CN103638916A - Bound single electron oxygen vacancy-containing titanium dioxide/carbon composite visible-light-induced photocatalyst and preparation method thereof - Google Patents
Bound single electron oxygen vacancy-containing titanium dioxide/carbon composite visible-light-induced photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of visible-light-induced photocatalysts and relates to a bound single electron oxygen vacancy-containing titanium dioxide/carbon composite visible-light-induced photocatalyst and a preparation method thereof. Through drying, grinding, heating and calcination, the bound single electron oxygen vacancy-containing titanium dioxide/carbon composite visible-light-induced photocatalyst is prepared from titanium dioxide sol. The bound single electron oxygen vacancy-containing titanium dioxide/carbon composite visible-light-induced photocatalyst has obvious visible light catalytic effects and has relatively centralized pore size distribution. The preparation method adopts cheap and easily available raw materials and has a low production cost.
Description
technical field
The invention belongs to visible light catalyst technical field, be specifically related to a kind of titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room and preparation method thereof.
background technology
Environment and energy problem has become the challenging problem of tool of current and following facing mankind.Along with the primary energy such as petrochemical industry day by day lack and by it, brought as problems such as environmental pollution, climate warmings, the development and utilization of new forms of energy and the improvement of environment have been subjected to increasing attention.Photocatalysis is the new technology growing up nearly decades, at the aspects such as fixing and organic mineralising of hydrogen production by water decomposition, carbon dioxide, has good application prospect.At present, there have been more ripe technology and product for indoor air purification, antibacterial, the glass automatically cleaning of pottery etc.Yet, as everyone knows, arrive the sunshine medium ultraviolet light proportion less than 4% of earth surface, therefore, needs based on practical application, photochemical catalyst is had higher requirement, can make full use of excited by visible light photochemical catalyst and efficiently electronics and hole are transferred to reaction active site participation redox reaction from conduction band and valence band, for preparing hydrogen, chemical recycling of carbon dioxide and elimination organic pollution etc.
TiO
2it is one of material attracting most attention in numerous photochemical catalysts, be not only the focus of paying close attention in basic research, and be the main photochemical catalyst adopting in actual product, it has high photocatalysis efficiency, Stability Analysis of Structures, the feature such as cheap, nontoxic, is therefore subject to studying of domestic and international scientists extensively.Yet TiO
2a kind ofly to have compared with the semi-conducting material of broad-band gap (band-gap energy is 3.0-3.2 eV), can not be directly by excited by visible light, conventionally adopt the methods such as dye sensitization, transient metal doped and nonmetal doping to make it be applicable to visible region.Dye sensitization is except cost is higher, and under light, heat effect, dyestuff easily decomposes, and long-time stability are lower; Transient metal doped TiO
2not only heat endurance is lower, and foreign atom is to TiO
2the diffusion of lattice can produce electron-hole complex centre, reduces light-catalyzed reaction efficiency; And at TiO
2middle doped with non-metals element (as mixing B, F, N, C, S and I) is significantly improved visible light catalytic efficiency.Except element doping, at TiO
2the oxygen room of introducing constraint single electron in lattice is also a kind of TiO of making
2there is visible light-responded method.
The TiO containing constraint single electron oxygen room of bibliographical information
2the preparation method of visible light catalyst mainly contains two classes: (1) radio frequency plasma is processed TiO
2; (2) at TiO
2in lattice, mix N element, comprising: high-temperature calcination TiCl
4ammonia spirit hydrolysate, with ammonia heat treatment P25 TiO
2with nanotube metatitanic acid etc.But above two class methods have its weak point.Adopting radio frequency plasma to process needs expensive precision equipment, yields poorly, and is not easy to large-scale production.Although can accomplish scale production with ammonia heat treatment titanium dioxide, technological requirement is higher, need to prevent pollution and murder by poisoning that ammonia leakage brings, and ammonia utilization rate is very low, cost is higher.High-temperature calcination TiCl
4the TiO of ammonia spirit hydrolysate gained
2not only contain constraint single electron oxygen room, and contain Ti
3+ion, the latter can become the complex centre of photogenerated charge, reduces the catalytic efficiency of photochemical catalyst.
summary of the invention
The object of the present invention is to provide a kind of preparation method of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room, the titanium dioxide/carbon composite visible light catalyst that simultaneously provides a kind of the method to make.
To achieve these goals, the present invention is by the following technical solutions:
Containing a preparation method who fetters titanium dioxide/carbon composite visible light catalyst in single electron oxygen room, its step is as follows:
(1) TiO 2 sol keeps 1-4h at ambient temperature, then is dried 8-72h at 80-100 ℃, through grinding, obtains titania gel powder;
(2) titania gel powder is heated under inert gas shielding to 300-800 ℃ and keep 1-4h;
(3) then at 300-800 ℃, in air, calcine, calcination time is 1-4h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Described inert gas is nitrogen, argon gas or Krypton etc.
Described TiO 2 sol is made through Hydrolyze method by titanium source compound.
The step of Hydrolyze method is as follows: under stirring, 30mL titanium source compound is added drop-wise in 120mL absolute ethyl alcohol, then adds 10mL acetic acid, add 2.5mL deionized water and 10mL triethylamine after 30min, stir 4h, obtain faint yellow TiO 2 sol.
The alkoxide that described titanium source compound is titanium, the alkoxide of titanium such as butyl titanate, tetraisopropyl titanate, tetraethyl titanate etc.
Titanium dioxide/carbon the composite visible light catalyst containing constraint single electron oxygen room making according to above method.
The application of titanium dioxide/carbon composite visible light catalyst aspect catalytic degradation organic dyestuff containing constraint single electron oxygen room.
The present invention's preparation has the following advantages containing the method for titanium dioxide/carbon composite visible light catalyst in constraint single electron oxygen room:
1) this composite visible light catalyst has the oxygen room of constraint single electron, makes it possess visible light catalytic effect;
2) titanium dioxide/carbon composite visible light catalyst pore-size distribution containing constraint single electron oxygen room that the inventive method makes is relatively concentrated, presents little mesoporous distribution;
3) raw material is cheap and easy to get, and production cost is lower, advantages of nontoxic raw materials, guarantee environment and staff's safety;
4) in preparation process, required temperature is not high, and operation is simple, not high to equipment requirement, and processing ease easily carries out large-scale production.
Titanium dioxide/carbon composite visible light catalyst that the present invention makes has significant visible light photocatalytic degradation effect to organic dyestuff such as methyl orange, methylene blues.
accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room of the present invention, and as can be seen from the figure, described diffraction maximum all belongs to anatase TiO
2crystal structure (JCPDS card number: 73-1764); Because the content of carbon is lower, do not find the diffraction maximum of ownership carbon;
Fig. 2 is the TEM photo of the titanium dioxide/carbon compounded visible light photocatalyst containing constraint single electron oxygen room of the present invention, as can be seen from the figure, and TiO
2the particle diameter of nano particle is less than 20 nm, has numerous apertures between the particle of gathering;
Fig. 3 is titanium dioxide/carbon compounded visible light photocatalyst (3b) and the P25 TiO containing constraint single electron oxygen room of the present invention
2(3a) N
2adsorption/desorption isotherms, pore size distribution curve and BET specific area; P25 TiO
2in the scope of 3-55nm, presenting mesopore-macropore distributes, and the present invention is relatively concentrated containing the pore-size distribution of titanium dioxide/carbon compounded visible light photocatalyst in constraint single electron oxygen room, present little mesoporous distribution (<2.2 nm), in addition, containing the BET specific area (81.0m that fetters titanium dioxide/carbon compounded visible light photocatalyst in single electron oxygen room
2/ g) higher than P25 TiO
2(54.4m
2/ g);
Fig. 4 is titanium dioxide/carbon composite visible light catalyst and the P25 TiO containing constraint single electron oxygen room of the present invention
2eSR collection of illustrative plates, the symmetrical peak at g=2.001 place belong to constraint single electron oxygen room;
Fig. 5 is the XPS collection of illustrative plates of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room of the present invention, Fig. 5 a is C1s spectrum, the peak of center in 288.9eV shows the existence of carbonizable substance, and Fig. 5 b is Ti2p spectrum, and the peak that is centered close to 457.6eV and 464.4eV belongs to Ti
4+, show that this material main component is TiO
2;
Fig. 6 is the thermal analysis curue of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room of the present invention, from thermogravimetric (TG) figure and difference quotient heat minute (DTG) figure, can find out near 600 ℃, there is obvious weightlessness, owing to the aerial oxidational losses of institute's carbonaceous material in material; The mass content that can be calculated carbon by weight loss on TG figure is about 1.5%;
Fig. 7 is titanium dioxide/carbon composite visible light catalyst and the P25 TiO containing constraint single electron oxygen room of the present invention
2uv-visible absorption spectra, as seen from the figure, compare with P25 titanium dioxide, the visible ray that product of the present invention is greater than 400nm to wavelength has obvious absorption, and the obvious red shift of ABSORPTION EDGE, this is owing to the synergy of constraint single electron oxygen room and carbon;
Fig. 8 is titanium dioxide/carbon composite visible light catalyst and the P25 TiO containing constraint single electron oxygen room of the present invention
2to the degradation rate of methyl orange and the graph of a relation of radiation of visible light time, product of the present invention has significant photocatalytic Degradation to methyl orange as seen from the figure.
the specific embodiment
With specific embodiment, technical scheme of the present invention is described below, but protection scope of the present invention is not limited to this:
Embodiment 1:
(1) take butyl titanate as titanium source compound, adopt hydrolytic preparation of titanium dioxide colloidal sol, detailed process is: under stirring, 30mL butyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 1h at ambient temperature, then be dried 24h at 80 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under nitrogen atmosphere protection, is heated to 600 ℃, and keeps 1h at 600 ℃;
(4) then at 500 ℃, in air, calcine, calcination time is 2h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Embodiment 2:
(1) take tetraisopropyl titanate as titanium source compound, adopt Hydrolyze method solution to prepare TiO 2 sol, detailed process is: under stirring, 30mL tetraisopropyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 1h at ambient temperature, then be dried 24h at 80 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under nitrogen atmosphere protection, is heated to 600 ℃, and keeps 1h at 600 ℃;
(4) then at 500 ℃, in air, calcine, calcination time is 2h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Embodiment 3:
(1) take butyl titanate as titanium source compound, adopt hydrolytic preparation of titanium dioxide colloidal sol, detailed process is: under stirring, 30mL butyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 2h at ambient temperature, then be dried 12h at 100 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under nitrogen atmosphere protection, is heated to 600 ℃, and keeps 1h at 600 ℃;
(4) then at 800 ℃, in air, calcine, calcination time is 2h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Embodiment 4:
(1) take butyl titanate as titanium source compound, adopt hydrolytic preparation of titanium dioxide colloidal sol, detailed process is: under stirring, 30mL butyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 1h at ambient temperature, then be dried 24h at 80 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under nitrogen atmosphere protection, is heated to 700 ℃, and keeps 1h at 700 ℃;
(4) then at 300 ℃, in air, calcine, calcination time is 4h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Embodiment 5:
(1) take butyl titanate as titanium source compound, adopt hydrolytic preparation of titanium dioxide colloidal sol, detailed process is: under stirring, 30mL butyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 1h at ambient temperature, then be dried 24h at 80 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under argon gas atmosphere protection, is heated to 600 ℃, and keeps 1h at 600 ℃;
(4) then at 500 ℃, in air, calcine, calcination time is 2h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Embodiment 6:
(1) take butyl titanate as titanium source compound, adopt hydrolytic preparation of titanium dioxide colloidal sol, detailed process is: under stirring, 30mL butyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 1h at ambient temperature, then be dried 72h at 80 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under argon gas atmosphere protection, is heated to 300 ℃, and keeps 1h at 300 ℃;
(4) then at 500 ℃, in air, calcine, calcination time is 1h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
Embodiment 7:
(1) take butyl titanate as titanium source compound, adopt hydrolytic preparation of titanium dioxide colloidal sol, detailed process is: under stirring, 30mL butyl titanate is added drop-wise in 120mL absolute ethyl alcohol, add again 10mL acetic acid, after 30min, add 2.5mL deionized water and 10mL triethylamine, stir 4h, obtain faint yellow TiO 2 sol;
(2) then TiO 2 sol is kept to 4h at ambient temperature, then be dried 24h at 80 ℃, through grinding, obtain titania gel powder;
(3) titania gel powder is placed in to tube furnace, under argon gas atmosphere protection, is heated to 800 ℃, and keeps 1h at 800 ℃;
(4) then at 400 ℃, in air, calcine, calcination time is 3h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
The relevant drawings of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room that the embodiment of the present invention 1 makes as Figure 1-Figure 8.
Wherein in Fig. 8, the experimentation of light-catalyzed reaction and condition are as follows: by the methyl orange of 100 mL (MO) aqueous solution (MO content: 20mg/L) He the 0.1 g titanium dioxide/carbon composite visible light catalyst powder containing constraint single electron oxygen room of the present invention joins in 120 mL reaction bulbs successively, and magnetic agitation mixes.Before light-catalyzed reaction, first under dark state, make photochemical catalyst reach balance to the absorption of methyl orange.Open light source, light source adopts the xenon arc lamp of 150 W, installs the edge filter (λ > 420 nm, Xiao Te glass) of 420 nm between lamp and reaction bulb additional.At regular intervals, use UV-Vis spectrophotometer, adopt 464 nm wavelength, detect the concentration of MO.As a comparison, under similarity condition, adopt the P25 TiO of Degussa company
2for photochemical catalyst carries out same experiment.
Claims (4)
1. containing a preparation method who fetters titanium dioxide/carbon composite visible light catalyst in single electron oxygen room, it is characterized in that, step is as follows:
(1) TiO 2 sol keeps 1-4h at ambient temperature, then is dried 8-72h at 80-100 ℃, through grinding, obtains titania gel powder;
(2) titania gel powder is heated under inert gas shielding to 300-800 ℃ and keep 1-4h;
(3) then at 300-800 ℃, in air, calcine, calcination time is 1-4h, is cooled to room temperature, through grinding the titanium dioxide/carbon composite visible light catalyst obtaining containing constraint single electron oxygen room.
2. the preparation method of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room as claimed in claim 1, is characterized in that, described TiO 2 sol is made through Hydrolyze method by titanium source compound.
3. titanium dioxide/carbon the composite visible light catalyst containing constraint single electron oxygen room making according to claim 1 method.
4. the application of the titanium dioxide/carbon composite visible light catalyst containing constraint single electron oxygen room claimed in claim 3 aspect catalytic degradation organic dyestuff.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104162427A (en) * | 2014-08-12 | 2014-11-26 | 河南大学 | Metal ion-grafted TiO2 high-efficiency photocatalyst containing restriction single electron oxygen vacancy as well as preparation and application thereof |
| CN109985618A (en) * | 2019-05-08 | 2019-07-09 | 陕西科技大学 | A kind of H occupies BiVO4The catalysis material of-OVs, preparation method and applications |
| CN111545184A (en) * | 2020-03-31 | 2020-08-18 | 上海电力大学 | Preparation method of oxygen-enriched vacancy titanium dioxide, product and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104162427A (en) * | 2014-08-12 | 2014-11-26 | 河南大学 | Metal ion-grafted TiO2 high-efficiency photocatalyst containing restriction single electron oxygen vacancy as well as preparation and application thereof |
| CN109985618A (en) * | 2019-05-08 | 2019-07-09 | 陕西科技大学 | A kind of H occupies BiVO4The catalysis material of-OVs, preparation method and applications |
| CN109985618B (en) * | 2019-05-08 | 2022-02-01 | 陕西科技大学 | H occupies BiVO4-OVs photocatalytic material, preparation method and application thereof |
| CN111545184A (en) * | 2020-03-31 | 2020-08-18 | 上海电力大学 | Preparation method of oxygen-enriched vacancy titanium dioxide, product and application thereof |
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Application publication date: 20140319 |