CN1300002C - Process for preparing nano grade vanadium trioxide - Google Patents
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- CN1300002C CN1300002C CN 200510018838 CN200510018838A CN1300002C CN 1300002 C CN1300002 C CN 1300002C CN 200510018838 CN200510018838 CN 200510018838 CN 200510018838 A CN200510018838 A CN 200510018838A CN 1300002 C CN1300002 C CN 1300002C
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- vanadium trioxide
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Abstract
The present invention relates to a method for preparing nanometer-grade vanadium trioxide. The solution of vanadium oxalate is added into an autoclave, then temperature is raise to a certain degree and kept for certain time under certain pressure, and finally, the powder of the nanometer-grade vanadium trioxide with crystal form is obtained by unloading solvent. The method has the characteristics of simple implementation, low reaction temperature, low price, etc.; the obtained nanometer-grade vanadium trioxide after the reaction has good crystal phase structure before calcination, and thereby, the nanometer-grade vanadium trioxide has important application value.
Description
Technical field
The present invention relates to a kind of method for preparing nano grade vanadium trioxide, it belongs to technical field of inorganic, also belongs to technical field of function materials.
Background technology
Vanadous oxide (V
2O
3) normal temperature is down black powder.When temperature to 730 ℃, unformed vanadous oxide can change the crystal formation vanadous oxide into.Vanadous oxide has two phase transformations relevant with temperature.Near-113 ℃, the first-order phase transition of the antiferromagnetic insulation phase of low temperature (AFI) to high temperature paramagnetic metal phase (PM) takes place, change in resistance is the NTC characteristic, and the sudden change of monocrystalline resistivity reaches 7 orders of magnitude.At the second-order phase transition of about 277 ℃ generation low temperature paramagnetic metal phase (PM) to high temperature paramagnetic metal phase (PM '), resistivity is the positive temperature coefficient ptc characteristics during phase transformation.V
2O
3Being accompanied by the sudden change of electricity, light, magnetic property during material phase transformation, is the excellent thermo-sensitive material that a kind of potential has wide application prospect.But, V
2O
3Its unit cell volume has 1.5% variation approximately during phase transformation, and the huge stress of its generation makes material microfracture can occur in the thermal cycling process, causes material property to degenerate.This has also just limited V
2O
3Being extensive use of of material.Because the special and excellent properties of nano material is if obtain nanometer V
2O
3Powder body material makes it to sinter into the high density nano ceramic material, then can overcome above deficiency.
Nanometer V
2O
3The preparation method of powder body material mainly contains following several:
People such as O.Toshiyuki have disclosed a kind of preparation nanometer V
2O
3The method of powder (J Photopolym Sci.Technol., 1997,10 (2): 211-215).This method is to use induced with laser VOCl
3Gas phase H
2Reduction method obtains nanometer V
2O
3Powder.This method is very high to the requirement of equipment.
People such as Sullivan R.J. have disclosed a kind of preparation nanometer V
2O
3The method of powder (J.Am.Ceram.Soc., 1990,73:3715).This method is to use H
2The V that obtains of reason solution spray thermolysis also
2O
5Thereby the preparation particle diameter is less than the spherical V of 10 μ m
2O
3Micro mist.This method has the high shortcoming of temperature of reaction.
Chinese invention patent ZL01129948.7 has disclosed a kind of preparation nanometer V
2O
3The method of powder.This method is to utilize (NH
4)
5[(VO)
6(CO
3)
4(OH)
9] 10H
2O 650 ℃ of reduction pyrolysis in hydrogen can obtain the ball shaped nano level V of particle diameter less than 30nm in 1 hour
2O
3Powder.Long and the expensive deficiency of this method desired raw material synthetic route.
Above preparation method's not only cost is very high, and temperature of reaction is all higher, therefore, is badly in need of the low nanometer V of a kind of cost
2O
3The preparation method of powder.
Summary of the invention
In view of the deficiencies in the prior art, the present invention will provide a kind of cost low nano level V
2O
3The preparation method of powder.
Ultimate principle of the present invention is in overcritical or meto-super-critical fluid, utilizes the oxalic acid vanadyl to decompose and obtains crystallized nano level vanadous oxide.
Concrete technical scheme is as follows:
A kind of method for preparing nano grade vanadium trioxide: oxalic acid vanadyl organic solution is joined in the autoclave, be warmed up to certain temperature, under certain pressure, keep for some time, keep the temperature-resistant nano grade vanadium trioxide powder that solvent can obtain having crystal formation that draws off at last.Powder is of a size of 20～50nm, powder be shaped as sphere.
According to technical scheme of the present invention, oxalic acid vanadyl solution can prepare as follows: raw material vanadium pentoxide powder and oxalic acid are distributed to react in the appropriate organic solvent and make oxalic acid vanadyl solution.
According to technical scheme of the present invention, described organic solvent is the mixed solvent of a kind of or above-mentioned alcohols in methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, the isopropylcarbinol.
According to technical scheme of the present invention, reaction pressure of the present invention is 1～20MPa, serves as better with 3～15MPa wherein.Temperature of reaction is 160～400 ℃, serves as better with 220～300 ℃ wherein.Reaction times is 0.1～20h, serves as better with 0.5～5h wherein.Gained vanadous oxide powder has crystalline structure preferably after drawing off solvent.
Compared with the prior art, method disclosed by the invention has the following advantages:
1. temperature of reaction is low;
2. solvent for use is common organic solvent, and is cheap;
3. the nano grade vanadium trioxide that obtains after the reaction just has good crystal phase structure before the calcining;
Description of drawings
Fig. 1 is gained nanometer V of the present invention
2O
3Transmission electron microscope (TEM) photo;
Fig. 2 is gained nanometer V of the present invention
2O
3XRD spectra.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described:
Embodiment 1
With 9.00gV
2O
5With 20.2g H
2C
2O
42H
2O is added in the 100mL dehydrated alcohol, and back flow reaction 2h obtains VOC
2O
4Ethanolic soln.With dehydrated alcohol with this solution dilution to 250mL, transfer to then in the 0.5L autoclave, progressively be warmed up to 250 ℃ behind the good seal, system pressure also is raised to 9.1MPa.In this case, behind the insulation 3h, constant temperature is emitted ethanol in 1.7h.When solvent was about to put, the still temperature sharply raise, and reaches 300 ℃.Close heating, naturally cool to room temperature.Obtain the 6.60g black powder.
Embodiment 2
With 8.00g VOC
2O
4Be added in the 250mL methyl alcohol, transfer to then in the 0.5L autoclave, progressively be warmed up to 200 ℃ behind the good seal, system pressure also is raised to 7.0MPa.In this case, behind the insulation 2.4h, constant temperature is emitted methyl alcohol in 1.2h.When solvent was about to put, the still temperature sharply raise, and reaches 256 ℃.Close heating, naturally cool to room temperature.Obtain 3.34g black nano V
2O
3Powder.
Embodiment 3
With 8.00g VOC
2O
4Dissolve in 250mL ethanol and the isopropyl alcohol mixed solvent in (volume ratio is 2: 1), transfer to then in the 0.5L autoclave, progressively be warmed up to 245 ℃ behind the good seal, system pressure also is raised to 7.8MPa.In this case, behind the insulation 2.0h, constant temperature is emitted solvent in 1.0h.When solvent was about to put, the still temperature sharply raise, and reaches 270 ℃.Close heating, naturally cool to room temperature.Obtain 3.30g black nano V
2O
3Powder.
Claims (4)
1, a kind of method for preparing nano grade vanadium trioxide, it is characterized in that: oxalic acid vanadyl organic solution is joined in the autoclave, be warmed up to 160～400 ℃, under 1～20MPa pressure, kept 0.1～20 hour, and drew off solvent and can obtain nano level, as to have crystal phase structure vanadous oxide powder; Used organic solvent is the mixed solvent of a kind of or above-mentioned alcohols in methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, the isopropylcarbinol.
2, method according to claim 1, the pressure in it is characterized in that reacting is 3～15MPa.
3, method according to claim 1 is characterized in that temperature of reaction is 220～300 ℃.
4, method according to claim 1 is characterized in that the reaction times is 0.5～5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510018838 CN1300002C (en) | 2005-06-03 | 2005-06-03 | Process for preparing nano grade vanadium trioxide |
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|---|---|---|---|
| CN 200510018838 CN1300002C (en) | 2005-06-03 | 2005-06-03 | Process for preparing nano grade vanadium trioxide |
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| Publication Number | Publication Date |
|---|---|
| CN1724386A CN1724386A (en) | 2006-01-25 |
| CN1300002C true CN1300002C (en) | 2007-02-14 |
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ID=35924040
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|---|---|---|---|
| CN 200510018838 Expired - Fee Related CN1300002C (en) | 2005-06-03 | 2005-06-03 | Process for preparing nano grade vanadium trioxide |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993111B (en) * | 2010-10-21 | 2012-07-25 | 沈阳化工大学 | Method for preparing nanometer vanadous oxide |
| CN103011290B (en) * | 2012-11-23 | 2014-05-28 | 湖北大学 | Method for preparing vanadium trioxide microsphere powder under induction action of tartaric acid |
| CN106006736B (en) * | 2016-05-16 | 2017-06-13 | 武汉理工大学 | Using hydrogen from the method containing vanadium trioxide is prepared in vanadium solution |
| WO2017208892A1 (en) * | 2016-05-30 | 2017-12-07 | コニカミノルタ株式会社 | Process for producing vanadium-dioxide-containing particles |
| CN106044854B (en) * | 2016-08-05 | 2017-09-15 | 北京有色金属研究总院 | A kind of preparation method of submicron order vanadium trioxide powder |
| CN106540678B (en) * | 2016-11-01 | 2019-02-05 | 东北大学 | Vanadium trioxide nano particle and preparation method |
| CN107662946B (en) * | 2017-08-11 | 2020-01-14 | 攀枝花学院 | Preparation method of vanadium trioxide |
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2005
- 2005-06-03 CN CN 200510018838 patent/CN1300002C/en not_active Expired - Fee Related
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| CN1724386A (en) | 2006-01-25 |
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