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Preparation method of high-purity vanadyl sulfate solution

A vanadyl sulfate solution and solution technology, applied in the preparation of vanadium compounds, chemical instruments and methods, vanadium compounds, etc., can solve the problems of many by-products, long process flow, complicated preparation process, etc., and achieve low cost and energy consumption , The process is simple and the process time is short

Active Publication Date: 2017-05-31
深圳力合通科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of the above method is: vanadyl sulfate is dissolved in concentrated sulfuric acid or is difficult to be reduced to tetravalent vanadium by oxalic acid. Although the color of the solution changes from red to blue, in fact the valence state of vanadium in the solution still has a part of pentavalent Incomplete conversion of vanadium, pentavalent vanadium
Due to the use of strong acidic solution in this method, SO 2 The gas is difficult to dissolve in the solution, and the conversion rate is also extremely low
There are also some literatures that describe the method of preparing high-purity vanadyl sulfate by reacting vanadium pentoxide with alkaline solution, but the preparation process is complicated, requiring multi-stage countercurrent extraction and repeated reduction methods, which has a long process flow and high energy consumption. , many by-products and low production efficiency

Method used

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preparation example Construction

[0021] The preparation method of the high-purity vanadyl sulfate solution provided by the present invention includes the following steps:

[0022] S1 uses a strong alkaline solution to dissolve vanadium salt or vanadium compound, and performs filtration and impurity removal treatment.

[0023] In this step, the vanadium salt or vanadium compound can be vanadium pentoxide, sodium aluminate, sodium metavanadate, vanadium slag, sodium orthovanadate, potassium orthovanadate, potassium metavanadate or ammonium metavanadate Wait at least one. The strong alkaline solution can be 5-30% sodium hydroxide, 10-28% ammonia solution, etc.

[0024] This step is alkaline impurity removal, which can remove most of the impurities in vanadium salt or vanadium compounds and Fe that is insoluble or less soluble in alkali 3+ , Mn 2+ , Cr 3+ , Ni 2+ , Cu 2+ , SiO 2 Plasma or matter.

[0025] After S2 filtration and impurity removal, adjust the pH of the solution to a pH value of 1.0-5.0, make the solution ...

Embodiment 1

[0037] S1 chooses 1000g vanadium pentoxide and adds it to a strong alkali solution (10%) containing 600g sodium hydroxide to dissolve it, and then filter it to remove a small amount of Fe 3+ , Mn 2+ , Cr 3+ , Ni 2+ , Cu 2+ , SiO 2 And other impurities.

[0038] S2 After filtering the filtrate in the above steps, adjust the pH of the solution with sulfuric acid to make the pH of the solution 2.5, then add 200g of ferrous ammonium sulfate, and add 300g of phosphate diester precipitation inhibitor for combined reduction, so that the pentavalent vanadium in the solution is reduced to Tetravalent vanadium, to obtain a tetravalent vanadium salt solution. At the same time, fully stir the solution to make the remaining Fe in the solution 2+ , SiO 2 Iso impurity ions are adsorbed by the phosphate diester precipitation inhibitor floating on the upper layer of the solution, and a small amount of oxidized Fe 3+ Remains in solution;

[0039] S3 mixes 150g of vanadium into a solution, adds it to...

Embodiment 2

[0045] S1 uses 500g ammonium metavanadate, adds 5000g of 10% ammonia solution to dissolve, and then filters it to remove Fe 3 + , Mn 2+ , Cr 3+ , SiO 2 And other impurities.

[0046] S2 After filtering the filtrate in the above steps, add sulfuric acid to adjust the pH of the solution to make the solution pH=3.0, then add 120g of ferrous sulfate, and add 150g of phosphate diester precipitation inhibitor, combined reduction, so that the pentavalent vanadium in the solution is reduced to tetravalent Vanadium to obtain a tetravalent vanadium salt solution. At the same time, fully stir the solution to make the remaining Fe in the solution 2+ , SiO 2 Iso impurity ions are adsorbed by the phosphate diester precipitation inhibitor floating on the upper layer of the solution, and a small amount of oxidized Fe 3+ Still remain in solution.

[0047] S3 mixes 50g of vanadium into a solution, and adds it to the tetravalent vanadium salt solution in step S2, and fully reacts to remove Fe in the ...

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Abstract

The invention provides a preparation method of high-purity vanadyl sulfate. The method comprises the following steps: selecting a strong alkali solution for dissolving vanadium salts or vanadium compounds, removing impurities, filtering and adjusting a pH value of the solution to 1.5-5.0, then adding high-reducibility sulfuric acid compounds and phosphate diester precipitation preventing agents to obtain a tetravalent vanadium compound solution; enabling an alum solution and the tetravalent vanadium compound solution to fully react and generate water-insoluble tetravalent vanadium compound solid powder; washing the tetravalent vanadium compound solid powder with deionized water or distilled water, then carrying out solid-liquid separation; drying and firing the washed tetravalent vanadium compound solid powder, and then dissolving the tetravalent vanadium compound solid powder in a dilute sulfuric acid solution to obtain a water-soluble high-purity vanadyl sulfate solution. The method is capable of effectively removing various impurities in the vanadium salts or the vanadium compounds, fully reducing pentavalent vanadium compounds to tetravalent vanadium compounds and obtaining the high-purity vanadyl sulfate solution; the method is high in utilization rate of vanadium, short in technological process, low in cost and free of by-products; the large-scale production is easy to implement.

Description

Technical field [0001] The invention belongs to the technical field of preparation of vanadyl sulfate, and particularly relates to a method for preparing a high-purity vanadyl sulfate solution. Background technique [0002] Vanadium sulfate is a chemical raw material with a wide range of uses. At present, the preparation of vanadium oxysulfate with vanadium pentoxide as a raw material generally involves dissolving the raw materials in concentrated sulfuric acid, and then introducing liquid ammonia (1 ton of raw material vanadium pentoxide, using 1.8 tons of liquid ammonia) to reduce the pentavalent vanadium solution. It is obtained after obtaining tetravalent vanadium; some others are obtained by dissolving vanadium pentoxide in concentrated sulfuric acid and then reducing the pentavalent vanadium solution with oxalic acid to obtain vanadyl sulfate solution. The disadvantage of the above method is that it is difficult to reduce vanadyl sulfate to tetravalent vanadium by dissolvi...

Claims

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Application Information

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IPC IPC(8): C01G31/00
CPCC01G31/003
Inventor 陈建军许小弟陈鑫鲁海霞
Owner 深圳力合通科技有限公司
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