CN101690896A - Phosphor doping type nano titanium dioxide having efficient sunlight catalytic capability and preparation method thereof - Google Patents
Phosphor doping type nano titanium dioxide having efficient sunlight catalytic capability and preparation method thereof Download PDFInfo
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- CN101690896A CN101690896A CN200910036299A CN200910036299A CN101690896A CN 101690896 A CN101690896 A CN 101690896A CN 200910036299 A CN200910036299 A CN 200910036299A CN 200910036299 A CN200910036299 A CN 200910036299A CN 101690896 A CN101690896 A CN 101690896A
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Abstract
The invention relates to phosphor doping type nano titanium dioxide having efficient sunlight catalytic capability and a preparation method thereof. The average grain size of the phosphor doping type nano titanium dioxide is no more than15nm, and the specific surface of the nano titanium dioxide is 126.9m<2>/g. The preparation method is: taking tetrabutyl titanate as titanium source and phosphoric acid as phosphorus source, and using sol-gel method to synthesize phosphor doping type nano titanium dioxide grains; and grinding the obtained solid to be fine, and calcining at 400-900 DEG C to obtain P doping nano titanium dioxide grains. The best calcination temperature is 500 DEG C. The invention only requires to add phosphoric acid in alcoholic solution of tetrabutyl titanate to obtain phosphor doping nano titanium dioxide grains. When the nano grains are used for performing photocatalytic degradation on dye rhodamine B, sunlight can be directly adopted as the light source, and under the same conditions, the efficiency of photocatalytic degradation can exceed the commercial P25.
Description
Technical field
The present invention relates to a kind of nonmetalloid phosphorus doping nano titanium oxide, be specifically related to a kind of phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability, and the preparation method of this nano titanium oxide.
Background technology
Multiphase photocatalysis is the organic and inorganic pollution technology in a kind of good removal waste water, yet the photocatalytic system of the actual use that present people pay close attention to the most all concentrates on the application of reproducible solar energy resources.Use sunshine excite catalyze and degrade organic pollutants than have better commercial promise with the artificial ultraviolet excitation process that needs the high-energy input (Angew.Chem.Int.Ed., 2003,42,4908-4911.).
The anatase titania molecular structure is a kind of catalysis material efficiently, air purge, water pollute aspects such as handling and remove harmful substance all can bring into play very big effect (Chem.Rev., 1995,95.69-96).The anatase titania of nano-scale since its have than mutually much bigger specific surface of body and high forbidden band energy level, and demonstrate than body mutually better photocatalytic activity (Bull.Chem.Soc.Jpn., 2004,77,1427-1442.).Yet the relative body of the anatase of nano-scale is met and be converted into rutile structure under lower temperature.From anatase be transformed into rutile meet the specific surface that reduces particle widely (J.Photochem.Photobiol.A, 2002,148,263-271.).Thereby cause the reduction of the photocatalytic activity of titanium dioxide.In order to widen the application of titanium dioxide catalytic performance, improve its catalytic capability, the equilibrium temperature of necessary raising anatase phase increases its light conversion efficiency.Had some the report by doped metallic elements (J.Mater.Chem., 2003,13,2261-2265.) and nonmetalloid (Chem.Lett., 2003,32,330-331.) enter the titanium dioxide lattice and improve the titanium dioxide catalytic performance.Found that doping lanthanide ion in the titanium dioxide can improve the equilibrium temperature of anatase phase; And pass through the chemical bond fixed photocatalyst on other work object, and need under hot conditions, operate usually, be an important factors that influences its photocatalysis performance so whether photochemical catalyst is at high temperature stablized.Zhang et al. (J.Mater.Chem., 2003,13,2261-2265.) prepare micro-structural and lanthanide-doped titanium dioxide with photocatalysis performance by sol-gel process, they report by doping La
3+, Eu
3+, Gd
3 +, or Yb
3+After suppressed nano titanium oxide greatly and changed rutile into from anatase.By doping 1at%La
3+Perhaps Eu
3+The back still is an anatase behind 900 ℃ of calcining 1h.
Though a lot of in addition bibliographical informations have improved the TiO 2 visible light catalytic activity by doping, the catalytic activity under ultraviolet light seldom has with P25 makes comparisons.Wang et al. (Appl.Catal.B:Environment, 2005,57,223-231.) a kind of nitrogen-doped titanium dioxide of report degradation of phenol under various light sources, the result is presented under the radiation of visible light, and nitrogen-doped titanium dioxide demonstrates the better photocatalytic activity than commercial P25.Yet under solar light irradiation, the photocatalytic activity of nitrogen-doped titanium dioxide is not as P25.Efficiently a kind of in order to obtain, more economical high-temperature stability titanium dioxide, we prepare a kind of phosphorus doping titanium dioxide, and it still is not converted into the rutile phase under 900 ℃ of high temperature, and the phase transition temperature that changes rutile from anatase into improves greatly than unadulterated.The more important thing is that it has under solar light irradiation and than P25 better photocatalysis performance is arranged, utilize renewable solar energy degradation of contaminant more more convenient, direct, need not manually to drop into energy, have good commercial application prospect than visible light and ultraviolet light.
Summary of the invention
The purpose of this invention is to provide a kind of phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability, and the preparation method of this nano titanium oxide.This scheme will develop a kind of new efficient novel doping titanium dioxide nano particle that directly utilizes the sunshine degradating organic dye.On the one hand can energy savings, can also improve the dye wastewater treatment effeciency on the other hand.
The scheme of finishing the foregoing invention task is, a kind of phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability is characterized in that, described phosphor doping type nano titanium dioxide average particle size is below 15nm.
BET test shows, the specific surface of phosphor doping type nano titanium dioxide of the present invention are 126.9m
2/ g.
Say that more optimally the described phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability of the application is meant the nano titanium oxide that makes in order to the below method:
With the butyl titanate is the titanium source, and phosphoric acid is the phosphorus source, uses the synthetic phosphorus doping titanium dioxide nano-particle of sol-gel process; With the solid porphyrize that obtains, 400～900 ℃ of calcinings obtain the titania-doped powder of P again.The application recommends: best calcining heat is 500 ℃.
The scheme of finishing the 2nd invention task of the application is that a kind of above-mentioned preparation method with phosphor doping type nano titanium dioxide of efficient sunlight catalytic capability is characterized in that step is:
With the butyl titanate is the titanium source, and phosphoric acid is the phosphorus source, uses the synthetic phosphorus doping titanium dioxide nano-particle of sol-gel process; With the solid porphyrize that obtains, 400～900 ℃ of calcinings obtain the titania-doped powder of P again.The application recommends: best calcining heat is 500 ℃.
Be light source then with the sunshine, quartz curette is a container, the dyestuff rhodamine B is the degraded object, in the container of the rhodamine B solution of the 12mg/L that 25mL is housed, add prepared titanium dioxide nano-particle 5mg, rhodamine B and titanium dioxide nano-particle concentration ratio are 6: 5, shone 40 minutes down in sunshine, detect the absorption value A of rhodamine B with Cary5000 type UV, visible light sub-ray spectrometer, application of formula D%=(1-At/A at 553nm wavelength place
0Thereby) * 100 determine that the degradation rate of rhodamine B is 90.29%.
More optimize and more particularly, step of the present invention is:
Get alcohols, under magnetic agitation, add Ti (OC (1), earlier
4H
9)
4Alcohols and Ti (OC
4H
9)
4Volume ratio be 5～12: 1, optimum ratio is 10: 1, described alcohols can be used anhydrous C
2H
5OH, methyl alcohol or propyl alcohol.
(2), add ice CH again
3COOH, magnetic stirrer mixing, the solution that obtains are A liquid; Ti (OC
4H
9)
4With ice CH
3The volume ratio of COOH is 0.8～1.2: 1, and optimum ratio is 1: 1.
(3), in addition get a container, measure the pH value and be 2 the HCl aqueous solution, the HCl aqueous solution and Ti (OC
4H
9)
4Volume ratio be 1～1.5: 1, optimum ratio is 1.25: 1, adds H again
3PO
4, the solution that the vibration mixing obtains is B liquid;
(4), B liquid is slowly splashed in the A liquid, keep magnetic agitation, obtain stable transparent colloidal sol; The mol ratio of phosphoric acid and butyl titanate is 0.040～0.050: 1; The application recommends: the optimum mole ratio of phosphoric acid and butyl titanate is 0.044: 1.
(5), again the colloidal sol evaporation is obtained gel;
(6), then gel is dried in baking oven;
(7), again with the solid porphyrize that obtains, 400～900 ℃ of calcinings obtain the titania-doped powder of P.
The application recommends: best calcining heat is 500 ℃.
Advantage of the present invention
1. the present invention at the preparation nano titanium oxide, obtains phosphorus doping titanium dioxide nano-particle as long as add phosphoric acid in the alcoholic solution of butyl titanate with sol-gel process.
2. with the titanium dioxide nano-particle of the present invention preparation, the nano particle average-size that obtains through 500 ℃ of calcinings is less than 15nm, specific surface 126m
2/ g, and still remain anatase after 900 ℃ of calcinings, improve the phase transition temperature that anatase is converted into rutile greatly.
3. the phosphorus doping nano particle that obtains of the present invention's 500 ℃ of calcinings of preparing, when being used for the photocatalytic degradation of dye rhodamine B, directly using sunshine is light source, photocatalytic degradation efficient surpasses commercial P25 under the equal conditions.
Description of drawings
Fig. 1: P doped Ti O
2Nano particle after 500 ℃ of calcinings (P500) TEM figure.As can be seen from the figure the P doped with nanometer particle is a loose structure, and average particle size has to a certain degree and reunites less than 15nm.
Fig. 2: P500, P25, not doped Ti O
2The Uv-Vis of the nano particle spectrogram that diffuses.Show on the figure that the P500 sample absorbs light than P25 and doped Ti O not in the ultra-violet (UV) band
2Nano particle is strong.
Fig. 3: the P doped samples shows among the figure that the P doped samples anatase crystal just occurs 120 ℃ of processing, and still be the anatase phase after 900 ℃ of calcining at the XRD figure of different temperatures calcining.
Fig. 4: the XPS spectrum figure of P500 sample, the peak proof P element doping that the 133.22eV place occurs in the spectrogram has entered in the titanium dioxide nano-particle.
Fig. 5: P500, P25, the degradation rate of doping titanium dioxide nano particle catalytic degradation rhodamine B under solar light irradiation change curve in time not, and contrast with blank rhodamine B self photoactivate under similarity condition.As can be seen from the figure, P500 degradation effect the best under the same conditions, rhodamine B self has certain photoactivate performance, but with the reacting phase that adds catalyst than obviously ignoring.
The specific embodiment
Device required for the present invention mainly contains magnetic stirring apparatus, dropping funel, conical flask, graduated cylinder, liquid-transfering gun, mortar, crucible, Rotary Evaporators, baking oven, Muffle furnace etc.; The P doped titanium dioxide collosol that sol-gel process is made is rotated evaporation, the organic matters such as most of butanols that reaction is generated are evaporated and obtain gel, again gel 120 ℃ of oven dry of baking oven, pulverize in mortar then changes in the crucible that the following 500 ℃ of calcinings of air atmosphere obtained sample in 3 hours in Muffle furnace over to.
Embodiment 1 is the titanium source with the butyl titanate, and phosphoric acid is the phosphorus source, preparation P doping titanium dioxide nano particle under the room temperature.
With mol ratio [H
3PO
4]/[Ti (OC
4H
9)
4]=0.044/1 sampling, a typical preparation method gets the anhydrous C of 20mL earlier
2H
5OH adds 4mL Ti (OC under magnetic agitation in the 50mL conical flask
4H
9)
4, add 4mL ice CH again
3COOH, magnetic stirrer mixing, the solution that obtains are A liquid; Other gets a 20mL conical flask, measures the anhydrous C of 20mL
2H
5OH is measured 5mL, pH value and is 2 the HCl aqueous solution in conical flask again in conical flask, add 30 μ L then and analyze pure H
3PO
4, the solution that the vibration mixing obtains is B liquid; B liquid changed over to slowly splash in the A liquid in the dropping funel, keep magnetic agitation, approximately 2h dropwises, obtain stable transparent colloidal sol, again the colloidal sol rotary evaporation is obtained gel, then with gel 120 ℃ of oven dry in baking oven, again with the solid porphyrize that obtains, divide into groups in Muffle furnace to calcine 3h respectively and to obtain the titania-doped powder of P with 400～900 ℃ different temperatures.The powder that makes is characterized with TEM, Uv-Vis, XRD, XPS.(see Fig. 1～Fig. 4)
Catalytic degradation rhodamine B under the P doped samples sunshine after the calcining of embodiment 2 different temperatures
Take by weighing each 5mg of different temperatures (400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃) calcining P doped samples in 5 quartz curettes, the rhodamine B solution that adds 25mL 0.01g/L again, behind the ultrasonic 15min of lucifuge with 5 quartz curettes simultaneously in outdoor sunshine down behind the irradiation 30min, from 5 quartz curettes, take out 3mL degraded back troubled liquor respectively, centrifugal, get supernatant liquor and record the absorbance A value, according to formula D%=(1-A at 553nm peak position place
t/ A
0Percent of decolourization is calculated in) * 100.
The embodiment 3 variety classes titanium dioxide rhodamine B of under sunshine, degrading
Take by weighing respectively that 5mg is not titania-doped, P is titania-doped, P25 is in same quartz curette, in 3 quartz curettes, add 25mL 0.01g/L rhodamine B solution more respectively, behind the ultrasonic 15min of lucifuge, other gets a same quartz curette and also adds rhodamine B solution with concentration, four quartz curettes all are placed on irradiation 40min under the outdoor sunshine, every the 10min sampling once, centrifugal, get supernatant liquor test absorption spectrum, take a sample and finish illumination four times, read the absorption A value at 553nm peak position place, according to formula D%=(1-A
t/ A
0Percent of decolourization is calculated in) * 100, obtains Fig. 5.
Embodiment 4, substantially the same manner as Example 1, but following change is arranged:
Alcohols alcohols described in (1) step and Ti (OC
4H
9)
4Volume ratio be 10: 1, described alcohols is a methyl alcohol;
Ti (OC described in (2) step
4H
9)
4With ice CH
3The volume ratio of COOH is 1: 1;
The HCl aqueous solution described in (3) step and Ti (OC
4H
9)
4Volume ratio be 1.25: 1;
The mol ratio of phosphoric acid and butyl titanate described in (4) step is for being 0.044: 1;
Calcining heat described in (7) step is 500 ℃.
Embodiment 5, substantially the same manner as Example 1, but following change is arranged:
Alcohols alcohols described in (1) step and Ti (OC
4H
9)
4Volume ratio be 5: 1; Described alcohols is a propyl alcohol;
Ti (OC described in (2) step
4H
9)
4With ice CH
3The volume ratio of COOH is 0.8: 1;
The HCl aqueous solution described in (3) step and Ti (OC
4H
9)
4Volume ratio be 1: 1;
The mol ratio of phosphoric acid and butyl titanate described in (4) step is 0.040: 1.
Embodiment 6, substantially the same manner as Example 1, but following change is arranged:
Alcohols alcohols described in (1) step and Ti (OC
4H
9)
4Volume ratio be 12: 1;
Ti (OC described in (2) step
4H
9)
4With ice CH
3The volume ratio of COOH is 1.2: 1;
The HCl aqueous solution described in (3) step and Ti (OC
4H
9)
4Volume ratio be 1.5: 1;
The mol ratio of phosphoric acid and butyl titanate described in (4) step is 0.050: 1.
Claims (8)
1. the phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability is characterized in that, described phosphor doping type nano titanium dioxide average particle size is below 15nm.
2. the phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability according to claim 1 is characterized in that, the specific surface of described phosphor doping type nano titanium dioxide is 126.9m
2/ g.
3. the phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability according to claim 1 and 2, it is characterized in that, described phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability is meant the nano titanium oxide that makes in order to the below method:
With the butyl titanate is the titanium source, and phosphoric acid is the phosphorus source, uses the synthetic phosphorus doping titanium dioxide nano-particle of sol-gel process; With the solid porphyrize that obtains, 400～900 ℃ of calcinings obtain the titania-doped powder of P again.
4. the phosphor doping type nano titanium dioxide with efficient sunlight catalytic capability according to claim 3 is characterized in that, described calcining heat is 500 ℃.
5. described preparation method with phosphor doping type nano titanium dioxide of efficient sunlight catalytic capability of claim 1 is characterized in that step is:
With the butyl titanate is the titanium source, and phosphoric acid is the phosphorus source, uses the synthetic phosphorus doping titanium dioxide nano-particle of sol-gel process; With the solid porphyrize that obtains, 400～900 ℃ of calcinings obtain the titania-doped powder of P again.
6. the preparation method with phosphor doping type nano titanium dioxide of efficient sunlight catalytic capability according to claim 5 is characterized in that, the concrete operations step is:
Get alcohols, under magnetic agitation, add Ti (OC (1), earlier
4H
9)
4Alcohols and Ti (OC
4H
9)
4Volume ratio be 5～12: 1;
(2), add ice CH again
3COOH, magnetic stirrer mixing, the solution that obtains are A liquid; Ti (OC
4H
9)
4With ice CH
3The volume ratio of COOH is 0.8～1.2: 1;
(3), in addition get a container, measure the pH value and be 2 the HCl aqueous solution, the HCl aqueous solution and Ti (OC
4H
9)
4Volume ratio be 1～1.5: 1, add H again
3PO
4, the solution that the vibration mixing obtains is B liquid;
(4), B liquid is slowly splashed in the A liquid, keep magnetic agitation, obtain stable transparent colloidal sol; The mol ratio of phosphoric acid and butyl titanate is 0.040～0.050: 1;
(5), again the colloidal sol evaporation is obtained gel;
(6), then gel is dried in baking oven;
(7), again with the solid porphyrize that obtains, 400～900 ℃ of calcinings obtain the titania-doped powder of P.
7. according to claim 5 or 6 described preparation methods, it is characterized in that with phosphor doping type nano titanium dioxide of efficient sunlight catalytic capability,
Alcohols alcohols described in (1) step and Ti (OC
4H
9)
4Volume ratio be 10: 1, described alcohols is anhydrous C
2H
5OH, methyl alcohol or propyl alcohol;
Ti (OC described in (2) step
4H
9)
4With ice CH
3The volume ratio of COOH is 1: 1;
The HCl aqueous solution described in (3) step and Ti (OC
4H
9)
4Volume ratio be 1.25: 1;
The mol ratio of phosphoric acid and butyl titanate described in (4) step is for being 0.044: 1.
8. the preparation method with phosphor doping type nano titanium dioxide of efficient sunlight catalytic capability according to claim 7 is characterized in that described calcining heat described in (7) step is 500 ℃.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188986A (en) * | 2011-03-31 | 2011-09-21 | 北京化工大学 | Preparation of visible light response titanium base film and method for degrading binary dye |
| CN102515271A (en) * | 2011-12-22 | 2012-06-27 | 东北大学秦皇岛分校 | TiO2 powder with visible light catalytic activity and preparation method thereof |
| CN103394343A (en) * | 2013-08-16 | 2013-11-20 | 河海大学 | Preparation method and application of metal-doped titanium dioxide material |
| CN104096540A (en) * | 2014-07-17 | 2014-10-15 | 同济大学 | Preparation method of adsorption and catalysis material for removing heavy metals and organic pollutants in municipal sludge |
| CN107433202A (en) * | 2017-09-22 | 2017-12-05 | 常州大学 | A kind of preparation method of phosphorus doping manganese tungstate |
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| CN116273088A (en) * | 2023-03-30 | 2023-06-23 | 深圳先进技术研究院 | Phosphorus doped titanium dioxide and preparation method and application thereof |
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2009
- 2009-10-13 CN CN200910036299A patent/CN101690896A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188986A (en) * | 2011-03-31 | 2011-09-21 | 北京化工大学 | Preparation of visible light response titanium base film and method for degrading binary dye |
| CN102515271A (en) * | 2011-12-22 | 2012-06-27 | 东北大学秦皇岛分校 | TiO2 powder with visible light catalytic activity and preparation method thereof |
| CN103394343A (en) * | 2013-08-16 | 2013-11-20 | 河海大学 | Preparation method and application of metal-doped titanium dioxide material |
| CN104096540A (en) * | 2014-07-17 | 2014-10-15 | 同济大学 | Preparation method of adsorption and catalysis material for removing heavy metals and organic pollutants in municipal sludge |
| CN107433202A (en) * | 2017-09-22 | 2017-12-05 | 常州大学 | A kind of preparation method of phosphorus doping manganese tungstate |
| CN109095951A (en) * | 2018-07-03 | 2018-12-28 | 佛山欧神诺陶瓷有限公司 | A kind of Antibacterial ceramic tile and preparation method thereof digitizing inkjet printing |
| CN109809711A (en) * | 2019-03-27 | 2019-05-28 | 揭阳市宏光镀膜玻璃有限公司 | Three silver medal LOW-E glass of phosphorus doping self-cleaning and preparation method thereof |
| CN116273088A (en) * | 2023-03-30 | 2023-06-23 | 深圳先进技术研究院 | Phosphorus doped titanium dioxide and preparation method and application thereof |
| WO2024198511A1 (en) * | 2023-03-30 | 2024-10-03 | 深圳先进技术研究院 | Phosphorus-doped titanium dioxide, preparation method therefor and use thereof |
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Open date: 20100407 |