CN106423169A - Mesoporous Ti-Fe2O3 photocatalyst and preparation method and application thereof - Google Patents
Mesoporous Ti-Fe2O3 photocatalyst and preparation method and application thereof Download PDFInfo
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims description 46
- 229910011212 Ti—Fe Inorganic materials 0.000 claims description 25
- 239000010936 titanium Substances 0.000 claims description 23
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 238000005286 illumination Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000015556 catabolic process Effects 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 3
- 239000011259 mixed solution Substances 0.000 abstract 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 21
- 238000012360 testing method Methods 0.000 description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 12
- 238000009826 distribution Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000002336 sorption--desorption measurement Methods 0.000 description 5
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001507 sample dispersion Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 101100258233 Caenorhabditis elegans sun-1 gene Proteins 0.000 description 1
- 101100024583 Mus musculus Mtf1 gene Proteins 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 by weight percentage Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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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
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J35/39—Photocatalytic 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a mesoporous Ti-Fe2O3 photocatalyst and a preparation method and application thereof. After ferric nitrate and an ethanol solution containing a surface active agent are stirred and mixed to be uniform, a titaniferous solution is added, after the materials are stirred to be uniform, the pH of the solution is regulated to range from 1 to 2, and a mixed solution is obtained; the mixed solution is added into a hydrothermal still, a hydrothermal reaction is carried out, and Ti-Fe2O3 containing the surface active agent is obtained; after Ti-Fe2O3 containing the surface active agent is dried, Ti-Fe2O3 is placed in a muffle furnace to be calcined, the product is cooled to room temperature, grinding is carried out, and the target product is obtained. According to the mesoporous Ti-Fe2O3 photocatalyst and the preparation method and application thereof, metal ion doping is achieved while the specific surface area is increased, and therefore the aim of enhancing photocatalytic activity is achieved. The preparation method is simple, conditions are mild, very good industrial production prospects are achieved, and the obtained mesoporous Ti-Fe2O3 photocatalyst can degrade isopropanol under irradiation of visible light of 420 nm or above.
Description
Technical field
The invention belongs to catalysis material technical field, it is specifically related to a kind of mesoporous Ti-Fe of Doped with Titanium2O3Photocatalysis
Agent and its preparation method and application.
Background technology
Photocatalysis technology is a kind of environmentally friendly technology, and catalysis material can be obtained using sunshine hydrogen production by water decomposition
Regenerative resource, applies also for the depollution of environment, solves energy and the environmental problem that human development is faced.Iron oxide is (red
Iron ore) it is a kind of metal N-type semiconductor, as the very promising catalysis material of one kind, it can absorb and account for sunshine gross energy
38% all ultraviolet lights and most of visible ray, more because being cheap semi-conducting material and being subject to the extensive pass of people
Note, its energy gap is 2.1eV, all ultraviolet lights of inclusion of absorbable below 600nm and most of visible ray.Iron oxide conduct
A kind of semiconductor light-catalyst, have the advantages that nontoxic, inexpensive, can magnetic force reclaim, it is in environmental pollution degraded, light decomposition water
The fields such as hydrogen manufacturing have wide practical use.But, the absorption coefficient of light of iron oxide is little, the short life of carrier, electronics and sky
Cave easily material internal be combined, diffusion length little (<5nm), conductive capability is weak, and resistivity is high, and Carrier recombination rate is high,
Therefore how to reduce iron oxide photocatalyst Carrier recombination rate becomes an emphasis of people's research.
Content of the invention
In order to solve problem above, it is an object of the invention to provide a kind of one-step synthesis method has the same of bigger serface
When, realize the mesoporous Ti-Fe of metal ion mixing2O3Photochemical catalyst.Two aspect collective effects improve the photocatalytic of iron oxide
Can be so as to have the surface configuration of nano-pore, thus improving the efficiency of catalytic reaction.
The technical solution used in the present invention is：A kind of mesoporous Ti-Fe2O3Photochemical catalyst, described mesoporous Ti-Fe2O3Light is urged
Agent, specific surface area is 57-126m2/ g, aperture is 5-20nm；By weight percentage, Ti:Fe=1-3:100.
A kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, method is as follows：
1), after ferric nitrate and the ethanol solution containing surfactant being uniformly mixed, titaniferous solution, stirring are added
After uniformly, the pH adjusting solution, to 1-2, obtains mixed liquor；
2) mixed liquor is added in water heating kettle, hydro-thermal reaction, obtain the Ti-Fe containing surfactant2O3；
3) by the Ti-Fe containing surfactant2O3After drying, it is placed in Muffle kiln roasting, is cooled to room temperature, grind, obtain
To target product.
Above-mentioned a kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, described surfactant is F127.
Above-mentioned a kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, described titaniferous solution is butyl titanate.
Above-mentioned a kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, by weight percentage, Ti:Fe=1-3:100,
Take ferric nitrate and titanium solution.
Above-mentioned a kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, step 2) in, hydrothermal reaction condition is, hydro-thermal
Temperature is 110-130 DEG C, and the hydro-thermal time is 9-11h.
Above-mentioned a kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, step 3) be, by containing surfactant
Ti-Fe2O3In baking oven, 60-70 DEG C, after 6-7h is dried, it is placed in Muffle furnace, 350-400 DEG C, roasting 1-2 hour, is cooled to
Room temperature, grinds, obtains target product.
Above-mentioned mesoporous Ti-Fe2O3Application in degradation of small molecular organic matter for the photochemical catalyst.Method is as follows：Will be mesoporous
Ti-Fe2O3Photochemical catalyst is placed in the confined space containing small organic molecule, degrades under visible light illumination.
The invention has the advantages that：
1. the present invention, one-step synthesis method, low cost, simple, convenient, can prepare on a large scale.
2. the present invention, the mesoporous material obtaining, even aperture distribution, there is larger specific surface area.
3. the present invention, by surfactant pore-creating, removes surfactant by roasting afterwards, obtains nano-pore knot
Structure, then this structure is passed through to grind the photochemical catalyst of the special appearance that can get powder.This photochemical catalyst has uniqueness
Surface topography, it is possible to increase photocatalysis area, simultaneously titanium doped with beneficial to photo-generate electron-hole to separate, extend photochemical catalyst
Life-span, therefore can strengthen photocatalytic activity.
4. the present invention, preparation method both can avoid, using dangerous chemicals, obtaining metal-doped porous material simultaneously
Material.Obtained titanium doped amount is 3% mesoporous Ti-Fe2O3There is larger specific surface area 57-126m2/ g, aperture is 5-
20nm, the structure of these porous provides more response locations so that (420nm) degraded isopropanol arrives under visible light illumination
The speed of acetone reaches 46.44ppm/min, is 17.39 times of pure iron oxide.
5. the present invention, in order to reduce Fe2O3Carrier recombination rate, so that electron-hole pair is more effectively separated, select to mix
Miscellaneous titanium ion reducing the compound of electron hole pair, to reach efficiently separating of electron hole.Fe can be made by doping2O3Conduction band
Current potential moves down, and band gap narrows, thus widening threshold wave-length, can be in Fe by doping2O3Band gap in produce in new capture
The heart, to realize the capture to light induced electron.Fe can be made by doping2O3Threshold wave-length to visible region red shift, thus improving
Photocatalytic activity.The specific surface area simultaneously improving di-iron trioxide is remarkably improved photocatalysis performance, the urging of bigger serface
Agent can provide more Adsorptions, shortens the diffusion length of photo-generated carrier, thus greatly improving catalytic reaction
Efficiency.
Brief description
Fig. 1 is pure Fe2O3, the XRD of MTF-1, MTF-3.
Fig. 2 is pure Fe2O3The SEM figure of photochemical catalyst.
The pure Fe of Fig. 32O3The nitrogen adsorption desorption isotherm of photochemical catalyst and corresponding graph of pore diameter distribution
Fig. 4 is the Ti-Fe that the titanium doped amount that in embodiment 1, step 3 obtains is 1%2O3The SEM figure of photochemical catalyst.
Fig. 5 a is that the XPS of Fe in the MTF-1 photochemical catalyst that in embodiment 1, step 3 obtains finely composes.
Fig. 5 b is that the XPS of Ti in the MTF-1 photochemical catalyst that in embodiment 1, step 3 obtains finely composes.
Fig. 6 is that the XPS of the MTF-1 photochemical catalyst that step 3 obtains in embodiment 1 composes entirely
Fig. 7 is the nitrogen adsorption desorption isotherm of MTF-1 photochemical catalyst and corresponding hole that in embodiment 1, step 3 obtains
Footpath distribution map.
Fig. 8 is the Ti-Fe that the titanium doped amount that in embodiment 2, step 3 obtains is 3%2O3The SEM figure of photochemical catalyst.
Fig. 9 a is that the XPS of Fe in the MTF-3 photochemical catalyst that in embodiment 2, step 3 obtains finely composes.
Fig. 9 b is that the XPS of Ti in the MTF-3 photochemical catalyst that in embodiment 2, step 3 obtains finely composes.
Figure 10 is that the XPS of the MTF-3 photochemical catalyst that step 3 obtains in embodiment 2 composes entirely.
Figure 11 is the nitrogen adsorption desorption isotherm of MTF-3 photochemical catalyst and corresponding hole that in embodiment 2, step 3 obtains
Footpath distribution map.
Figure 12 is pure Fe2O3, the degraded photochemical catalyst of MTF-1, MTF-3 degrades the activity of isopropanol under visible light illumination
Contrast schematic diagram.
Specific embodiment
Pure Fe2O3Preparation：
The nine water ferric nitrates of 4.04g are dissolved in 20ml ethanol, ultrasonically treated 1h, solution is put in water heating kettle, 120 DEG C
Under the conditions of hydro-thermal 10h, obtain final product pure Fe2O3.
By the pure Fe preparing2O3Carry out XRD test, result as shown in figure 1, as seen from Figure 1, with di-iron trioxide
Standard diffraction peak is consistent.
By the pure Fe preparing2O3Carry out SEM test, result is as shown in Fig. 2 from Figure 2 it can be seen that pure Fe2O3It is shown as scattered
The spheric granules of shape.
By the pure Fe preparing2O3Carry out nitrogen adsorption desorption test, result is as shown in figure 3, as seen from Figure 3, pure
Fe2O3Specific surface area be 19.814m2/ g, is substantially not present hole in terms of graph of pore diameter distribution.
A kind of mesoporous Ti-Fe of embodiment 12O3Photochemical catalyst (MTF-1)
(1) preparation method is as follows：
1) 1g F127 and 20ml absolute ethyl alcohol are mixed, after ultrasonic disperse 1h, add 4.04gFe (NO3)3·9H2O, surpasses
After sound dispersion 1h, then it is added thereto to 0.034g butyl titanate (by weight percentage, Ti:Fe=1:100), stirring mixing is equal
Even, drip nitric acid, adjust pH to 1-2, stir to transparent, obtain mixed liquor.
2) mixed liquor is added in water heating kettle, at 120 DEG C, hydro-thermal reaction 10h, obtain the Ti-Fe containing F1272O3.
3) by the Ti-Fe containing F1272O3In an oven, at 60-70 DEG C, after drying 6h, it is placed in Muffle furnace, in 380
At DEG C, roasting 2h, it is cooled to room temperature, grind, the doping obtaining titanium is 1% mesoporous Ti-Fe2O3Photochemical catalyst, is designated as MTF-
1.
(2) testing result
By step 3) MTF-1 for preparing carries out XRD test, test result as shown in figure 1, as seen from Figure 1, the sample of preparation
It is typical Fe2O3Diffraction maximum, with prepared pure Fe2O3Diffraction maximum similar.
By step 3) MTF-1 for preparing carries out SEM test, and result is as shown in figure 4, from fig. 4, it can be seen that prepared sample is
It is made up of scattered spherical little particle, illustrate that the sample dispersion prepared is good.
By step 3) MTF-1 for preparing carries out XPS test, the fine spectrum result of Ti, Fe as shown in figure 5 a and 5b, Quan Pu
As shown in fig. 6, the peak seeing titanium that can be apparent from complete composing it was demonstrated that Ti be entrained in di-iron trioxide lattice in.
By step 3) MTF-1 for preparing carries out nitrogen adsorption desorption test, result as shown in fig. 7, as seen from Figure 7, display
Hysteresis loop, illustrates Ti-Fe2O3There is loose structure, pore-size distribution is shown as 5-28nm, the porous that test result display obtains
Ti-Fe2O3There is 44.361m2The specific surface area of/g.
(3) apply
By mesoporous Ti-Fe manufactured in the present embodiment2O3Photochemical catalyst (MTF-1) carries out photocatalytic degradation isopropanol experiment.
Test process is：With 300W xenon lamp as light source, respectively by the mesoporous Ti-Fe of 0.1g photochemical catalyst of above-mentioned preparation2O3
(MTF-1), the pure Fe of preparation2O3It is put in 4cm2In glass guide channel, the glass guide channel of photocatalyst-bearing is put into and includes an atmospheric pressure
In the 300ml reactor of air, in the most backward reactor, inject 5ul isopropanol liquid, standing makes system adsorption-desorption in 3 hours
Balance, isopropanol of then degrading under visible light illumination.
As shown in figure 12, in Figure 12, rectangular length represents the speed that acetone produces under visible light illumination to result, by
Figure 12 understands, the MTF-1 of preparation shows good photocatalytic activity, reaches 13.27ppm/min, and the pure Fe preparing2O3Only
Reach 2.67ppm/min.
A kind of mesoporous Ti-Fe of embodiment 22O3Photochemical catalyst (MTF-3)
(1) preparation method is as follows：
1) 1g F127 and 20ml absolute ethyl alcohol are mixed, after ultrasonic disperse 1h, add 4.04gFe (NO3)3·9H2O, surpasses
After sound dispersion 1h, then it is added thereto to 0.102g butyl titanate (by weight percentage, Ti:Fe=3:100), stirring mixing is equal
Even, drip nitric acid, adjust pH to 1-2, stir to transparent, obtain mixed liquor.
2) mixed liquor is added in water heating kettle, at 120 DEG C, hydro-thermal reaction 10h, obtain the Ti-Fe containing F1272O3.
3) by the Ti-Fe containing F1272O3In an oven, at 60-70 DEG C, after drying 6h, it is placed in Muffle furnace, in 380
At DEG C, roasting 2h, it is cooled to room temperature, grind, the doping obtaining titanium is 3% mesoporous Ti-Fe2O3Photochemical catalyst, is designated as MTF-
3.
(2) testing result
By step 3) MTF-3 for preparing carries out XRD test, and test result is as shown in figure 1, as can be seen from the figure prepare
Sample is typical Fe2O3Diffraction maximum, with prepared pure Fe2O3Diffraction maximum similar.
By step 3) MTF-3 for preparing carries out SEM test, and as shown in figure 8, as seen from Figure 8, prepared sample is result
It is made up of scattered spherical little particle, illustrate that the sample dispersion prepared is good.
By step 3) MTF-3 for preparing carries out XPS test, the fine spectrum result of Ti, Fe as shown in figures 9 a and 9b, Quan Pu
As shown in Figure 10, the peak seeing titanium that can be apparent from complete composing it was demonstrated that Ti be entrained in di-iron trioxide lattice in.
By step 3) MTF-3 for preparing carries out nitrogen adsorption desorption test, and as shown in figure 11, in figure shows delayed result
Ring, illustrates Ti-Fe2O3There is loose structure, pore-size distribution is shown as 5-18nm, the Ti- of the porous that test result display obtains
Fe2O3There is 57.340m2The specific surface area of/g.
(3) apply
By mesoporous Ti-Fe manufactured in the present embodiment2O3Photochemical catalyst (MTF-3) carries out photocatalytic degradation isopropanol experiment.
Test process is：With 300W xenon lamp as light source, respectively by the mesoporous Ti-Fe of 0.1g photochemical catalyst of above-mentioned preparation2O3
(MTF-3), the pure Fe of preparation2O3It is put in 4cm2In glass guide channel, the glass guide channel of photocatalyst-bearing is put into and includes an atmospheric pressure
In the 300ml reactor of air, in the most backward reactor, inject 5ul isopropanol liquid, standing makes system adsorption-desorption in 3 hours
Balance, isopropanol of then degrading under visible light illumination.
As shown in figure 12, the rectangular length of in figure represents the speed that acetone produces under visible light illumination, as seen from the figure
The MTF-3 of preparation shows good photocatalytic activity, reaches 46.44ppm/min, and the pure Fe preparing2O3Only reach 2.67ppm/
min.
Claims (10)
1. a kind of mesoporous Ti-Fe2O3Photochemical catalyst is it is characterised in that described mesoporous Ti-Fe2O3Photochemical catalyst, specific surface area is
40-126m2/ g, aperture is 5-20nm；By weight percentage, Ti:Fe=1-3:100.
2. a kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst is it is characterised in that method is as follows：
1), after ferric nitrate and the ethanol solution containing surfactant being uniformly mixed, add titaniferous solution, stir
Afterwards, adjust the pH of solution to 1-2, obtain mixed liquor；
2) mixed liquor is added in water heating kettle, hydro-thermal reaction, obtain the Ti-Fe containing surfactant2O3；
3) by the Ti-Fe containing surfactant2O3After drying, it is placed in Muffle kiln roasting, is cooled to room temperature, grind, obtain mesh
Mark product.
3. a kind of mesoporous Ti-Fe according to claim 22O3The preparation method of photochemical catalyst is it is characterised in that described
Surfactant is F127.
4. a kind of mesoporous Ti-Fe according to claim 22O3The preparation method of photochemical catalyst is it is characterised in that described
Titaniferous solution is butyl titanate.
5. a kind of mesoporous Ti-Fe according to claim 22O3The preparation method of photochemical catalyst is it is characterised in that by weight
Percentage, Ti:Fe=1-3:100, take ferric nitrate and titanium solution.
6. a kind of mesoporous Ti-Fe according to claim 22O3The preparation method of photochemical catalyst is it is characterised in that step 2)
In, hydrothermal reaction condition is that hydrothermal temperature is 110-130 DEG C, and the hydro-thermal time is 9-11h.
7. a kind of mesoporous Ti-Fe according to claim 22O3The preparation method of photochemical catalyst is it is characterised in that step 3)
For by the Ti-Fe containing surfactant2O3In baking oven, 60-70 DEG C, after 6-7h is dried, it is placed in Muffle furnace, 350-400
DEG C, roasting 1-2 hour, it is cooled to room temperature, grind, obtain target product.
8. the mesoporous Ti-Fe described in claim 12O3Application in degradation of small molecular organic matter for the photochemical catalyst.
9. application according to claim 8 is it is characterised in that method is as follows：By mesoporous Ti-Fe2O3Photochemical catalyst is placed on and contains
Have in the confined space of small organic molecule, degrade under visible light illumination.
10. the application described in claim 8 or 9 is it is characterised in that described small organic molecule is isopropanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610895032.1A CN106423169B (en) | 2016-10-13 | 2016-10-13 | A kind of mesoporous Ti-Fe2O3Photochemical catalyst and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610895032.1A CN106423169B (en) | 2016-10-13 | 2016-10-13 | A kind of mesoporous Ti-Fe2O3Photochemical catalyst and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106423169A true CN106423169A (en) | 2017-02-22 |
| CN106423169B CN106423169B (en) | 2019-11-29 |
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| CN113398930A (en) * | 2021-05-27 | 2021-09-17 | 华北电力大学科技学院 | Nano iron oxide photocatalyst and preparation method thereof |
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| CN113398930A (en) * | 2021-05-27 | 2021-09-17 | 华北电力大学科技学院 | Nano iron oxide photocatalyst and preparation method thereof |
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