CN107010674A - α-Fe2O3Nanometer rods and Au/ α-Fe2O3Catalyst and its synthesis and application - Google Patents
α-Fe2O3Nanometer rods and Au/ α-Fe2O3Catalyst and its synthesis and application Download PDFInfo
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- CN107010674A CN107010674A CN201610048168.9A CN201610048168A CN107010674A CN 107010674 A CN107010674 A CN 107010674A CN 201610048168 A CN201610048168 A CN 201610048168A CN 107010674 A CN107010674 A CN 107010674A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses α Fe2O3Nanometer rods and Au/ α Fe2O3Catalyst and its synthesis and application.α Fe of the present invention2O3The bar-shaped structure of porous nano is maintained, the average-size of Au particles increases to 8.6nm from 2.2nm.Meanwhile, α Fe2O3Nano bar-shape structure can also modulation Au nano-particles pattern, through 300,400,500 DEG C be calcined after Au/ α Fe2O3The pattern of Au nano-particles is respectively dimensional thinlayer shape on catalyst, three-dimensional rescinded angle is octahedra and sheet rescinded angle is octahedra, embodies α Fe2O3Uniqueness of the club shaped structure on scattered and stable Au nano particle structures.Prepared Au/ α Fe2O3Catalyst can be catalyzed CO oxidations at room temperature, and its reaction rate reaches 0.8047molCO/gAuh。
Description
Technical field
The present invention relates to a kind of porous α-Fe2O3Nanometer rods and its synthetic method.
The present invention relates to a kind of α-Fe2O3Load Au nano-particle catalysts and regulation and control Au/ α-Fe2O3Au receives on catalyst
The synthetic method of rice corpuscles pattern.
The present invention relates to a kind of Au/ α-Fe2O3The application of catalytic CO Oxidation at room temperature reaction.
Background technology
α-Fe2O3With excellent redox property and crystalline phase stability, it is widely used as metal nanoparticles loaded
Catalyst carrier.Such as, Au/ α-Fe2O3Catalyst shows excellent catalysis CO by the interaction of metal and carrier and aoxidized
Reactivity worth [Chem.Lett., 1987,16,405；J.Catal.,1989,115,301；Science,2008,321,1331；
Catal.Sci.Technol.,2013,3,2881].Numerous studies show α-Fe2O3Pattern and size be influence Au/ α-
Fe2O3One of key factor of catalyst performance；Such as G.H.Wang by Au nanometer particle loads different sizes and pattern α-
Fe2O3In nano material, the more nanometer spindle α-Fe of defective bit are found2O3Prepared Au/ α-Fe2O3It is catalyzed CO oxidations
Activity is far above rhombus α-Fe2O3The Au catalyst [Appl.Catal.A, 2009,364,42] of nanometer particle load.
A.Gedanken etc. utilizes the α-Fe containing 1-5nm cavernous structures2O3During nanometer rods load gold nano particle, it is found that its CO is aoxidized
Activity be higher than the Au catalyst that is loaded with nano spherical particle, its reason is this poroid α-Fe2O3It can be very good point
Scattered and stable 1-5nm golden nanometer particle [Chem.Mater., 2007,19,4776].Influence Au/ α-Fe2O3Catalyst performance
Another key factor is the pattern of Au nano-particles.Such as A.A.Herzing has found Au/ α-Fe2O3It is catalyzed the activity of CO oxidations
Position is the Au nano-clusters with double-decker, and the activity of the Au nano-clusters of single layer structure catalysis CO oxidations is then poor
[Science,2008,321,1331].But due to α-Fe2O3The heterogeneity of carrier dimensions and pattern, the ratio of Au active species is small
In 20%, cause Au atom utilization ratios relatively low.Up to the present, in regulation and control α-Fe2O3On carrier in terms of Au species pattern still
Lack effective technology path.
In addition, Au/ α-Fe2O3Catalyst is during calcination process, and generally existing Au nano-particles easy-sintering and becomes big,
Cause the significantly decline of catalyst performance.Au/ α-the Fe prepared such as J.Hua et al. using coprecipitation2O3Catalyst is in 350-
After 550 DEG C of roasting 2h, Au nano-particles sizes rise to 8.5nm from 5.7nm, and its size distribution ranges is significantly broadened
(3.0-18.0nm)[Appl.Catal.A,2004,259,121].The Au/ α that P.Landon et al. is prepared using coprecipitation-
Fe2O3Catalyst is calcined after 3h in 400-600 DEG C, and subsphaeroidal Au nano-particles sizes increase to 16.1nm from 3.7nm
[J.Mater.Chem.,2006,16,199].As can be seen that how to suppress Au/ α-Fe from the studies above progress2O3Catalyst
Sintering of the upper Au nano-particles in roasting process, especially in α-Fe2O3The pattern of selective regulation Au species is still on carrier
It is the challenge of current nano material and nano-catalytic research field.
The content of the invention
It is an object of the invention to provide a kind of porous α-Fe2O3The preparation method of nanometer rods.
It is an object of the invention to provide utilize above-mentioned α-Fe2O3Nanometer rods regulate and control Au nano-particles sizes and pattern, solve Au and receive
Rice corpuscles high temperature easy-sintering, the problem of decentralization declines.
It is an object of the invention to provide above-mentioned α-Fe2O3Nanometer rods load Au nano-particles are that catalyst is applied to room temperature CO oxygen
Change reaction.
The purpose of the present invention is achieved by the following technical solution：
A kind of α-Fe2O3Nanometer rods synthetic method, comprises the following steps：
(1) inorganic molysite, NaCl, polyethylene glycol (PEG-400) are dissolved in a certain amount of water, form iron concentration
For 0.05~0.2mol/L solution, stir and heat up and be heated to 100~140 DEG C；
(2) by a certain amount of 0.1~0.5mol/L Na2CO3Solution is slowly added into above-mentioned solution, and stirring aging 1 is small
When, the pH of system is 8.0~12.0；
(3) product of aging is obtained into β-FeOOH nanometer rods after filtering, washing, drying；
(4) α-Fe are obtained in 300~600 DEG C of DEG C of air roastings 3~6 hours in β-FeOOH presomas2O3Nanometer rods.
The molysite is FeCl3·6H2O；The volume ratio of described solvent is PEG/H2O=1/19；
NaCl mass concentration is 58.5g/L in the system.
0.05~0.2mol/L of iron concentration of described system is preferred.
The Na of the system2CO30.1~0.5mol/L of concentration is preferred.
Described system pH=8.0~12.0 are preferred.
Described reaction temperature is preferred with 100~140 DEG C.
Product structure is characterized using Rigaku D/MAX-2500/PC types x-ray powder diffraction instrument, its XRD test result is such as
Shown in Fig. 1 a, it is the single α-Fe of crystalline phase to show product2O3.Using Hitachi HT7700 type transmission electron microscope observing α-Fe2O3's
Pattern, test result such as Fig. 2, a diameter of 40-50nm, length is 300-500nm, while having loose structure.
A kind of α-Fe2O3Supported active Au nano-particle catalyst synthetic methods, comprise the following steps：
(1) described α-Fe are utilized2O3Nanometer rods are distributed to (2~5) × 10 as carrier-4The mol/L gold salt aqueous solution
In, and it is heated to 60~100 DEG C；
(2) by a certain amount of 0.005~0.02mol/L Na2CO3Solution is slowly added into above-mentioned solution, and regulation pH is
5.0~7.0, stirring aging 1 hour；
(3) solid product is calcined in 300~500 DEG C of air after filtering, washing, drying, obtains product Au-T and urge
Agent (T represents sintering temperature).
The gold salt is HAuCl4The aqueous solution, concentration is with (2~5) × 10~4Mol/L is preferred.
The precipitating reagent is Na2CO3The aqueous solution, concentration is preferred using 0.005~0.02mol/L.
Described system is preferred with pH=5.0~7.0.
Described reaction temperature is preferred with 300~500 DEG C.
Product structure is characterized using Rigaku D/MAX-2500/PC types x-ray powder diffraction instrument, its XRD test result is such as
Shown in Fig. 1 b-d, it is the single α-Fe of crystalline phase to show product2O3, peak shape is sharp, shows that product crystallinity is good.Using JEM-
ARM200F type transmission electron microscope observing Au/ α-Fe2O3Pattern, the size of Au particles is adjustable in the range of 2.2~8.6nm；Au
The pattern of nano-particle is respectively dimensional thinlayer shape, three-dimensional rescinded angle is octahedra and sheet rescinded angle is octahedra.
Utilize α-Fe2O3Nanometer rods load Au nano-particle catalysts are used for room temperature CO oxidation reactions, comprise the following steps：
(1) described α-Fe are utilized2O3Nanometer rods load Au 15~200mg of nano-particle catalyst, 300 DEG C,
20vol.%O2/N21~2h is pre-processed under atmosphere, room temperature (25~30 DEG C) is down to；
(2) in room temperature (25~30 DEG C), be passed through reacting gas 1.0vol.%CO/2.5vol.%O2/ He, flow velocity 50~
200mL/min, reacts 12h；
The catalyst amount is preferred using 15~200mg.
The reaction pretreatment time is preferred using 1~2h
The reaction flow velocity is preferred using 50~200mL/min.
Using gas-chromatography on-line analysis product, its CO oxidation reactions result as shown in fig. 6, Au-300 and Au-400 catalysis
The CO of agent conversion ratio is respectively 95% and 24%, and Au-500 catalyst embodies obvious size then almost without activity
Sensitiveness.Corresponding reaction dynamics data is shown in Table 1, illustrated in Figure 1 where it can be seen that when the average-size of Au particles is from 2.2nm (Au-
300) 3.5nm (Au-400) is increased to, it is 0.0392mol that reaction rate lowers from 0.8074CO/(gAuh)；And when gold particle is flat
When equal size increases to 8.6nm, then almost without catalytic activity.
The present invention effect and advantage be：(1) using polyol process synthesis α-Fe2O3Nanometer rods, technique is simple, environment friend
It is good；(2) inorganic Jin Yuan is used, deposition-precipitation method prepares Au/ α-Fe2O3Catalyst, the heat endurance and decentralization of Au nano-particles
It is improved；(3)Au/α-Fe2O3Can room temperature catalysis CO oxidation reactions, and show obvious dimensional effect.
Brief description of the drawings
Fig. 1 is the XRD spectra of the sample as prepared by the embodiment 1-4 using the inventive method.Abscissa is the θ of angle 2, single
Position is ° (degree), and ordinate is diffracted intensity, and unit is a.u. (absolute unit).
Fig. 2 is the transmission electron microscope picture (TEM) of sample prepared by the embodiment of the present invention 1.
Fig. 3 is the transmission electron microscope picture (TEM) of sample prepared by the embodiment of the present invention 2.
Fig. 4 is the transmission electron microscope picture (TEM) of sample prepared by the embodiment of the present invention 3.
Fig. 5 is the transmission electron microscope picture (TEM) of sample prepared by the embodiment of the present invention 4.
Fig. 6 is the reactivity worth of sample catalysis CO oxidations prepared by 2-4 of the embodiment of the present invention.
Embodiment
Table 1 is the reaction dynamics data that 2-4 of the embodiment of the present invention prepares gained sample.
Embodiment 1
By 5.408g FeCl3·6H2O, 11.6g NaCl, 10mL PEG add 190mL water in, stir and heat up as
120℃；Then by 200mL 0.2mol/L Na2CO3Solution is added to above-mentioned in the speed (6 hours) with 0.55mL/min
After solution, continue to stir simultaneously aging 1 hour；It is 8.0~12.0 to adjust pH, by the product of aging after filtering, washing, drying,
In being calcined 5 hours at 500 DEG C, solid powder is obtained.It is α-Fe through XRD analysis2O3Crystalline phase, its XRD spectra is shown in Fig. 1 a；TEM image
Fig. 2 is seen respectively.As a result synthesized α-Fe are shown2O3Sample has nano bar-shape structure, and a diameter of 40-50nm, length is 300-
500nm, its specific surface area is 79m2/ g, average pore size about 20nm.
Embodiment 2
Take the 1g α-Fe obtained in case study on implementation 12O3Nanometer rods are scattered in 300mL and contain HAuCl4(4.9×10-4mol/L)
The aqueous solution in, be heated to after 80 DEG C, add 60mL0.01mol/L Na2CO3Solution, regulation pH is 5.9.At such a temperature
After aging 1h, after filtering, washing, 120 DEG C of dry 12h obtain solid precursor.In 300 DEG C of air be calcined 5h obtained by Au/ α-
Fe2O3Catalyst is labeled as Au-300, and wherein Au loading is 1.6wt.%.Its XRD spectra and TEM pictures are shown in Fig. 1 b respectively
With Fig. 3 a；A diameter of 40-50nm of carrier nanometer rods, length is 300-500nm；The average-size of Au nano-particles is 2.2nm,
Further find that Au nano-particles are mainly dimensional thinlayer shape structure by HRTEM (Fig. 3 b) analysis.
Embodiment 3
Take in case study on implementation 2 solid precursor to be calcined 5h in 400 DEG C, gained sample is labeled as Au-400, its XRD spectra and
TEM pictures are shown in Fig. 1 c and Fig. 4 a respectively；α-Fe2O3The pattern and crystalline phase of carrier keep constant；The average-size of Au nano-particles is
3.5nm, its pattern is mainly that three-dimensional rescinded angle is octahedra (Fig. 4 b).
Embodiment 4
Take in case study on implementation 2 solid precursor to be calcined 5h in 500 DEG C, gained sample is labeled as Au-500, its XRD spectra and
TEM pictures are shown in Fig. 1 d and Fig. 5 a respectively.α-Fe2O3The pattern and crystalline phase of carrier keep constant；The average-size of Au nano-particles is
8.6nm, its pattern is mainly that sheet rescinded angle is octahedra (Fig. 5 b).
Embodiment 5
In room temperature (25~30 DEG C), reaction gas 1.0vol.%CO/2.5vol.%O2Under the conditions of/He, flow velocity 50mL/min,
Prepared Au/ α-Fe are investigated2O3The CO oxidation susceptibilities of catalyst, as a result as shown in Figure 6.Au-300 and Au-400 catalyst
CO conversion ratio be respectively 95% and 24%, and Au-500 catalyst embodies obvious size quick then almost without activity
Perception.Corresponding reaction dynamics data is shown in Table 1, it can be seen that when the average-size of Au particles increases from 2.2nm (Au-300)
To 3.5nm (Au-400), it is 0.0392mol that reaction rate lowers from 0.8074CO/(gAuh)；And when gold particle average-size increases
When arriving 8.6nm greatly, then almost without catalytic activity.Simultaneously it can also be seen that reaction rate and gold particle pattern are also closely related；
The Au nano-particles and the interface girth of iron oxide formation for wherein exposing the lamelliform of more two-dimensional structure are maximum, are to obtain CO
Aoxidize the key factor of high activity.
Table 1
The present invention is using NaCl as structure directing agent, and polyethylene glycol (PEG) is pattern controlling agent, Na2CO3For precipitating reagent, in water
By controlling the hydrolysis dynamics of iron ion in solution, a diameter of 40-50nm is synthesized, length is 300-500nm, and with many
α-the Fe of pore structure2O3Nanometer rods.With this α-Fe2O3Nanometer rods are carrier, and Au/ α-Fe are prepared for using deposition-precipitation method2O3Urge
Agent.It is calcined in 300~500 DEG C of air after 5h, α-Fe2O3Maintain the bar-shaped structure of porous nano, the average-sizes of Au particles from
2.2nm increases to 8.6nm.Meanwhile, α-Fe2O3Nano bar-shape structure can also modulation Au nano-particles pattern, through 300,400,
Au/ α-Fe after 500 DEG C of roastings2O3The pattern of Au nano-particles is respectively dimensional thinlayer shape, three-dimensional rescinded angle octahedron on catalyst
It is octahedra with sheet rescinded angle, embody α-Fe2O3Uniqueness of the club shaped structure on scattered and stable Au nano particle structures.Institute
Au/ α-the Fe of preparation2O3Catalyst can be catalyzed CO oxidations at room temperature, and its reaction rate reaches 0.8047molCO/gAu h。
Claims (8)
1. a kind of α-Fe2O3Nanometer rods, a diameter of 40-50nm, length is 300-500nm, and specific surface area is 79g/m2。
2. α-Fe described in a kind of claim 12O3The synthetic method of nanometer rods, its processing step is：
(1) soluble inorganic molysite, NaCl, polyethylene glycol (PEG-400) are dissolved into the aqueous solution, forming iron concentration is
0.05~0.2mol/L solution, stirs and heats up and be heated to 100~140 DEG C；
(2) by 0.1~0.5mol/L Na2CO3Solution is slowly added into above-mentioned solution, stirring aging more than 1 hour, control
The pH of system is 8.0~12.0；
(3) product of aging is obtained into β-FeOOH nanometer rods after filtering, washing, drying；
(4) it is calcined 3~6 hours in 300~600 DEG C of air, obtains α-Fe2O3Nanometer rods.
3. α-Fe according to claim 22O3The synthetic method of nanometer rods, it is characterised in that the molysite is FeCl3·
6H2O。
4. α-Fe according to claim 12O3The synthetic method of nanometer rods, it is characterised in that：Polyethylene glycol in the system
With H2O volume ratio is 1/19.
5. α-Fe according to claim 12O3The synthetic method of nanometer rods, it is characterised in that：NaCl matter in the system
Amount concentration is 58.5g/L.
6. a kind of Au/ α-Fe2O3Catalyst, it is characterised in that：Carrier is the α-Fe described in claim 12O3Nanometer rods, Au is with carrying
The mass ratio (1.0~4.0)/100 of body, i.e. golden load capacity are 1.0%~4.0wt.% of carrier quality.
7. Au/ α-Fe described in a kind of claim 62O3Process for synthetic catalyst, it is characterised in that comprise the following steps：
(1) α-Fe described in claim 1 are utilized2O3Nanometer rods are distributed to (2~5) × 10 as carrier-4Mol/L gold salt water
In solution, 60~100 DEG C are heated to；
(2) by 0.005~0.2mol/L Na2CO3Solution is added in above-mentioned solution, and regulation system pH is 5.0~7.0, stirring
Aging more than 1 hour；
(3) product of aging is calcined 3~6 hours in 300~500 DEG C of air after filtering, washing, drying, obtains Au-T
Catalyst (T represents the temperature of roasting).
8. Au/ α-Fe described in a kind of claim 62O3Catalyst is used in the reaction of carbon monoxide Oxidation at room temperature.
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Cited By (4)
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| CN108389726A (en) * | 2018-02-11 | 2018-08-10 | 国家纳米科学中心 | A kind of alpha-ferric oxide nanometer stick array of carbon film coated and its preparation method and application |
| CN108538632A (en) * | 2018-04-18 | 2018-09-14 | 中南大学 | A kind of FeOOH electrode and its preparation method and application |
| CN109731582A (en) * | 2019-02-21 | 2019-05-10 | 北京工业大学 | A kind of AuMnO of efficiently catalyzing and oxidizing benzenex/ mesoporous Fe2O3The preparation of catalyst |
| CN110339844A (en) * | 2018-04-08 | 2019-10-18 | 中国科学院大连化学物理研究所 | Fe nanometer rods and Pt@Fe Nanorods Catalyst and synthesis and application |
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| CN101204655A (en) * | 2006-12-21 | 2008-06-25 | 中国人民解放军63971部队 | Process for preparing nanometer gold catalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108389726A (en) * | 2018-02-11 | 2018-08-10 | 国家纳米科学中心 | A kind of alpha-ferric oxide nanometer stick array of carbon film coated and its preparation method and application |
| CN110339844A (en) * | 2018-04-08 | 2019-10-18 | 中国科学院大连化学物理研究所 | Fe nanometer rods and Pt@Fe Nanorods Catalyst and synthesis and application |
| CN110339844B (en) * | 2018-04-08 | 2021-08-17 | 中国科学院大连化学物理研究所 | Fe nanorod and Pt @ Fe nanorod catalyst as well as synthesis and application thereof |
| CN108538632A (en) * | 2018-04-18 | 2018-09-14 | 中南大学 | A kind of FeOOH electrode and its preparation method and application |
| CN109731582A (en) * | 2019-02-21 | 2019-05-10 | 北京工业大学 | A kind of AuMnO of efficiently catalyzing and oxidizing benzenex/ mesoporous Fe2O3The preparation of catalyst |
| CN109731582B (en) * | 2019-02-21 | 2022-07-19 | 北京工业大学 | AuMnO for efficiently catalyzing and oxidizing benzenexMesoporous Fe2O3Preparation of the catalyst |
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