Preparation method of vanadyl sulfate
A technology of vanadyl sulfate and sulfuric acid, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of insufficient purity of vanadyl sulfate products and low dry basis content.
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preparation example Construction
[0012] The invention provides a preparation method of vanadyl sulfate, which comprises the following steps: (1) dissolving vanadium pentoxide with sulfuric acid to obtain an activation solution; (2) contacting the activation solution with a reducing agent so that the The pentavalent vanadium in the activation solution is reduced to tetravalent vanadium to obtain a reduction product; (3) adjusting the pH value of the reduction product with an alkali, so that the tetravalent vanadium in the reduction product is separated out as a precipitate; (4) Dissolving the precipitate with sulfuric acid is used for crystallization to obtain vanadyl sulfate solid, and relative to 1 mole of tetravalent vanadium in the precipitate, the sulfuric acid is used in an amount of 0.9-1.1 moles.
[0013] Wherein, vanadium pentoxide can be obtained by methods known in the art, for example, by heating and decomposing ammonium vanadate, or can be obtained commercially. After vanadium pentoxide is dissolv...
Embodiment approach
[0031] According to a particularly preferred embodiment of the present invention, the method of the present invention comprises the following steps:
[0032] (1) dissolving vanadium pentoxide with 40-60% by weight of sulfuric acid aqueous solution under boiling conditions for 30-100 minutes to obtain an activated solution; the molar ratio of the sulfuric acid to vanadium pentoxide is 1: 0.15-0.2;
[0033] Diluting the activation solution with water, relative to each gram of vanadium pentoxide used to form the activation solution, the amount of water used for dilution is 5-15ml;
[0034] (2) at 50-70°C, contacting the diluted activation solution with excess sulfur dioxide for 30-80 minutes, so that the pentavalent vanadium in the activation solution is reduced to tetravalent vanadium to obtain a reduced product;
[0035] (3) adjust the pH value of the reduction product with sodium hydroxide to 4-6, preferably 4.5-5.5, more preferably 5-5.5, so that the tetravalent vanadium in t...
Embodiment 1
[0043] This example is used to illustrate the method provided by the present invention.
[0044] In the vanadium pentoxide of 100g (purchased from the Vanadium Products Factory of Pangang Iron and Steel Vanadium Titanium Co., Ltd., the purity is greater than 99.5% by weight), adding 634g concentration is the sulfuric acid aqueous solution of 50% by weight (the mol ratio of sulfuric acid and vanadium pentoxide About 1:0.17), then heated to boiling, and maintained under boiling conditions for 60 minutes to obtain an activated solution.
[0045] The above activated solution was cooled to room temperature, and then 1000 ml of water was added thereto for dilution.
[0046] At 60° C., in the diluted activation solution, an excessive amount of sulfur dioxide gas (purity greater than 99% by volume, and an amount of introduction greater than 0.6 mole) is passed into the diluted activation solution for 60 minutes, so that the pentavalent vanadium in the activation solution is reduced to...
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