CN106423169B - A kind of mesoporous Ti-Fe2O3Photochemical catalyst and its preparation method and application - Google Patents
A kind of mesoporous Ti-Fe2O3Photochemical catalyst and its preparation method and application Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910011212 Ti—Fe Inorganic materials 0.000 claims abstract description 24
- 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 11
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 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
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction 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
- 238000003756 stirring Methods 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000005855 radiation Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 23
- 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
- 239000000463 material Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 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
- 238000001228 spectrum Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 3
- 239000011941 photocatalyst Substances 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding 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
- 238000001507 sample dispersion 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
- -1 by weight percentage Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000004064 recycling Methods 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 present invention discloses a kind of mesoporous Ti-Fe2O3Photochemical catalyst and its preparation method and application.After ferric nitrate and the ethanol solution containing surfactant are uniformly mixed, titaniferous solution is added and adjusts the pH to 1-2 of solution after mixing evenly, obtains mixed liquor；Mixed liquor is added in water heating kettle, hydro-thermal reaction obtains the Ti-Fe containing surfactant2O3；By the Ti-Fe containing surfactant2O3After drying, it is placed in Muffle kiln roasting, is cooled to room temperature, ground, obtain target product.The present invention realizes metal ion mixing while increasing specific surface area, to achieve the purpose that enhance photocatalytic activity.Preparation method of the present invention is simple, mild condition, there is good industrial production prospect, the photochemical catalyst of mesoporous metal doping obtained degradable isopropanol under the radiation of visible light of 420nm or more.
Description
Technical field
The invention belongs to catalysis material technical fields, are specifically related to a kind of mesoporous Ti-Fe of Doped with Titanium2O3Photocatalysis
Agent and its preparation method and application.
Background technique
Photocatalysis technology is a kind of environmentally friendly technology, and catalysis material can be obtained using sunlight hydrogen production by water decomposition
Renewable energy applies also for the depollution of environment, solves energy and environmental problem that human development is faced.Iron oxide is (red
Iron ore) it is a kind of metal N-type semiconductor, it is absorbable to account for sunshine gross energy as a kind of very promising catalysis material
38% all ultraviolet lights and most of visible light, more because being cheap semiconductor material and the extensive pass by people
Note, forbidden bandwidth 2.1eV, it includes all ultraviolet lights and most of visible light that it is below, which to can absorb 600nm,.Iron oxide conduct
A kind of semiconductor light-catalyst, have the advantages that it is nontoxic, inexpensive, can magnetic force recycling, in environmental pollution degradation, photodegradation water
The fields such as hydrogen manufacturing have wide practical use.But the absorption coefficient of light of iron oxide is small, the service life of carrier is short, electronics and sky
Cave is easy compound in material internal, and diffusion length is small (< 5nm), and 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.
Summary of the invention
In order to solve problem above, the object of the present invention is to provide a kind of one-step synthesis methods to have the same of bigger serface
When, realize the mesoporous Ti-Fe of metal ion mixing2O3Photochemical catalyst.The photocatalytic of two aspect collective effects improvement iron oxide
Can, the surface shape of nano-pore is made it have, to improve the efficiency of catalysis reaction.
A kind of the technical solution adopted by the present invention are as follows: mesoporous Ti-Fe2O3Photochemical catalyst, the mesoporous Ti-Fe2O3Light is urged
Agent, specific surface area 57-126m2/ g, aperture 5-20nm；By weight percentage, Ti:Fe=1-3:100.
A kind of mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, the method is as follows:
1) after being uniformly mixed ferric nitrate and the ethanol solution containing surfactant, titaniferous solution, stirring is added
After uniformly, the pH to 1-2 of solution is adjusted, mixed liquor is obtained；
2) mixed liquor is added in water heating kettle, hydro-thermal reaction obtains 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, ground, obtain
To target product.
A kind of above-mentioned mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, the surfactant are F127.
A kind of above-mentioned mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, the titaniferous solution are butyl titanate.
A kind of above-mentioned mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, by weight percentage, Ti:Fe=1-3:100,
Take ferric nitrate and titanium solution.
A kind of above-mentioned mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, in step 2), hydrothermal reaction condition is hydro-thermal
Temperature is 110-130 DEG C, and the hydro-thermal time is 9-11h.
A kind of above-mentioned mesoporous Ti-Fe2O3The preparation method of photochemical catalyst, step 3) are that will contain surfactant
Ti- Fe2O3In baking oven, 60-70 DEG C, after drying 6-7h, it is placed in Muffle furnace, 350-400 DEG C, roasts 1-2 hours, be cooled to
Room temperature, grinding, obtains target product.
Above-mentioned mesoporous Ti-Fe2O3Application of the photochemical catalyst in degradation of small molecular organic matter.Method is as follows: will be mesoporous
Ti- Fe2O3Photochemical catalyst is placed in the confined space containing small organic molecule, is degraded under visible light illumination.
The invention has the following advantages:
1. the present invention, one-step synthesis method is at low cost, simple, convenient, can be prepared on a large scale.
2. the present invention, obtained mesoporous material, even aperture distribution have biggish specific surface area.
3. the present invention removes surfactant by roasting later, obtains nano-pore knot by surfactant pore-creating
Structure, then this structure is passed through into grinding, the photochemical catalyst of powdered special appearance can be obtained.The photochemical catalyst has unique
Surface topography, can be improved photocatalysis area, while titanium is separated doped with being conducive to photo-generate electron-hole pairs, extends photochemical catalyst
Service life, therefore photocatalytic activity can be enhanced.
4. the present invention, preparation method both be can avoid using dangerous chemicals, while obtain metal-doped porous material
Material.The mesoporous Ti-Fe that obtained titanium doped amount is 3%2O3With biggish specific surface area 57-126m2/ g, aperture 5-
20nm, these porous structures provide more response locations, so that (420nm) degradation isopropanol arrives under visible light illumination
The rate 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, separate electron-hole pair more effectively, selection is mixed
Miscellaneous titanium ion reduces the compound of electron hole pair, to reach efficiently separating for electron hole.It can make Fe by doping2O3Conduction band
Current potential moves down, and band gap narrows, so that threshold wave-length is widened, it can be in Fe by doping2O3Band gap in generate in new capture
The heart, to realize the capture to light induced electron.It can make Fe by doping2O3Threshold wave-length to visible region red shift, to improve
Photocatalytic activity.The specific surface area for improving di-iron trioxide simultaneously is remarkably improved photocatalysis performance, and bigger serface is urged
Agent can provide more Adsorptions, shorten the diffusion length of photo-generated carrier, to greatly improve catalysis reaction
Efficiency.
Detailed description of the invention
Fig. 1 is pure Fe2O3, MTF-1, MTF-3 XRD diagram.
Fig. 2 is pure Fe2O3The SEM of photochemical catalyst schemes.
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 step 3 obtains in embodiment 1 is 1%2O3The SEM of photochemical catalyst schemes.
The XPS of Fe is finely composed in the MTF-1 photochemical catalyst that Fig. 5 a obtains for step 3 in embodiment 1.
The XPS of Ti is finely composed in the MTF-1 photochemical catalyst that Fig. 5 b obtains for step 3 in embodiment 1.
Fig. 6 is that the XPS for the MTF-1 photochemical catalyst that step 3 obtains in embodiment 1 is composed entirely
The nitrogen adsorption desorption isotherm for the MTF-1 photochemical catalyst that Fig. 7 obtains for step 3 in embodiment 1 and corresponding hole
Diameter distribution map.
Fig. 8 is the Ti-Fe that the titanium doped amount that step 3 obtains in embodiment 2 is 3%2O3The SEM of photochemical catalyst schemes.
The XPS of Fe is finely composed in the MTF-3 photochemical catalyst that Fig. 9 a obtains for step 3 in embodiment 2.
The XPS of Ti is finely composed in the MTF-3 photochemical catalyst that Fig. 9 b obtains for step 3 in embodiment 2.
Figure 10 is that the XPS for the MTF-3 photochemical catalyst that step 3 obtains in embodiment 2 is composed entirely.
The nitrogen adsorption desorption isotherm for the MTF-3 photochemical catalyst that Figure 11 obtains for step 3 in embodiment 2 and corresponding hole
Diameter distribution map.
Figure 12 is pure Fe2O3, MTF-1, MTF-3 degradation photochemical catalyst degrade under visible light illumination the activity of isopropanol
Contrast schematic diagram.
Specific embodiment
Pure Fe2O3Preparation:
The nine water ferric nitrates of 4.04g are dissolved in 20ml ethyl alcohol, 1h is ultrasonically treated, solution is put into water heating kettle, 120 DEG C
Under the conditions of hydro-thermal 10h to get pure Fe2O3。
The pure Fe that will be prepared2O3XRD test is carried out, as a result as shown in Figure 1, as seen from Figure 1, with di-iron trioxide
Standard diffraction peak is consistent.
The pure Fe that will be prepared2O3SEM test is carried out, as a result as shown in Fig. 2, from Figure 2 it can be seen that pure Fe2O3It is shown as scattered
The spheric granules of shape.
The pure Fe that will be prepared2O3Nitrogen adsorption desorption test is carried out, it is pure as a result as shown in figure 3, as seen from Figure 3
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) the preparation method is as follows:
1) 1g F127 and 20ml dehydrated alcohol is mixed, after ultrasonic disperse 1h, 4.04gFe (NO is added3)3·9H2O surpasses
After sound disperses 1h, then 0.034g butyl titanate (by weight percentage, Ti:Fe=1:100) is added thereto, is stirred
It is even, nitric acid is added dropwise, adjusts pH to 1-2, stirring obtains mixed liquor to transparent.
2) mixed liquor is added in water heating kettle, at 120 DEG C, hydro-thermal reaction 10h obtains the Ti-Fe containing F1272O3。
3) by the Ti-Fe containing F1272O3In an oven, it at 60-70 DEG C, after drying 6h, is placed in Muffle furnace, in 380
At DEG C, 2h is roasted, is cooled to room temperature, ground, obtains the mesoporous Ti-Fe that the doping of titanium is 1%2O3Photochemical catalyst is denoted as MTF-
1。
(2) testing result
The MTF-1 of step 3) preparation is subjected to XRD test, test results are shown in figure 1, as seen from Figure 1, the sample of preparation
It is typical Fe2O3Diffraction maximum, with pure Fe obtained2O3Diffraction maximum it is similar.
The MTF-1 of step 3) preparation is subjected to SEM test, as a result as shown in figure 4, from fig. 4, it can be seen that prepared sample is
It is made of the spherical little particle dispersed, illustrates that the sample dispersion of preparation is good.
By step 3) preparation MTF-1 carry 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, can see clearly that the peak of titanium from full spectrum, it was demonstrated that Ti is entrained in the lattice of di-iron trioxide.
The MTF-1 of step 3) preparation is subjected to nitrogen adsorption desorption test, as a result as shown in fig. 7, as seen from Figure 7, showing
Hysteresis loop illustrates Ti-Fe2O3With porous structure, pore-size distribution is shown as 5-28nm, and test result display obtains porous
Ti- Fe2O3With 44.361m2The specific surface area of/g.
(3) it applies
By mesoporous Ti-Fe manufactured in the present embodiment2O3Photochemical catalyst (MTF-1) carries out the experiment of photocatalytic degradation isopropanol.
Test process are as follows: using 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 prepared2O3It 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, 5ul isopropanol liquid is finally injected into reactor, standing 3 hours makes system adsorption-desorption
Balance, isopropanol of then degrading under visible light illumination.
As a result as shown in figure 12, the rectangular length expression rate that acetone generates under visible light illumination in Figure 12, by
Figure 12 is it is found that the MTF-1 of preparation shows good photocatalytic activity, the pure Fe for reaching 13.27ppm/min, and preparing2O3Only
Up to 2.67ppm/min.
A kind of mesoporous Ti-Fe of embodiment 22O3Photochemical catalyst (MTF-3)
(1) the preparation method is as follows:
1) 1g F127 and 20ml dehydrated alcohol is mixed, after ultrasonic disperse 1h, 4.04gFe (NO is added3)3·9H2O surpasses
After sound disperses 1h, then 0.102g butyl titanate (by weight percentage, Ti:Fe=3:100) is added thereto, is stirred
It is even, nitric acid is added dropwise, adjusts pH to 1-2, stirring obtains mixed liquor to transparent.
2) mixed liquor is added in water heating kettle, at 120 DEG C, hydro-thermal reaction 10h obtains the Ti-Fe containing F1272O3。
3) by the Ti-Fe containing F1272O3In an oven, it at 60-70 DEG C, after drying 6h, is placed in Muffle furnace, in 380
At DEG C, 2h is roasted, is cooled to room temperature, ground, obtains the mesoporous Ti-Fe that the doping of titanium is 3%2O3Photochemical catalyst is denoted as MTF-
3。
(2) testing result
The MTF-3 of step 3) preparation is subjected to XRD test, test results are shown in figure 1, as can be seen from the figure prepares
Sample is typical Fe2O3Diffraction maximum, with pure Fe obtained2O3Diffraction maximum it is similar.
The MTF-3 of step 3) preparation is subjected to SEM test, as a result as shown in figure 8, as seen from Figure 8, prepared sample is
It is made of the spherical little particle dispersed, illustrates that the sample dispersion of preparation is good.
By step 3) preparation MTF-3 carry 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, it can see clearly that the peak of titanium from full spectrum, it was demonstrated that Ti is entrained in the lattice of di-iron trioxide.
The MTF-3 of step 3) preparation is subjected to nitrogen adsorption desorption test, as a result as shown in figure 11, in figure shows lag
Ring illustrates Ti-Fe2O3With porous structure, pore-size distribution is shown as 5-18nm, the porous Ti- that test result display obtains
Fe2O3With 57.340m2The specific surface area of/g.
(3) it applies
By mesoporous Ti-Fe manufactured in the present embodiment2O3Photochemical catalyst (MTF-3) carries out the experiment of photocatalytic degradation isopropanol.
Test process are as follows: using 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 prepared2O3It 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, 5ul isopropanol liquid is finally injected into reactor, standing 3 hours makes system adsorption-desorption
Balance, isopropanol of then degrading under visible light illumination.
As shown in figure 12, the rectangular length expression rate that acetone generates under visible light illumination in figure, as seen from the figure
The MTF-3 of preparation shows good photocatalytic activity, reaches 46.44ppm/min, and the pure Fe prepared2O3Only reach 2.67ppm
/min。
Claims (6)
1. a kind of mesoporous Ti-Fe2O3Application of the photochemical catalyst in degradation of small molecular organic matter, which is characterized in that by mesoporous Ti-
Fe2O3Photochemical catalyst is placed in the confined space containing isopropanol, is degraded under visible light illumination,
The mesoporous Ti-Fe2O3The preparation method of photochemical catalyst includes the following steps:
1) after being uniformly mixed ferric nitrate and the ethanol solution containing surfactant, titaniferous solution is added, stirs evenly
Afterwards, the pH to 1-2 for adjusting solution, obtains mixed liquor；
2) mixed liquor is added in water heating kettle, hydro-thermal reaction obtains 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, ground, obtain mesh
Mark product；
The mesoporous Ti-Fe2O3Photochemical catalyst, specific surface area 40-126m2/ g, aperture 5-20nm；By weight percentage,
Ti:Fe=1-3:100.
2. application according to claim 1, which is characterized in that the surfactant is F127.
3. application according to claim 1, which is characterized in that the titaniferous solution is butyl titanate.
4. application according to claim 1, which is characterized in that by weight percentage, Ti:Fe=1-3:100 takes ferric nitrate
And titanium solution.
5. application according to claim 1, which is characterized in that in step 2), hydrothermal reaction condition is that hydrothermal temperature is
110-130 DEG C, the hydro-thermal time is 9-11h.
6. application according to claim 1, which is characterized in that step 3) is, by the Ti-Fe containing surfactant2O3In
In baking oven, 60-70 DEG C, after drying 6-7h, it is placed in Muffle furnace, 350-400 DEG C, roasts 1-2 hours, be cooled to room temperature, grind,
Obtain target product.
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| CN103173828A (en) * | 2013-03-20 | 2013-06-26 | 浙江大学 | Method for improving electro-catalytic property by depositing Fe3O4 on surface of titanium doped nanocrystalline iron oxide thin film |
| CN103184443A (en) * | 2013-03-21 | 2013-07-03 | 浙江大学 | Electrochemical method for improving photoelectric property of nano iron oxide film |
| CN105498773A (en) * | 2014-09-26 | 2016-04-20 | 中国科学院大连化学物理研究所 | Preparation method for doped iron oxide nanorod catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103173828A (en) * | 2013-03-20 | 2013-06-26 | 浙江大学 | Method for improving electro-catalytic property by depositing Fe3O4 on surface of titanium doped nanocrystalline iron oxide thin film |
| CN103184443A (en) * | 2013-03-21 | 2013-07-03 | 浙江大学 | Electrochemical method for improving photoelectric property of nano iron oxide film |
| CN105498773A (en) * | 2014-09-26 | 2016-04-20 | 中国科学院大连化学物理研究所 | Preparation method for doped iron oxide nanorod catalyst |
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| Fe2O3/carbon quantum dots complex photocatalysts and their enhanced photocatalytic activity under visible light;Hengchao Zhang et al;《Dalton Transactions》;20111231;第40卷;10822-10825 * |
| Sol–gel synthesis of mesoporous mixed Fe2O3/TiO2 photocatalyst:Application for degradation of 4-chlorophenol;B. Palanisamya et al;《Journal of Hazardous Materials》;20130307;233-242 * |
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