CN101791565B - TiO2@ graphite phase carbon nitride heterojunction composite photocatalyst and preparation method thereof - Google Patents
TiO2@ graphite phase carbon nitride heterojunction composite photocatalyst and preparation method thereof Download PDFInfo
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- CN101791565B CN101791565B CN2010101354293A CN201010135429A CN101791565B CN 101791565 B CN101791565 B CN 101791565B CN 2010101354293 A CN2010101354293 A CN 2010101354293A CN 201010135429 A CN201010135429 A CN 201010135429A CN 101791565 B CN101791565 B CN 101791565B
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Abstract
The invention discloses a TiO2@ graphite phase carbon nitride heterojunction composite photocatalyst and a preparation method thereof. The catalyst has a structure of a core made of TiO2 nanoparticles and a shell made of a graphite phase carbon nitride layer. The preparation method comprises the following steps: a) preparing TiO2 nanoparticles coated by Melem by hydro-thermal reaction; and b), washing, separating, drying and calcining the TiO2 nanoparticles to obtain the TiO2@ graphite phase carbon nitride heterojunction composite photocatalyst. The invention has the advantages that: the method is simple, low in cost and suitable for large-scale industrial production; and the composite photocatalyst has high visible light response activity and stability and can be widely used in fields such as photocatalysis and photoelectric conversion.
Description
Technical field
The present invention relates to a kind of TiO
2Graphite phase carbon nitride heterojunction composite photocatalyst and preparation method thereof belongs to photocatalysis field.
Background technology
Along with the continuous development of global process of industrialization, environmental pollution and energy shortage problem are serious day by day, have become the whole world severe challenge to facing altogether.The solar radiation energy is big, and cleanliness without any pollution is inexhaustible, and what use is not the desirable alternative energy source that international community generally acknowledges.Find monocrystalline TiO from Fujishima in 1972 and Honda
2Electrode photodissociation water and Carey etc. are successfully with TiO
2Be used for since the photocatalytic degradation water organic pollution, the conductor photocatalysis technology receives various countries researcher's common concern rapidly owing to can pure utilization pollution-free and inexhaustible solar energy be combined with environmental protection.In in the past 40 years, the oxide of the metal that photocatalysis technology adopts usually or sulfide are as photochemical catalyst, like TiO
2, ZnO
2Deng, it is bigger usually that it prohibits bandwidth, only can utilize the ultraviolet part of sunlight irradiation, and quantum yield is lower, has hindered the practical application of photocatalysis technology.Recently, Wong and Domen etc. have reported a kind of novel no metal-containing polymer semiconductor light-catalyst-graphite phase carbon nitride (g-C
3N
4) under the visible light effect photodissociation water generate hydrogen and oxygen (Wong Xinchen, Nature Mater., 2009,8:76-80) since; The graphite phase carbon nitride has high visible light response activity owing to prohibit bandwidth less (2.7eV), and oxidisability is stronger; Preparation technology is simple, and is cheap, becomes the new direction (Lyth of photochemical catalyst research rapidly; J.Phys.Chem.C, 2009,113:20148-20151; Li, Langmuir, 2009,25:10397-10401; Li, Langmuir, 2010,26:3894-3901).Yet, Domen and Wong etc. further further investigation graphite phase carbon nitride when visible photodissociation water generates oxygen (Domen, J.Phys.Chem.C, 2009,113:4940-4947), find this catalyst under the effect of photohole, self partly decompose and generate N
2Thereby, cause light-catalyzed reaction unstable.Therefore, improving chemical stability, avoid oxidation Decomposition, is that polymer photochemical catalyst-graphite phase carbon nitride moves towards one of key of practical application.
Summary of the invention
The objective of the invention is deficiency, provide a kind of chemical stability good, novel graphite phase carbon nitride composite photo-catalyst of visible light catalytic function admirable and preparation method thereof to above-mentioned graphite phase carbon nitride existence.
The objective of the invention is to realize: a kind of TiO through following mode
2Graphite phase carbon nitride heterojunction composite photocatalyst, the structure of this composite photo-catalyst is: examine and be TiO
2Nano particle, shell are the graphite phase carbon nitride.
TiO
2The crystal formation of nano particle is anatase or rutile or both mixtures.
A kind of TiO
2The preparation method of graphite phase carbon nitride heterojunction composite photocatalyst, preparation process is following:
A) with TiO
2The hydrosol and cyanamide compounds prepare the TiO that surperficial Miller amine coats through hydro-thermal reaction
2Nano particle;
B) to TiO
2After nano particle washing, separation, the drying, promptly get TiO through calcining
2Graphite phase carbon nitride heterojunction composite photocatalyst.
Said cyanamide compounds is meant the mixture of a kind of of cyanamide, double focusing cyanamide or melamine or several kinds.
Hydrothermal reaction condition is: 100 ℃～400 ℃ of reaction temperatures, reaction time 0.5h～50h.
Calcining heat is 300 ℃～1000 ℃, and calcination time is 0.5～10 hour; Be preferably: 400 ℃～800 ℃, calcination time is 1～5 hour.
Calcination atmosphere can be any of air, nitrogen or argon gas.
The present invention has following beneficial effect, and method of the present invention is adopted in (1), can effectively avoid graphite phase carbon nitride self to decompose, and improves chemical stability; (2) through being that the contrast photocatalysis experiment of analogies shows with the parachlorophenol; The graphite phase carbon nitride that composite photo-catalyst of the present invention is purer has higher visible light catalysis activity; Explain that composite photo-catalyst helps the separation of charge of photo-generated carrier, improve quantum yield; (3) preparation technology of the present invention is simple, and the raw material that is adopted is the industrial chemicals of industrial-scale production and cheap, and the composite photo-catalyst cost that therefore adopts method of the present invention to be prepared from is low, and suitable large-scale industrial production.
Fig. 1 is TiO of the present invention
2Graphite phase carbon nitride heterojunction composite photocatalyst structural representation;
Fig. 2 is TiO of the present invention
2The catalytic mechanism sketch map of graphite phase carbon nitride heterojunction composite photocatalyst;
Fig. 3 is TiO of the present invention
2Graphite phase carbon nitride heterojunction composite photocatalyst prepares the process sketch map;
Fig. 4 is the X-ray diffractogram of the embodiment of the invention 1
Fig. 5 is the transmission electron microscope picture of the embodiment of the invention 1;
Fig. 6 is the high-resolution-ration transmission electric-lens figure of the embodiment of the invention 1;
Fig. 7 is the X-ray diffractogram of the embodiment of the invention 2;
Fig. 8 is the high-resolution-ration transmission electric-lens figure of the embodiment of the invention 2
Fig. 9 is the ultraviolet-visible of the embodiment of the invention 2 spectrogram that diffuses;
Figure 10 is the visible light photocatalytic degradation 4-chlorophenol experiment of the embodiment of the invention 2;
The photocatalytic activity stability experiment of Figure 11 embodiment of the invention.
The photocatalytic activity stability experiment of Figure 12 graphite phase carbon nitride.
The specific embodiment
As shown in Figure 1, a kind of TiO
2Graphite phase carbon nitride heterojunction composite photocatalyst, the structure of this composite photo-catalyst is: examine and be TiO
2Nano particle, shell are the graphite phase carbon nitride.
As shown in Figure 2, mechanism of the present invention is following: under light irradiation, and (the g-C of shell graphite phase carbon nitride
3N
4) produce light induced electron, and be injected into TiO
2Conduction band, and and TiO
2The oxygen reaction of surface adsorption generates the superoxide radical spike.Subsequently, from TiO
2Electronics of valence band migration to graphite phase carbon nitride, and at TiO with positive lotus
2Valence band produce the hole, the hole again with the water molecule reaction of absorption, produce the hydroxyl free radical spike.Be of the effect of graphite phase carbon nitride, thereby avoid it, reach the object of the invention by the photohole oxidation to photosensitizer.
As shown in Figure 3, a kind of TiO
2Graphite phase carbon nitride heterojunction composite photocatalyst preparation principle:
Because the nitrogen-atoms band lone electron pair of melamine is with positively charged TiO
2There is electrostatic force in nano particle, is adsorbed to TiO
2The surface of nano particle, under high-temperature and high-pressure conditions, the polycondensation of melamine generation deamination generates Miller amine then, thereby at TiO
2The surface of nano particle forms Miller amine clad.After washing, separation, drying, TiO
2The deamination polycondensation at high temperature further takes place in the Miller amine clad on the surface of nano particle, forms the black phase carbon nitride (g-C of stone
3N
4) layer, promptly get TiO according to the invention
2Graphite phase carbon nitride heterojunction composite photocatalyst.
Following embodiment further specifies of the present invention.
TiO
2The hydrosol can with reference to but and nonessential by the preparation of following method:
Under the vigorous stirring, 10mlTiCl4 is added in the 200ml frozen water, behind about 30Min, rise to room temperature, continue to stir 2h, dialysing to pH value through dialysis membrane then is about 5, can make TiO
2The hydrosol.
Embodiment 1:
The 0.56g melamine is joined 70mlTiO
2Colloidal sol, after stirring and dissolving, ultrasonic 10Min, 100 hydrothermal reaction kettles of packing into then, 180 ℃ of insulation 6h, naturally cool to room temperature then after, centrifugation and with distilled water washing 5 times, 80 ℃ of vacuum drying 12h at 550 ℃ of heat treatment 4h, promptly make TiO then
2Graphite phase carbon nitride heterojunction composite photocatalyst.The X-ray diffraction test shows, as shown in Figure 4: TiO
2Crystalline form is an anatase, calculates according to the Xie Leshi formula, and the about 5nm of its crystal grain, carbonitride are the graphite phase.The high resolution transmission electron microscopy result shows that as shown in Figure 6: catalyst is a nucleocapsid structure, examines to be TiO
2Nano particle, the about 5nm of particle diameter, shell are carbonitride, thick about 2nm.
Embodiment 2:
The 0.56g melamine is joined 70mlTiO
2Colloidal sol, after stirring and dissolving, ultrasonic 10Min, 100 hydrothermal reaction kettles of packing into then, 200 ℃ of insulation 6h, naturally cool to room temperature then after, centrifugation and with distilled water washing 5 times, 80 ℃ of vacuum drying 12h at 550 ℃ of heat treatment 4h, promptly make TiO then
2Graphite phase carbon nitride heterojunction composite photocatalyst.The X-ray diffraction test shows, as shown in Figure 7: TiO
2Crystalline form is an anatase, calculates according to the Xie Leshi formula, and the about 6.2nm of its crystal grain, carbonitride are the graphite phase.The high resolution transmission electron microscopy result shows that as shown in Figure 8: catalyst is a nucleocapsid structure, examines to be TiO
2Nano particle, the about 6nm of particle diameter, shell are carbonitride, thick about 2nm.Ultraviolet-visible diffuse reflection spectrum (Fig. 9) shows that composite photo-catalyst has good absorbent properties to visible light, absorbs sideband and is about 485nm; With the 4-chlorophenol is that the catalytic degradation experiment of simulating pollution thing shows (Figure 10), and this composite photo-catalyst has good visible light catalysis activity, and illumination 60Min can be with 4-chlorophenol degraded 80%.
Embodiment 3:
The 0.84g melamine is joined 70mlTiO
2Colloidal sol, after stirring and dissolving, ultrasonic 10Min, 100 hydrothermal reaction kettles of packing into then, 200 ℃ of insulation 6h, naturally cool to room temperature then after, centrifugation and with distilled water washing 5 times, 80 ℃ of vacuum drying 12h at 550 ℃ of heat treatment 4h, promptly make TiO then
2Graphite phase carbon nitride heterojunction composite photocatalyst.X-ray diffraction test shows: TiO
2Crystalline form is an anatase, calculates according to the Xie Leshi formula, and the about 5.2nm of its crystal grain, carbonitride are the graphite phase.The high resolution transmission electron microscopy result shows: catalyst is a nucleocapsid structure, examines to be TiO
2Nano particle, the about 5nm of particle diameter, shell are carbonitride, thick about 2nm.
Embodiment 4:
The 1.4g melamine is joined 70mlTiO
2Colloidal sol, after stirring and dissolving, ultrasonic 10Min, 100 hydrothermal reaction kettles of packing into then, 200 ℃ of insulation 6h, naturally cool to room temperature then after, centrifugation and with distilled water washing 5 times, 80 ℃ of vacuum drying 12h at 520 ℃ of heat treatment 4h, promptly make TiO then
2Graphite phase carbon nitride heterojunction composite photocatalyst.X-ray diffraction test shows: TiO
2Crystalline form is an anatase, calculates according to the Xie Leshi formula, and the about 5nm of its crystal grain, carbonitride are the graphite phase.The high resolution transmission electron microscopy result shows: catalyst is a nucleocapsid structure, examines to be TiO
2Nano particle, the about 5nm of particle diameter, shell are carbonitride, thick about 2nm.
Embodiment 5:
The 2.8g melamine is joined 70mlTiO
2Colloidal sol, after stirring and dissolving, ultrasonic 10Min, 100 hydrothermal reaction kettles of packing into then, 220 ℃ of insulation 6h, naturally cool to room temperature then after, centrifugation and with distilled water washing 5 times, 80 ℃ of vacuum drying 12h at 530 ℃ of heat treatment 4h, promptly make TiO then
2Graphite phase carbon nitride heterojunction composite photocatalyst.X-ray diffraction test shows: TiO
2Crystalline form is an anatase, calculates according to the Xie Leshi formula, and the about 4.8nm of its crystal grain, carbonitride are the graphite phase.The high resolution transmission electron microscopy result shows: catalyst is a nucleocapsid structure, examines to be TiO
2Nano particle, the about 5nm of particle diameter, shell are carbonitride, thick about 3nm.
The catalyst activity stability experiment:
Reference literature (Li, Langmuir, 2009,25:10397-10401), the 5g melamine at 550 ℃ of heat treatment 4h, is prepared pure graphite phase carbon nitride photochemical catalyst.
Accurately take by weighing pure graphite phase carbon nitride of 100mg and embodiment 2 prepared composite catalyst respectively, be added to 200ml 0.3 * 10
-4In the 4-chlorophenol aqueous solution of M, ultrasonic 5Min is after lucifuge stirs 1h; Adopting the 300W xenon lamp is analog light source; The following light of filtering 420nm wavelength is taken a sample behind the certain hour at interval, is flowing phase with methyl alcohol/deionized water (40: 60); Flow velocity 1ml/Min adopts residual 4-chlorophenol concentration in the high-performance liquid chromatogram determination solution.
Then with the centrifugal recovery of photochemical catalyst, 80 ℃ of dryings 6 hours.By above operation, reuse 4 times, carry out the catalyst activity stability experiment, like Figure 11, shown in 12.Visible from scheming: prepared composite photochemical catalyst of the present invention is under visible light irradiation, and 60Min is the 4-chlorophenol of degradable about 80%, and under the same terms, pure graphite phase carbon nitride can only degrade about 35%.In addition, with the increase of photochemical catalyst access times, pure graphite phase carbon nitride catalytic activity descends gradually; After reusing 4 times; At only can degrade about 25% 4-chlorophenol of visible light irradiation 60Min, and under the same terms, composite photo-catalyst still can keep about 80% degradation rate.The result shows that prepared composite photochemical catalyst of the present invention not only has good visible light catalysis activity, also has good stable property simultaneously.
Claims (7)
1. TiO
2Graphite phase carbon nitride heterojunction composite photocatalyst is characterized in that: the structure of this composite photo-catalyst is: examine and be TiO
2Nano particle, shell are the graphite phase carbon nitride.
2. according to the said a kind of TiO of claim 1
2Graphite phase carbon nitride heterojunction composite photocatalyst is characterized in that: TiO
2The crystal formation of nano particle is anatase or rutile or both mixtures.
3. a kind of TiO according to claim 1
2The preparation method of graphite phase carbon nitride heterojunction composite photocatalyst, it is characterized in that: preparation process is following:
A) with TiO
2The hydrosol and cyanamide compounds prepare the TiO that surperficial Miller amine coats through hydro-thermal reaction
2Nano particle;
B) to TiO
2After nano particle washing, separation, the drying, promptly get TiO through calcining
2Graphite phase carbon nitride heterojunction composite photocatalyst.
4. according to the said a kind of TiO of claim 3
2The preparation method of graphite phase carbon nitride heterojunction composite photocatalyst is characterized in that: said cyanamide compounds is meant the mixture of a kind of of cyanamide, double focusing cyanamide or melamine or several kinds.
5. according to the said a kind of TiO of claim 3
2The preparation method of graphite phase carbon nitride heterojunction composite photocatalyst is characterized in that: hydrothermal reaction condition is: 100 ℃～400 ℃ of reaction temperatures, reaction time 0.5h～50h.
6. according to the said a kind of TiO of claim 3
2The preparation method of graphite phase carbon nitride heterojunction composite photocatalyst is characterized in that: calcining heat is 300 ℃～1000 ℃, and calcination time is 0.5～10 hour.
7. according to the said a kind of TiO of claim 3
2The preparation method of graphite phase carbon nitride heterojunction composite photocatalyst is characterized in that: calcination atmosphere can be any of air, nitrogen or argon gas.
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