CN108927139A - Nano bar-shape Nb-CeO2Material preparation method and products thereof and application - Google Patents
Nano bar-shape Nb-CeO2Material preparation method and products thereof and application Download PDFInfo
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- CN108927139A CN108927139A CN201810650296.XA CN201810650296A CN108927139A CN 108927139 A CN108927139 A CN 108927139A CN 201810650296 A CN201810650296 A CN 201810650296A CN 108927139 A CN108927139 A CN 108927139A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000010955 niobium Substances 0.000 claims abstract description 15
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 11
- 229910052758 niobium Inorganic materials 0.000 claims description 11
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 11
- 229910000510 noble metal Inorganic materials 0.000 claims description 5
- 239000008246 gaseous mixture Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000002019 doping agent Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 150000004687 hexahydrates Chemical class 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 11
- 238000006555 catalytic reaction Methods 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 14
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 239000003643 water by type Substances 0.000 description 9
- 239000010931 gold Substances 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 229910000484 niobium oxide Inorganic materials 0.000 description 5
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- CQGVSILDZJUINE-UHFFFAOYSA-N cerium;hydrate Chemical compound O.[Ce] CQGVSILDZJUINE-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of nano bar-shape Nb-CeO2Material and its preparation method and application, the material are by the Nb of mass ratio 1%-3%2O5With the CeO of 97%-99%2Composition, it is dissolved after niobium oxalate and cerous nitrate while being added drop-wise in sodium hydroxide solution respectively by deionized water, filtration washing obtains after being placed in Muffle furnace simply roasting, method of the invention has preparation easy, do not introduce template, the advantages that product is evenly distributed, and is suitable for industrial mass production.The material has excellent reduction-oxidation performance, can be used as catalyst or carrier is applied in all kinds of catalysis reaction.
Description
Technical field
The present invention relates to a kind of nano bar-shape Nb-CeO2Material preparation method and products thereof and application, belong to material preparation and
Environmental technology field, which can be used as catalyst or carrier uses.
Background technique
CeO2With unique cubic fluorite type crystal structure, there is the characteristic easily appraised at the current rate, pass through Ce3+And Ce4+It is mutual
The storage and release of oxygen are realized in conversion, are a kind of environmentally friendly materials, have in fields such as energy and environment all more important
Using.Cerium oxide acts not only as active component, and can also be as the good carrier of other active components.Into cerium oxide
Second of metal is added, can further improve its performance by introducing lattice defect.It is designed by microscopic appearance structure, Ke Yijin
One step expands material specific surface area, improves catalytic activity.
Along with application of the vanadium in environmental pollution, niobium also starts to be concerned as it with the element of family.In fact,
The compound of niobium is gone as new catalytic material in hydrocarbon oxidation dehydrogenation, methane oxidation coupling, oxidation and ammoxidation, nitrogen oxide
Except etc. numerous kinds catalysis reaction in significant catalytic action has had been displayed, as carrier in hydrogenation, metathesis reaction, oxygen
Change, solid acid reaction etc. play apparent facilitation, only its in the environment using on the low side.Due to redox ability
It is one of field of environmental improvement key factor in need of consideration, meanwhile, the compound of niobium has certain redox ability, can
As carrier or auxiliary agent intensified response activity.Therefore, niobium is incorporated into cerium oxide by the present invention, prepares the cerium oxide of niobium doping
Object is closed, the more active crystal face of nano bar-shape microstructure exposure will greatly improve the performance of catalyst.
Found through retrieval, adulterate the second metal in cerium oxide in recent years while adjusting the research of its microscopic appearance it is more, it is such as special
Sharp CN106745170A, hydro-thermal method have synthesized a kind of cobalt doped cerium oxide nano materials of laminated structure；Patent
CN106732540A, hydro-thermal method have synthesized a kind of additive Mn cerium dioxide nano flower visible-light photocatalyst, have shown preferable
Catalytic activity.But need to introduce surfactant in above-mentioned synthetic method to promote the self assembly of nano particle or using melting
The raw material of state causes higher raw material/energy waste and increases cost.Although the cerium oxide of synthesis nano bar-shape has had
It reports (patent CN105502468A), but incorporation niobium oxide prepares the cerium oxide of the niobium doping of nano bar-shape simultaneously into cerium oxide
Without relevant report.Moreover, as previously mentioned, the material of niobium doping is in related oxidized reaction using seldom.Based on this, the present invention is mentioned
For a kind of nano bar-shape niobium doped cerium oxide material, and a kind of simple preparation method is provided, is applied to benzene combustion reaction
In.The material will have very big application potential in VOCs improvement field.
Summary of the invention
In order to overcome the deficiencies of the prior art, it is an object of that present invention to provide a kind of nano bar-shape Nb-CeO2The preparation of material
Method.
Another object of the present invention is: providing a kind of nano bar-shape Nb-CeO of above method preparation2Material product.
Another object of the present invention is to: a kind of application of the said goods is provided.
The present invention is achieved by the following technical solutions: a kind of nano bar-shape Nb-CeO2The preparation method of material, it is special
Sign is that the material is by the Nb of mass ratio 1%-3%2O5With the CeO of 97%-99%2Composition, which is by deionization moisture
It Rong Xie not be added drop-wise in sodium hydroxide solution simultaneously after niobium oxalate and cerous nitrate, filtration washing is placed in Muffle furnace and simply roasts
After obtain, comprising the following steps:
The first step weighs cerous nitrate (III) hexahydrate and is dissolved in deionized water, after stirring and dissolving solution A；Weigh a small amount of grass
Sour niobium, after stirring and dissolving solution B；Sodium hydroxide is separately weighed, obtains solution C after stirring and dissolving；
Under second step, strong stirring, solution A and solution B are added dropwise in solution C simultaneously, and continue to stir 0.5-1h, obtained
Suspension D；
Suspension D is put into hydrothermal reaction kettle by third step, hydrothermal reaction kettle is put into the baking oven for set temperature and is carried out instead
It answers, obtains suspension E after the reaction was completed；
4th step, by suspension E washing repeatedly until filtrate be neutrality, be placed in set temperature baking oven and dried, later
Obtain precipitating F；
5th step will precipitate F and be placed in and sets Muffle kiln roasting certain time of temperature to get to the Nb-CeO2's
Catalysis material.
The first step, in the solution A, B, C, solution concentration is respectively 0.5mol/L, 0.005 ~ 0.01mol/L, 6mol/L,
Solution concentration is adjusted according to dopant material mass ratio difference.
Third step, oven temperature are set as 100 DEG C, and the reaction time is -36h for 24 hours.
4th step, oven temperature are set as 70 DEG C, baking time 12h-24h.
5th step, muffle furnace are set as 400 DEG C, calcining time 2-4h.
A kind of nano bar-shape Nb-CeO2Material is prepared according to any of the above-described the method, which is by mass ratio
The Nb of 1%-3%2O5With the CeO of 97%-99%2Composition.
A kind of nano bar-shape Nb-CeO2Material is as carrier, when carried noble metal, in the aflame application of benzene, reaction pressure
Power is normal pressure~1 atm, and reaction velocity is 30000 mL/ (gh), and in the gaseous mixture of air and benzene vapor, the concentration of benzene is
1000 ppm。
The present invention provides a kind of Nb2O5The CeO of doping2Nano bar-shape new material and preparation method thereof, provided material can
As carrier, when carried noble metal, fabulous benzene combustibility is shown；Provided method has preparation easy, does not introduce
The advantages that template/surfactant, product is evenly distributed, is suitable for industrial mass production.After SEM shows doping vario-property
Oxide is uniform nano bar-shape pattern, and XRD is the result shows that obtained doping oxide is face-centred cubic fluorite structure.
The present invention needs the conditions such as suitable hydrothermal temperature and roasting heating rate.Firstly, to obtain good mix
Miscellaneous oxide catalyst and its crystallite dimension is controlled, the present invention needs to select suitable maturing temperature, when temperature is too low, is unfavorable for
The rock-steady structure for the nanometer rods being self-assembly of, and reactant reaction is insufficient causes there are hydroxide, temperature is excessively high then
Cause nanometer rods to be grown up and agglomerate into bulky grain, is unfavorable for the catalytic performance of material.Secondly it is heavy that the present invention, which selects sodium hydroxide,
Shallow lake agent, due to sodium hydroxide be highly basic, in high concentration basic environment, nanometer rods will by the nano particle of smaller particle assemble and
At, and more pore structure is formed, the specific surface area of catalysis material is improved, is conducive to adsorb more contaminant molecules, conducive to being negative
The noble metal of load provides anchor point.Heating rate, maturing temperature and time etc. will affect CO or CO in reaction process2Gas
The generation and release of body, and then influence the crystal phase structure and microscopic appearance of product.Heating rate will affect crystal structure, and temperature
It then will affect crystal grain with the time to grow up, and further the microscopic appearance of product had an impact.Further, due to cerium and niobium
Atom is of different sizes, when crystal grain is grown up, easily makes deformation of crystal structure, on the one hand may promote the raising of performance, on the other hand
Also the microscopic appearance and crystal phase structure of product be will affect.
Preferably, in third step: the hydrothermal temperature is 100 DEG C, and the reaction time is -36h for 24 hours.Suitable hydro-thermal
Reaction temperature help to obtain good crystal phase structure, catalyst morphology, and suitable the hydro-thermal reaction time can guarantee nanometer
The completion of self assembling process before grain, avoids the random agglomeration of subsequent process, influences material property.In the temperature of selection
It spends under (100 DEG C), it is ensured that come into full contact between hydroxide particles, obtain the doping oxide of nano bar-shape, and to benzene
Catalysis oxidation shows optimal performance.
Preferably, in the 5th step: the maturing temperature is 400 DEG C, calcining time 2h-4h.Suitable maturing temperature and
Time can guarantee that presoma decomposes sufficiently, and Effective Doping can also be protected conducive to the catalysis material with more crystal defect is obtained
Demonstrate,prove the stabilization of nanometer rods pattern.
Method disclosed by the invention can be prepared by uniform nano bar-shape Nb-CeO without introducing template2Material is compared
Bigger in granular material specific surface area, catalytic performance is good.Preparation method of the present invention be suitable for other simple two-spots or
In the synthesis of ternary metal oxide；The preparation method is cheap, easy to operate with raw material, does not introduce template, product point
The advantages that cloth is uniform, is suitable for industrial mass production, products therefrom can be used as carrier-supported precious metal, the combustion of this catalyst
The activity for burning VOCs is very high.Compared with prior art, the invention has the following advantages that
(1) the present invention provides a kind of novel nano club-shaped material, which can be used as the preparation such as carrier-supported precious metal such as gold
The activity of noble metal catalyst, catalysis burning benzene is very high.
(2) present invention used in raw material it is simple, it is low in cost, easy to operate, do not introduce template/surfactant, produce
The advantages that object is evenly distributed, and is suitable for industrial mass production.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the XRD diagram of material described in the embodiment of the present invention 1；
Fig. 2 is the SEM figure of material described in the embodiment of the present invention 1；
Fig. 3 is the SEM figure of material described in the embodiment of the present invention 2；
Fig. 4 is the SEM figure of material described in the embodiment of the present invention 3；
Fig. 5 is the embodiment of the present invention 2, (wt after the gold of material load described in embodiment 3Au%=1) active testing figure.
Specific embodiment
Elaborate below to the embodiment of the present invention: the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1:
It weighs in six nitric hydrate cerium of 4.34g, 50 mL beaker, 20 mL deionized waters is added, obtain solution A after stirring and dissolving；Claim
It takes 5.38g niobium oxalate to be placed in 500mL beaker, 200 mL deionized waters is added, stirring and dissolving is placed on 1000mL volumetric flask and adds
Water constant volume, obtains solution B；It weighs 12g sodium hydroxide to be placed in 100 mL beakers, 50 mL deionized waters is added, heating stirring is molten
Solution obtains solution C.Under vigorous stirring, solution A and the solution B of 10ml are added dropwise in solution C simultaneously, form suspension D.It will
Suspension is transferred in 100mL hydrothermal reaction kettle, and water heating kettle is put into 100 DEG C of baking ovens and is reacted for 24 hours.After the reaction was completed, it will sink
It forms sediment and filters, repeatedly, drying is placed in Muffle furnace and is roasted, 2 DEG C/min of heating rate for washing, and 400 DEG C of maturing temperature, roasting
Time 2h is burnt, furnace cooling later is to get the Nb-CeO for arriving the nano bar-shape2Catalysis material (cerium oxide and niobium oxide
Molar ratio 100:1).As shown in Fig. 2 SEM result.The XRD of embodiment 1 is the result shows that catalyst is cubic fluorite structure in Fig. 1.
Embodiment 2:
It weighs in six nitric hydrate cerium of 4.34g, 50 mL beaker, 20 mL deionized waters is added, obtain solution A after stirring and dissolving；Claim
It takes 5.38g niobium oxalate to be placed in 500mL beaker, 200 mL deionized waters is added, stirring and dissolving is placed on 1000mL volumetric flask and adds
Water constant volume, obtains solution B；It weighs 12g sodium hydroxide to be placed in 100 mL beakers, 50 mL deionized waters is added, heating stirring is molten
Solution obtains solution C.Under vigorous stirring, solution A and the solution B of 10ml are added dropwise in solution C simultaneously, form suspension D.It will
Suspension is transferred in 100mL hydrothermal reaction kettle, and water heating kettle is put into 100 DEG C of baking ovens and reacts 36h.After the reaction was completed, it will sink
It forms sediment and filters, repeatedly, drying is placed in Muffle furnace and is roasted, 2 DEG C/min of heating rate for washing, and 400 DEG C of maturing temperature, roasting
Time 2h is burnt, furnace cooling later is to get the Nb-CeO for arriving the nano bar-shape2Catalysis material (cerium oxide and niobium oxide
Molar ratio 100:1).As shown in Fig. 3 SEM result.
Embodiment 3:
It weighs in six nitric hydrate cerium of 4.34g, 50 mL beaker, 20 mL deionized waters is added, obtain solution A after stirring and dissolving；Claim
It takes 5.38g niobium oxalate to be placed in 500mL beaker, 200 mL deionized waters is added, stirring and dissolving is placed on 1000mL volumetric flask and adds
Water constant volume, obtains solution B；It weighs 12g sodium hydroxide to be placed in 100 mL beakers, 50 mL deionized waters is added, heating stirring is molten
Solution obtains solution C.Under vigorous stirring, solution A and the solution B of 10ml are added dropwise in solution C simultaneously, form suspension D.It will
Suspension is transferred in 100mL hydrothermal reaction kettle, and water heating kettle is put into 100 DEG C of baking ovens and reacts 36h.After the reaction was completed, it will sink
It forms sediment and filters, repeatedly, drying is placed in Muffle furnace and is roasted, 2 DEG C/min of heating rate for washing, and 400 DEG C of maturing temperature, roasting
Time 4h is burnt, furnace cooling later is to get the Nb-CeO for arriving the nano bar-shape2Catalysis material (cerium oxide and niobium oxide
Molar ratio 100:1).Microscopic appearance is as shown in Fig. 4 SEM result.
Application examples
Using the cerium oxide carrier of above-mentioned doping niobium oxide as catalyst carrier, it is negative that coprecipitation mode is further sunk to the bottom using tradition
Active group parting is carried, and tests its catalytic activity.Material load gold described in embodiment 3 is prepared into after catalyst and is placed on
The gaseous mixture that benzene vapor and air are passed through in continuous flow fixed bed device is reacted；Reaction pressure is normal pressure~1 atm,
Reaction velocity is 30000 mL/ (gh), and in the gaseous mixture of air and benzene vapor, the concentration of benzene is 1000 ppm.
(wt after the material load gold as described in Fig. 5 is embodiment 2 and embodiment 3Au%=1) active testing figure, as a result table
Bright, material load Au catalyst described in embodiment 2 is 169 DEG C for the initiation temperature of benzene combustion reaction, the temperature of conversion ratio 90%
Degree is 258 DEG C, and material load Au catalyst described in embodiment 3 is 152 DEG C for the initiation temperature of benzene combustion reaction, conversion ratio
90% temperature is 249 DEG C.
Specific embodiments of the present invention are described above.It should be noted that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (7)
1. a kind of nano bar-shape Nb-CeO2The preparation method of material, it is characterised in that the material is by the Nb of mass ratio 1%-3%2O5
With the CeO of 97%-99%2Composition, which is after dissolving niobium oxalate and cerous nitrate respectively by deionized water while to be added drop-wise to
In sodium hydroxide solution, filtration washing obtains after being placed in Muffle furnace simply roasting, comprising the following steps:
The first step weighs cerous nitrate (III) hexahydrate and is dissolved in deionized water, after stirring and dissolving solution A；Weigh a small amount of grass
Sour niobium, after stirring and dissolving solution B；Sodium hydroxide is separately weighed, obtains solution C after stirring and dissolving；
Under second step, strong stirring, solution A and solution B are added dropwise in solution C simultaneously, and continue to stir 0.5-1h, obtained
Suspension D；
Suspension D is put into hydrothermal reaction kettle by third step, hydrothermal reaction kettle is put into the baking oven for set temperature and is carried out instead
It answers, obtains suspension E after the reaction was completed；
4th step, by suspension E washing repeatedly until filtrate be neutrality, be placed in set temperature baking oven and dried, later
Obtain precipitating F；
5th step will precipitate F and be placed in and sets Muffle kiln roasting certain time of temperature to get to the Nb-CeO2Urge
Change material.
2. nano bar-shape Nb-CeO according to claim 12The preparation method of material, which is characterized in that the first step, it is described molten
In liquid A, B, C, solution concentration is respectively 0.5mol/L, 0.005 ~ 0.01mol/L, 6mol/L, not according to dopant material mass ratio
With adjustment solution concentration.
3. nano bar-shape Nb-CeO according to claim 12The preparation method of material, which is characterized in that third step, baking oven temperature
Degree is set as 100 DEG C, and the reaction time is -36h for 24 hours.
4. nano bar-shape Nb-CeO according to claim 12Material and preparation method thereof, which is characterized in that the 4th step, baking oven
Temperature setting is 70 DEG C, baking time 12h-24h.
5. nano bar-shape Nb-CeO according to claim 12Material and preparation method thereof, which is characterized in that the 5th step, Muffle
Furnace temperature is set as 400 DEG C, calcining time 2-4h.
6. a kind of nano bar-shape Nb-CeO2Material, it is characterised in that -5 any preparation methods obtain according to claim 1, should
Material is by the Nb of mass ratio 1%-3%2O5With the CeO of 97%-99%2Composition.
7. nano bar-shape Nb-CeO according to claim 62Material is as carrier, when carried noble metal, answers benzene is aflame
It is normal pressure~1 atm with, reaction pressure, reaction velocity is 30000 mL/ (gh), in the gaseous mixture of air and benzene vapor, benzene
Concentration be 1000 ppm.
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