A kind of preparation method and application of vanadyl sulfate crystal

A technology of vanadyl sulfate crystals and vanadyl sulfate, which is applied in the field of vanadium batteries, can solve the problems of high reaction impurities, cumbersome reaction process, increase the number of contact reagents and containers of vanadyl sulfate, etc., and achieve low impurity ion content, process and The effect of simple equipment and easy large-scale preparation

Active Publication Date: 2018-04-06
HEBEI IRON AND STEEL
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0008] (1) Reaction process is loaded down with trivial details: in above-mentioned reaction process, need be prepared into vanadyl sulfate solution at first, then obtain vanadyl sulfate crystal or powder through evaporation crystallization, improved preparation cost
[0009] (2) High reaction impurities: In the above reaction process, the raw materials vanadium pentoxide and sulfuric acid are not purified from impurities, and the steps are numerous, which increases the number of contact reagents and containers of vanadyl sulfate, and easily introduces impurities

Method used

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preparation example Construction

[0044] The specific embodiment part of the present invention provides the preparation method of vanadyl sulfate crystal, and described method comprises the following steps:

[0045] (1) adding vanadium pentoxide with a purity of ≥99.5wt% and sulfuric acid with a concentration of ≥98wt% in a molar ratio of 1:(1.0~3.5) into the reactor and mixing uniformly;

[0046] (2) Place the reaction kettle filled with vanadium pentoxide and sulfuric acid with a concentration ≥ 98wt% in a closed reactor, and feed reducing gas into the closed reactor, and the reducing gas enters the reaction kettle from the bottom of the reactor to participate in the reaction. Reaction, wherein, the molar ratio of reducing gas to vanadium pentoxide is (1~10):1, is heated up to 250~360 ℃ and carries out reduction reaction;

[0047] (3) After the reduction reaction is finished, the reaction kettle is taken out at a temperature of 250-300° C. to obtain vanadyl sulfate crystals.

Embodiment 1

[0049] (1) get the vanadium pentoxide of 100g purity ≥ 99.5wt% to be placed in reactor, be that the mol ratio of the sulfuric acid of 18mol / L is 1:1.2 to add the sulfuric acid of concentration ≥ 98wt% by vanadium pentoxide and concentration, stir well mixed;

[0050] (2) The reaction kettle is placed in a closed high-temperature atmosphere furnace, and sulfur dioxide gas is introduced into the furnace. The molar ratio of sulfur dioxide and vanadium pentoxide is 2:1, and the sulfur dioxide gas enters the reaction kettle from the bottom of the reaction kettle, and the temperature is raised to 360 ℃ for reduction reaction 1h;

[0051] (3) After the reduction reaction is complete, the reactor is taken out at 250° C., and then cooled in a desiccator to obtain vanadyl sulfate crystals with a purity of 99.5 wt%.

[0052] The obtained vanadyl sulfate crystals were weighed to make vanadyl sulfate electrolyte. After chemical analysis, the contents of the main impurity elements were as ...

Embodiment 2

[0054] (1) get the vanadium pentoxide of 100g purity ≥ 99.5wt% to be placed in reactor, be that the mol ratio of the sulfuric acid of 18mol / L is 1:1.5 to add the sulfuric acid of concentration ≥ 98wt% by vanadium pentoxide and concentration, stir well mixed;

[0055] (2) The reaction kettle is placed in a closed high-temperature atmosphere furnace, and sulfur dioxide gas is introduced into the furnace. The molar ratio of sulfur dioxide to vanadium pentoxide is 10:1, and the sulfur dioxide gas enters the reaction kettle from the bottom of the reaction kettle, and the temperature is raised to 300 ℃ for reduction reaction 0.5h;

[0056] (3) After the reduction reaction is complete, the reactor is taken out at 270° C., and then cooled in a desiccator to obtain vanadyl sulfate crystals with a purity of 99.3 wt%.

[0057] The obtained vanadyl sulfate crystals were weighed to make vanadyl sulfate electrolyte. After chemical analysis, the contents of the main impurity elements were a...

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Abstract

The invention provides a preparation method of a vanadyl sulfate crystal and application of the vanadyl sulfate crystal.The method comprises the following steps that vanadium pentoxide and sulfuric acid with the concentration of 15 mol / L-20 mol / L are added into a reaction kettle and mixed to be uniform; the reaction kettle containing vanadium pentoxide and sulfuric acid with the concentration of 15 mol / L-20 mol / L is put into a sealed reactor, reduction gas is introduced into the sealed reactor, the temperature is increased, and a reduction reaction is conducted; after the reduction reaction is completed, the reaction kettle is taken out, and the vanadyl sulfate crystal is obtained.The high-purity vanadyl sulfate crystal is prepared directly through a reduction method, evaporation crystallization treatment is not needed in the whole technology process, operation is easy, the reaction condition is mild, the cost is low, and the content of foreign ions in vanadyl sulfate electrolytes prepared from the high-purity vanadyl sulfate crystal is low and lower than 10 ppm.

Description

technical field [0001] The invention belongs to the technical field of vanadium batteries, and relates to a method for preparing vanadyl sulfate crystals and an application thereof, in particular to a method for preparing high-purity vanadyl sulfate crystals through direct reduction and an application thereof. Background technique [0002] Due to the advantages of non-pollution, long life, high energy efficiency and simple maintenance, the all-vanadium liquid flow energy storage system has great potential in the fields of solar energy, wind energy storage and grid connection, grid peak regulation, remote area power supply system, and uninterruptible power supply. Huge application prospects. Compared with other energy storage technologies, the all-vanadium redox flow energy storage system has unique advantages such as low cost, high efficiency, deep discharge capability, cleanliness and high efficiency. At present, it has become one of the most promising energy storage techn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00H01M8/18
CPCC01G31/00C01P2006/80H01M8/188Y02E60/50Y02P70/50
Inventor 徐从美陈东辉李兰杰闫浩祁健王海旭
Owner HEBEI IRON AND STEEL
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