WO2002004353A2 - Method for preparing vanadylsulfate - Google Patents
Method for preparing vanadylsulfate Download PDFInfo
- Publication number
- WO2002004353A2 WO2002004353A2 PCT/IB2001/001203 IB0101203W WO0204353A2 WO 2002004353 A2 WO2002004353 A2 WO 2002004353A2 IB 0101203 W IB0101203 W IB 0101203W WO 0204353 A2 WO0204353 A2 WO 0204353A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- molar concentration
- solution
- process according
- starting material
- vanadyl sulphate
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
Definitions
- THIS invention relates to a process for the preparation of a vanadyl sulphate solution with a specified molar concentration.
- vanadyl sulphate by dissolving vanadium pentoxide in hot dilute sulphuric acid under vigorous agitation and continued heating with the aid of sulphur dioxide as a reducing agent.
- VOS0 4 vanadyl sulphate
- the vanadyl sulphate solution produced may have any desired molar concentration, for example 2M, 4M or up to a maximum of 6M.
- the first starting material is preferably substantially pure bulk commercial grade vanadium pentoxide having about a 99,5% vanadium pentoxide content.
- the second starting material is generally a commercial grade V 2 0 3 powder having an equivalent V 2 0 5 content of 1 18 to 122%.
- the sulphuric acid solution preferably has a molarity of from 2,8 to 8,5 depending upon the specified molar concentration of the vanadyl sulphate solution.
- Step (4) of the process is exothermic.
- the heat may be supplied by adding heated, preferably boiling water to the reaction, or by warming the sulphuric acid solution, e.g to a temperature of about 50°C.
- Figure 1 is a graph indicating the optimum ratio of V 2 0 3 , to V 2 O s needed for a complete reaction, expressed in mVolt.
- the crux of the invention is a process for the preparation of a vanadyl sulphate solution with a specified molar concentration, from a first starting material containing V 2 0 5 and a second starting material containing V 2 0 3 , and a sulphuric acid solution.
- the reaction may be monitored by measuring the reduction potential, as is illustrated in Figure 1.
- the start of the production of vanadyl sulphate is illustrated at the point where the graph dips sharply.
- V 2 0 5 , V 2 0 3 and a sulphuric acid solution is exothermic, for low molar concentrations of, for example ⁇ 3M vanadyl sulphate, it is preferable to add heat at the beginning of the dissolution step to trigger the reaction.
- the heat may be added in the form of heated, preferably boiling water, or by heating the sulphuric acid solution to a temperature of approximate 50°C.
- the dissolution time was 15 minutes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
A process for the preparation of a vanadyl sulphate solution with a specified molar concentration from a first starting material containing vanadium pentoxide (V2O5) and a second starting material containing vanadium trioxide (V2O3). The first and second starting materials are mixed together in amounts such that there are substantially equal quantities of vanadium in the first and second starting materials. A predetermined volume of a sulphuric acid solution having a predetermined molar concentration is added to produce a vanadyl sulphate (VOSO4) solution having the specified molar concentration.
Description
PROCESS
BACKGROUND TO THE INVENTION
THIS invention relates to a process for the preparation of a vanadyl sulphate solution with a specified molar concentration.
It is known to produce vanadyl sulphate by dissolving vanadium pentoxide in hot dilute sulphuric acid under vigorous agitation and continued heating with the aid of sulphur dioxide as a reducing agent.
The limited solubility of sulphur dioxide in acidic and aqueous solutions results in the emission of sulphur dioxide from the solution and this presents an environmental hazard. Overdosing of the solution with S02 gas results in the unwanted formation of the lower valent vanadium sulphate, namely V2S0 and not vanadyl sulphate (VOS04).
Since the dissolution of vanadium pentoxide in sulphuric acid is endothermic heat has to be provided to drive the formation of vanadyl sulphate.
There is always a need for a new method for the production of vanadyl sulphate.
SUMMARY OF THE INVENTION
According to the invention there is provided a process for the preparation of a vanadyl sulphate solution with a specified molar concentration which includes the steps of:
(1) providing a first starting material containing vanadium pentoxide (V205);
(2) providing a second starting material containing vanadium trioxide (V203);
(3) mixing the first and second starting materials in amounts such that there are substantially equal quantities of vanadium in the first and second starting materials; and
(4) adding a predetermined volume of a sulphuric acid solution having a predetermined molar concentration to produce a vanadyl sulphate (VOS04) solution having the specified molar concentration.
The vanadyl sulphate solution produced may have any desired molar concentration, for example 2M, 4M or up to a maximum of 6M.
The first starting material is preferably substantially pure bulk commercial grade vanadium pentoxide having about a 99,5% vanadium pentoxide content.
The second starting material is generally a commercial grade V203 powder having an equivalent V205 content of 1 18 to 122%.
The sulphuric acid solution preferably has a molarity of from 2,8 to 8,5 depending upon the specified molar concentration of the vanadyl sulphate solution.
Step (4) of the process is exothermic. However for low molar concentrations of, for example <3M vanadyl sulphate, it is preferable to supply heat at the beginning of the "'dissolution step to trigger the reaction. The heat may be
supplied by adding heated, preferably boiling water to the reaction, or by warming the sulphuric acid solution, e.g to a temperature of about 50°C.
BRIEF DESCRIPTION OF THE DRAWING
Figure 1 is a graph indicating the optimum ratio of V203, to V2Os needed for a complete reaction, expressed in mVolt.
DESCRIPTION OF EMBODIMENTS
The crux of the invention is a process for the preparation of a vanadyl sulphate solution with a specified molar concentration, from a first starting material containing V205 and a second starting material containing V203, and a sulphuric acid solution.
The reaction proceeds according to the following formula: V203 + V205 + 4H2S04 → 4VOS04 + 4H20.
The reaction may be monitored by measuring the reduction potential, as is illustrated in Figure 1. The start of the production of vanadyl sulphate is illustrated at the point where the graph dips sharply.
Although the reaction between the V205, V203 and a sulphuric acid solution is exothermic, for low molar concentrations of, for example <3M vanadyl sulphate, it is preferable to add heat at the beginning of the dissolution step to trigger the reaction. The heat may be added in the form of heated, preferably boiling water, or by heating the sulphuric acid solution to a temperature of approximate 50°C.
The advantages of the process of the invention are firstly that vaπous specified molar concentrations of vanadyl sulphate can be produced, secondly that no additional chemicals are required for the reaction, and thirdly that the process is environmentally friendly
Examples
Vaπous examples of the invention will now be given
The following mixtures were used for the preparation of 2, 4 and 6 molar solutions of vanadyl sulphate
Hivox (V203 powder) quality - 119,6% expressed as percent V205
The dissolution time was 15 minutes
The 2 and 4 molar solutions were filtered whilst warm using a laboratory vacuum pump with a GF/C fiber filter It was not possible to filter the 6 molar solution because of its viscosity
Claims
1. A process for the preparation of a vanadyl sulphate solution with a specified molar concentration includes the steps of:
(1 ) providing a first starting material containing vanadium pentoxide (V205);
(2) providing a second starting material containing vanadium trioxide (V203);
(3) mixing the first and second starting materials in amounts such that there are substantially equal quantities of vanadium in the first and second starting materials; and
(4) adding a predetermined volume of a sulphuric acid solution having a predetermined molar concentration to produce a vanadyl sulphate (VOS04) solution having the specified molar concentration.
2. A process according to claim 1 , wherein the vanadyl sulphate solution produced has a molar concentration up to a maximum of 6M.
3. A process according to claim 1 or claim 2, wherein the first starting material is substantially pure bulk commercial grade vanadium
. pentoxide having about a 99,5% vanadium pentoxide content.
4. A process according to any one of the preceding claims wherein the second starting material is a commercial grade V203 powder having an equivalent V205 content of 118 to 122%.
5. A process according to any one of the preceding claims wherein the sulphuric acid solution has a molarity of from 2,8 to 8,5 depending upon the specified molar concentration of the vanadyl sulphate solution.
6. A process according to any one of the preceding claims, wherein at low molar concentrations of the vandyl sulphate produced in step 4) heat is supplied at the beginning of step 4) to trigger the reaction.
7. A process according to claim 6, wherein the heat is supplied by adding heated water of by warming the suphuric acid solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2001267769A AU2001267769A1 (en) | 2000-07-12 | 2001-07-06 | Process |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ZA200003491 | 2000-07-12 | ||
| ZA2000/3491 | 2000-07-12 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| WO2002004353A2 true WO2002004353A2 (en) | 2002-01-17 |
| WO2002004353A3 WO2002004353A3 (en) | 2002-05-30 |
Family
ID=25588821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IB2001/001203 WO2002004353A2 (en) | 2000-07-12 | 2001-07-06 | Method for preparing vanadylsulfate |
Country Status (2)
| Country | Link |
|---|---|
| AU (1) | AU2001267769A1 (en) |
| WO (1) | WO2002004353A2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003101893A1 (en) * | 2002-05-31 | 2003-12-11 | Highveld Steel And Vanadium Corporation Limited | Process for the preparation of vanadyl sulfate solution |
| WO2007049126A1 (en) * | 2005-10-24 | 2007-05-03 | Highveld Steel And Vanadium Corporation Limited | Process for the preparation of an electrolyte |
| CN103043721A (en) * | 2012-12-25 | 2013-04-17 | 攀钢集团攀枝花钢钒有限公司 | Method for preparing vanadyl sulfate |
| WO2016059102A1 (en) * | 2014-10-16 | 2016-04-21 | Schmid Energy Systems Gmbh | Production of vanadyl sulfate from vanadium pentoxide |
| CN106129441A (en) * | 2016-06-29 | 2016-11-16 | 河北钢铁股份有限公司承德分公司 | The cleaning fast preparation method of a kind of vanadium oxysulfate solution and purposes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD151923A1 (en) * | 1980-07-09 | 1981-11-11 | Gerhard Ladwig | METHOD OF PREPARING CRYSTALLINE OXOVANADIUM (IV) SULFATE TRIHYDRATE |
| JP2000072441A (en) * | 1998-08-25 | 2000-03-07 | Taiyo Koko Co Ltd | Method for producing vanadium sulfate solution |
-
2001
- 2001-07-06 AU AU2001267769A patent/AU2001267769A1/en not_active Abandoned
- 2001-07-06 WO PCT/IB2001/001203 patent/WO2002004353A2/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD151923A1 (en) * | 1980-07-09 | 1981-11-11 | Gerhard Ladwig | METHOD OF PREPARING CRYSTALLINE OXOVANADIUM (IV) SULFATE TRIHYDRATE |
| JP2000072441A (en) * | 1998-08-25 | 2000-03-07 | Taiyo Koko Co Ltd | Method for producing vanadium sulfate solution |
Non-Patent Citations (1)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN vol. 2000, no. 06, 22 September 2000 (2000-09-22) & JP 2000 072441 A (TAIYO KOKO CO LTD), 7 March 2000 (2000-03-07) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003101893A1 (en) * | 2002-05-31 | 2003-12-11 | Highveld Steel And Vanadium Corporation Limited | Process for the preparation of vanadyl sulfate solution |
| US7083774B2 (en) | 2002-05-31 | 2006-08-01 | Highveld Steel And Vanadium Corporation Limited | Process for the preparation of vanadyl sulfate solution |
| AU2003232377B2 (en) * | 2002-05-31 | 2007-05-17 | Vanchem Vanadium Products (Pty) Limited | Process for the preparation of vanadyl sulfate solution |
| WO2007049126A1 (en) * | 2005-10-24 | 2007-05-03 | Highveld Steel And Vanadium Corporation Limited | Process for the preparation of an electrolyte |
| JP2009512622A (en) * | 2005-10-24 | 2009-03-26 | ハイベルド スティール アンド バナディウム コーポレーション リミテッド | Preparation method of electrolyte |
| CN103043721A (en) * | 2012-12-25 | 2013-04-17 | 攀钢集团攀枝花钢钒有限公司 | Method for preparing vanadyl sulfate |
| WO2016059102A1 (en) * | 2014-10-16 | 2016-04-21 | Schmid Energy Systems Gmbh | Production of vanadyl sulfate from vanadium pentoxide |
| DE102014115081A1 (en) | 2014-10-16 | 2016-04-21 | Schmid Energy Systems Gmbh | Preparation of vanadyl sulfate from vanadium pentoxide |
| CN106129441A (en) * | 2016-06-29 | 2016-11-16 | 河北钢铁股份有限公司承德分公司 | The cleaning fast preparation method of a kind of vanadium oxysulfate solution and purposes |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2001267769A1 (en) | 2002-01-21 |
| WO2002004353A3 (en) | 2002-05-30 |
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