CN1872698A - Precursor body of Nano tube of composite oxides of multielement vanadium, and preparation method - Google Patents
Precursor body of Nano tube of composite oxides of multielement vanadium, and preparation method Download PDFInfo
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- CN1872698A CN1872698A CN 200610019350 CN200610019350A CN1872698A CN 1872698 A CN1872698 A CN 1872698A CN 200610019350 CN200610019350 CN 200610019350 CN 200610019350 A CN200610019350 A CN 200610019350A CN 1872698 A CN1872698 A CN 1872698A
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Abstract
This invention provides a method for preparing the precursor of V/Cr or V/Ti composite oxide nanotubes, whose structural formula is expressed as V12-yMyO30-0.5y .H2O, wherein M is Cr or Ti, and y is in the range of 0.0-4.0. The method comprises: (1) mixing analytically pure V2O5 with Cr2O3 or TiH at a molar ratio greater than or equal to 1.0; (2) dissolving the mixture into H2O2, and stirring vigorously to obtain a solution of V/Cr or V/Ti composite oxide; (3) heating to decompose the peroxide and form a sol and then a gel; (4) drying the gel at 50-60 deg.C to form the dried gel of V/Cr or V/Ti composite oxide; (5) carrying out hydrothermal reaction of the dried gel at 160-200 deg.C for 6-8 days in the presence of C4-22 primary amine neutral surfactant, filtering, and drying at 70-100 deg.C for 10-12 h to obtain V/Cr or V/Ti composite oxide nanotubes. The method has such advantages of simple process, few requirements for the equipment, good reproducibility and easy control of V to Cr to Ti ratio, and is environmentally friendly.
Description
Technical field
The present invention relates to a kind of precursor body of Nano tube of composite oxides of multielement vanadium and preparation method, metal nanometer material and field of nanometer technology.
Background technology
Along with rapid development of science and technology, people need carry out deep research as the quantum scale effect that structure, the physics of nanoscale are relevant with chemical property and low-dimensional to the phenomenon of some microscopic dimensions.In addition, the device microminiaturization proposes higher requirement to new function material.Since carbon nanotube is found, started the upsurge of research low-dimensional nano structure material in the world wide, make investigation of materials enter a brand-new field.In various nano materials, nanotube produces the physical and chemical performance of many excellences because having significant anisotropism structure and inherent quantum confinement, simultaneously peculiar 4 the different contact areas of nanotube (between inwall, outer wall, nanometer pipe end and wall layers) for its structural modification and performance optimization provide may, thereby attracted numerous scholars' research interest, become worldwide research focus.In recent years, the multicomponent composite oxide nanotube receives much concern because of its wide application prospect.Utilize the research of the polynary barium oxide nanotube of Prepared by Sol Gel Method to rarely have report at present, the present invention has synthesized the presoma-polynary vanadium combined oxidation xerogel for preparing polynary vanadium combined oxidation nanotube by sol-gel method, can successfully obtain Nano tube of composite oxides of multielement vanadium in hydro-thermal reaction subsequently.This method technology is simple, low for equipment requirements, favorable reproducibility, and the controllable degree height meets environmental requirement, and greatly reduces synthetic cost.
Summary of the invention
Problem to be solved by this invention provides a kind of precursor body of Nano tube of composite oxides of multielement vanadium and preparation method
Technical scheme provided by the invention is:
A kind of precursor body of Nano tube of composite oxides of multielement vanadium material is characterized in that its phraseology is: V
12-yM
yO
30-0.5yH
2O, wherein M is Cr or Ti; 0.0＜y≤4.0.
Precursor body of Nano tube of composite oxides of multielement vanadium preparation methods of the present invention, its preparation process is:
Step 1, be 〉=1.0 with mol ratio, dissolved in mass concentration and be in 10%～40% the hydrogen peroxide vigorous stirring 30～50 hours, obtain vanadium and chromium or titanium composite oxide solution Vanadium Pentoxide in FLAKES and chromium trioxide or titanium hydride powders;
Step 2, the composite oxides solution that step 1 is obtained heated 〉=1 hour at 50～70 ℃, made peroxide breakdown formation colloidal sol wherein become gel then;
Step 3, the gel that step 2 is obtained form the composite oxides of multielement vanadium xerogel 50～60 ℃ of dryings, promptly obtain precursor body of Nano tube of composite oxides of multielement vanadium V
12-yM
yO
30-0.5yH
2O, wherein M is Cr or Ti; 0.0＜y≤4.0.
With the presoma of this xerogel as hydro-thermal reaction, be on 4～22 the basis of primary amine class neutral surface active agent at carbonatoms as structure directing agent, 160～200 ℃ of hydro-thermal reactions 6～8 days, reaction product is used dehydrated alcohol and deionized water wash for several times, dried 10～12 hours, and promptly obtained vanadium chromium or composite vanadium-titanium oxides nanotube for 70～100 ℃.
Above-mentioned preparation technology's feature is: titanium and vanadium, or the mol ratio of chromium and vanadium is 0＜～0.5; The collosol and gel formation condition is 50～70 ℃ of heating 1 hour; 50～60 ℃ of dryings 1 day; 180 ℃ of hydro-thermal reactions 6～8 days.
The present invention directly uses the presoma of composite oxides of multielement vanadium xerogel as hydro-thermal reaction, and technology is simple, and the controllable degree height meets environmental requirement.
Description of drawings
The XRD figure spectrum of Fig. 1 embodiment 1 product
The TEM image of Fig. 2 embodiment 1 product
The XRD figure spectrum of Fig. 3 embodiment 2 products
The TEM image of Fig. 4 example example 2 products
Embodiment
Embodiment 1:
(1) vanadium pentoxide powder and chromium trioxide powder being dissolved in mass concentration by 1: 1 mol ratio is vigorous stirring 50 hours in 10% the hydrogen peroxide, vanadium chromium composite oxides solution; (2) solution with gained becomes gel then at 50 ℃ of heating formation in 1 hour colloidal sol; (3) gel with gained forms vanadium chromium composite oxides xerogel V 55 ± 5 ℃ of dryings
8Cr
4O
28NH
2O, i.e. V
4/3Cr
2/3O
14/3MH
2O; (4) with V
4/3Cr
2/3O
14/3MH
2O and cetylamine move into after 48 hours in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate with molar ratio ingredient magnetic agitation in deionized water medium of 2: 1,195 ± 5 ℃ of hydro-thermal reactions 6 days; (5) washing filtering is 3 times, dries 12 hours, and promptly obtains vanadium chromium Nano tube of composite oxides for 70 ℃.The XRD of the vanadium chromium Nano tube of composite oxides of gained and TEM figure are respectively as accompanying drawing 1,2.
Accompanying drawing 1 explanation, the position of each diffraction peak of XRD figure of synthetic product and relative intensity all match with the barium oxide nanotube collection of illustrative plates of bibliographical information, the diffraction peak of (001) face occurred in the low angle district, show that nanotube has laminate structure.Wherein ° locate the strongest (001) crystal face diffraction peak in 2 θ=2.22, corresponding d value is 3.98 nanometers, and the interlamellar spacing that the nanotube walls composite oxides are described is 3.98 nanometers.
Accompanying drawing 2 explanations, synthetic product is typical many walls Nano tube of composite oxides, and the external diameter of nanotube is 60～90 nanometers, and internal diameter is 15～40 nanometers.
Embodiment 2
(1) vanadium pentoxide powder and titanium hydride powders being dissolved in mass concentration by 1: 1 mol ratio is vigorous stirring 50 hours in 40% the hydrogen peroxide, composite vanadium-titanium oxides solution; (2) solution with gained becomes gel then at 50 ℃ of heating formation in 1 hour colloidal sol; (3) gel with gained forms composite vanadium-titanium oxides xerogel V 55 ± 5 ℃ of dryings
8Ti
4O
28NH
2O, i.e. V
4/3Ti
2/3O
14/3MH
2O; (4) with V
4/3Ti
2/3O
14/3MH
2O and cetylamine move into after 48 hours in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate with molar ratio ingredient magnetic agitation in deionized water medium of 2: 1,165 ± 5 ℃ of hydro-thermal reactions 8 days;
(5) washing filtering is 3 times, dries 10 hours, and promptly obtains the composite vanadium-titanium oxides nanotube for 95 ± 5 ℃.The composite vanadium-titanium oxides nanotube XRD of gained and TEM figure are respectively as accompanying drawing 3,4.
Accompanying drawing 3 explanation, the position of each diffraction peak of XRD figure of synthetic product and relative intensity all match with the barium oxide nanotube collection of illustrative plates of bibliographical information, the diffraction peak of (001) face occurred in the low angle district, show that nanotube has laminate structure.Wherein ° locate the strongest (001) crystal face diffraction peak in 2 θ=2.24, corresponding d value is 3.29 nanometers, and the interlamellar spacing that the nanotube walls composite oxides are described is 3.29 nanometers.
Accompanying drawing 4 explanations, synthetic product is typical many walls Nano tube of composite oxides, and the external diameter of nanotube is 120～130 nanometers, and internal diameter is 50 nanometers.
Embodiment 3～embodiment 5:
| Embodiment number | Raw material | Mol ratio | Template | Hydro-thermal time/sky |
| Embodiment 3 | V 2O 5+CrO 3 | 1∶1 | N-Laurylamine | 7 |
| Embodiment 4 | V 2O 5+CrO 3 | 3∶2 | Cetylamine | 7 |
| Embodiment 5 | V 2O 5+TiH 2 | 1∶1 | N-Laurylamine | 7 |
| Embodiment 6 | V 2O 5+TiH 2 | 3∶2 | Cetylamine | 7 |
Can obtain corresponding vanadium chromium Nano tube of composite oxides product, composite vanadium-titanium oxides nanotube product by above experiment parameter with reference to the method for embodiment 1.
Claims (2)
1, a kind of precursor body of Nano tube of composite oxides of multielement vanadium material is characterized in that, its phraseology is: V
12-yM
yO
30-0.5yH
2O, wherein M is Cr or Ti; 0.0＜y≤4.0.
2, the described precursor body of Nano tube of composite oxides of multielement vanadium preparation methods of claim 1 is characterized in that preparation process is:
Step 1, be 〉=1.0 with mol ratio, dissolved in mass concentration and be in 10%～40% the hydrogen peroxide vigorous stirring 30～50 hours, obtain vanadium and chromium or titanium composite oxide solution Vanadium Pentoxide in FLAKES and chromium trioxide or titanium hydride powders;
Step 2, the composite oxides solution that step 1 is obtained heated 〉=1 hour at 50～70 ℃, made peroxide breakdown formation colloidal sol wherein become gel then;
Step 3, the gel that step 2 is obtained form the composite oxides of multielement vanadium xerogel 50～60 ℃ of dryings, promptly obtain precursor body of Nano tube of composite oxides of multielement vanadium V
12-yM
yO
30-0.5YH
2O, wherein M is Cr or Ti; 0.0＜y≤4.0.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101767771B (en) * | 2010-01-08 | 2013-03-20 | 武汉理工大学 | Preparation method of vanadium oxide/carbon nanometer tube composite materials with interpenetrating network structures |
| CN104091940A (en) * | 2014-07-04 | 2014-10-08 | 武汉理工大学 | Chrome-vanadium oxide nano-particle as well as preparation method and application thereof |
| CN104907064A (en) * | 2015-06-25 | 2015-09-16 | 湖北工业大学 | Catalyst composition for degrading methylene blue dye in wastewater as well as preparation method and application of catalyst composition |
| CN109775758A (en) * | 2018-12-26 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Preparation method of large-layer-spacing vanadium pentoxide |
| CN115072779A (en) * | 2022-06-08 | 2022-09-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Positive electrode material V of lithium ion battery 2 O 5 Nanotube and preparation method of lithium ion button battery thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2739373B1 (en) * | 1995-09-29 | 1997-10-31 | Rhone Poulenc Fibres | PROCESS FOR THE PREPARATION OF AMMOXIDATION CATALYSTS |
| DE19542755A1 (en) * | 1995-11-16 | 1997-05-22 | Basf Ag | Multimetal oxides |
| CN1202017C (en) * | 2003-09-04 | 2005-05-18 | 武汉理工大学 | Vanadium oxide nanometer tube adulterated with metal cation and preparation method thereof |
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2006
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101767771B (en) * | 2010-01-08 | 2013-03-20 | 武汉理工大学 | Preparation method of vanadium oxide/carbon nanometer tube composite materials with interpenetrating network structures |
| CN104091940A (en) * | 2014-07-04 | 2014-10-08 | 武汉理工大学 | Chrome-vanadium oxide nano-particle as well as preparation method and application thereof |
| CN104091940B (en) * | 2014-07-04 | 2016-08-31 | 武汉理工大学 | Chrome alum oxide nano particles and its preparation method and application |
| CN104907064A (en) * | 2015-06-25 | 2015-09-16 | 湖北工业大学 | Catalyst composition for degrading methylene blue dye in wastewater as well as preparation method and application of catalyst composition |
| CN109775758A (en) * | 2018-12-26 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Preparation method of large-layer-spacing vanadium pentoxide |
| CN115072779A (en) * | 2022-06-08 | 2022-09-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Positive electrode material V of lithium ion battery 2 O 5 Nanotube and preparation method of lithium ion button battery thereof |
| CN115072779B (en) * | 2022-06-08 | 2023-11-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Lithium ion battery anode material V 2 O 5 Preparation method of nanotube and lithium ion button cell thereof |
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| CN100404426C (en) | 2008-07-23 |
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