, so that the vanadyl sulfate can reach the purity of vanadium battery level, and can be well applicable to vanadium battery systems. The present invention adopts the pentavalent vanadium solution to first oxidize the low-priced iron ions in the vanadyl sulfate solution into high-valent iron ions, and then adjust the pH of the solution with ammonia water, so that the iron and ammonia react to form jarosite precipitation, and the iron ion impurities can be removed by filtration. Since it is difficult for pentavalent vanadium ions to oxidize lo...

Embodiment 1

[0041]Measure 200ml of crude vanadyl sulfate solution (the iron content and chromium content in the solution are 550.3mg / L and 269.6mg / L respectively), add 20ml of pentavalent vanadium solution with a concentration of 1.5M, under the condition that the water bath temperature is 60°C After reacting for 3.5 hours, the temperature was raised to 80°C, the pH was adjusted to 1.2 with ammonia water, and the reaction was stabilized for 3 hours. After filtering, the iron content in the vanadyl sulfate solution was measured to be 0.0027g / L. Continue to use ammonia water to adjust the pH of the solution to 7, fully stir for 1.5 hours, filter and dry, the measured chromium content in the vanadyl hydroxide solid is 98.7%. The obtained vanadyl hydroxide precipitate is dissolved in dilute sulfuric acid according to the metering ratio, the pH is controlled to be 1-2, and a high-purity vanadyl sulfate solution is finally obtained.

Embodiment 2

[0043] Measure 200ml of crude vanadyl sulfate solution (the iron content and chromium content in the solution are 550.3mg / L and 269.6mg / L respectively), add 20ml of pentavalent vanadium solution with a concentration of 1.7M, under the condition that the water bath temperature is 40°C After reacting for 4.0 hours, raise the temperature to 80° C., adjust the pH to 1.0 with ammonia water, react for 4 hours in a stable state, filter, and measure the iron content in the vanadyl sulfate solution to be 0.0019 g / L. Continue to use ammonia water to adjust the pH of the solution to 8, fully stir for 1.0 h, filter and dry, the measured chromium content in the vanadyl hydroxide solid is 99.1%. The obtained vanadyl hydroxide precipitate is dissolved in dilute sulfuric acid according to the metering ratio, the pH is controlled to be 1-2, and a high-purity vanadyl sulfate solution is finally obtained.

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Abstract

The invention belongs to the field of wet-process metallurgy, and mainly relates to a preparation method for a high-purity vanadyl sulfate solution. The preparation method for the high-purity vanadyl sulfate solution provided by the invention comprises the following steps: a), oxidation of Fe2+; b), removal of Fe3+; c), removal of chromium ions and preparation of oxovanadium hydroxide; and d), preparation of the high-purity vanadyl sulfate solution, wherein the rough vanadyl sulfate solution is the vanadyl sulfate solution with the chromium content of greater than or equal to 550.3 mg/L and the iron content of greater than or equal to 269.6 mg/L. The chromium content is less than or equal to 0.002% and the iron content is less than or equal to 0.0027 g/L in the vanadyl sulfate solution prepared by the method.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy, and mainly relates to the preparation of a high-purity vanadyl sulfate solution, its electrolyte solution and a vanadium battery. Background technique [0002] As an emerging energy storage system, vanadium battery has many advantages such as long service life, large capacity, high power, and high safety. It can be widely used in power grid peak regulation, public transportation airborne power supply, wind energy and solar energy storage system . The main reason restricting the development of vanadium battery at present is that its cost remains high, and the root cause is that the preparation cost of electrolyte is too high. The method of high-purity vanadium oxide and high-concentration electrolyte for vanadium battery), prepare battery-grade vanadyl sulfate based on high-purity vanadium pentoxide, and the process of preparing high-purity vanadium pentoxide often involves remelting, separation an...

Claims

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Application Information

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IPC IPC(8): H01M8/18
CPCH01M8/188H01M2300/002Y02E60/50
Inventor 刘波彭穗汪南方李道玉陈文龙曹敏龙秀丽陈勇韩慧果
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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