CN102513043A - Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres - Google Patents
Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres Download PDFInfo
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- CN102513043A CN102513043A CN2011103955133A CN201110395513A CN102513043A CN 102513043 A CN102513043 A CN 102513043A CN 2011103955133 A CN2011103955133 A CN 2011103955133A CN 201110395513 A CN201110395513 A CN 201110395513A CN 102513043 A CN102513043 A CN 102513043A
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- nitrogen
- microspheres
- titanium dioxide
- microballoon
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 title abstract description 9
- 239000004005 microsphere Substances 0.000 title abstract 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims 2
- 238000003756 stirring Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000003223 protective agent Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 12
- 229910010413 TiO 2 Inorganic materials 0.000 description 9
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229920002415 Pluronic P-123 Polymers 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- GMMZXKSNKIUKOW-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].C(C)O Chemical compound [O-2].[O-2].[Ti+4].C(C)O GMMZXKSNKIUKOW-UHFFFAOYSA-N 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- -1 solar cell Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres. In the invention, urea is used as a nitrogen source, hydrochloric acid is used as a protecting agent of butyl titanate (TBT), and a solvent heat method (ethanol and water mixing liquid is used as a solvent) is adopted for synthesizing the N-doped TiO2 microspheres. According to the method, TiO2 microspheres with good appearance can be prepared, and in addition, nitrogen elements in the urea is utilized for nitrogen doping, so the visible light absorption of the TiO2 microspheres is obviously improved. The method simultaneously realizes the microsphere preparation and the N doping, the preparation process is simple, the cost is low, and in addition, the application range is wide. The preparation method can be used in the fields of catalysis, dye solar cells, and the like.
Description
Technical field
The present invention relates to TiO
2The preparing technical field of microballoon is specifically related to the TiO that a kind of N mixes
2The preparation method of microballoon.
Background technology
TiO
2Be a kind of important inorganic material, the physical and chemical performance that have big specific area, high surface, thermal conductance is good, absorbing properties is good and good dispersion etc. is unique is widely used in fields such as photochemical catalyst, solar cell, gas sensor.TiO
2Energy gap be 3.2eV (Detitanium-ore-type), absorbing wavelength is less than 388nm, absorption bands is confined to ultraviolet region, this means TiO
2Can only utilize a spot of sunshine (3 ~ 5%), and the visible light that in sunshine, is in the great majority (about 45%) can't utilize.In order to expand absorption at visible region, further improve nano ZnO (referring to Burda C, Lou Y, Chen X, et a1 J] .Nano letters, 2003,3 (8): 1049-1051.), it is carried out ion doping is a kind of effective ways.Like anion (like C, N, B, S, F, Cl), cation (like Fe
3+, Mo
5+, Na
+/ Mg
2+Deng) and metal (like Pt, Au, Cr, Ag, the V) report improve its photocatalytic activity that mixes emerge in an endless stream.Nanoscale TiO2 has good catalytic performance in photocatalytic process in addition, but in use has shortcomings such as easy inactivation, easy reunion and difficult recovery, has limited its application at degraded water pollutant this respect.And micron order TiO
2Can avoid these shortcomings effectively, and can recycle and reuse, improve its utilization rate effectively.Present TiO
2The microballoon preparation has become a research direction of nano science.At present, preparation TiO
2The method of spheric granules mainly contains sol-gel process, the precipitation method, emulsion method and solvent-thermal method etc.
The researcher is around preparation TiO both at home and abroad
2Spheric granules has launched a large amount of research, and has obtained certain effect.Kim, and Y.J. etc. (referring to Kim, Y.J, Advanced Materials, 2009. 21 (36): p. 3668-3673.) adopt solvent-thermal method, use methyl alcohol, acetonitrile has prepared TiO as solvent
2Microballoon.But this method has been introduced poisonous acetonitrile, the methyl alcohol of people.In addition, this microballoon is very little to absorption of visible light, need mix with expansion TiO
2The photoresponse scope.Yu; H.K. etc. (referring to Yu; H.K Chemistry of Materials; 2008. 20 (8): p. 2704-2710.) prepared the microballoon that particle diameter can be controlled with Tween 20 and Pluronic P123 as surfactant, but cost of material being somewhat expensive, also is a very big problem so reduce cost of material.
Summary of the invention
To the problem that exists in the prior art, the purpose of this invention is to provide the TiO that a kind of N mixes
2The solvothermal preparation method of microballoon, this method has been carried out the N doping simultaneously in the preparation microballoon, can expand TiO preferably
2The absorption spectrum of material and light scattering property have wide practical use in photocatalysis and photochemical cell.
The objective of the invention is to realize like this: the mixed liquor of hydrochloric acid and butyl titanate is poured in the mixed liquor of urea and second alcohol and water and stirred, wherein ethanol: water: urea: hydrochloric acid: the mol ratio of butyl titanate is (111.2 ~ 130): (0 ~ 78.8): (5 ~ 1): (5 ~ 1): 1; Mixed solution is transferred in the Pressure solution bullet in 80～160 ℃ of insulations 2～10 hours, is collected bottom precipitation, will be deposited in 300～500 ℃ down calcining obtained the titania-doped microballoon of N in 2 hours.
The TiO that N provided by the invention mixes
2The solvothermal preparation method of microballoon, this method can realize simultaneously that the preparation of titanium dioxide microballoon sphere and nitrogen mix, and can promote the light scattering and its absorption spectrum ranges of expansion of titanic oxide material preferably.And this method technology is simple, with low cost, and good stability has wide practical use in fields such as photocatalysis and DSSCs.
Description of drawings
The pattern of titanium dioxide microballoon sphere when Fig. 1 is 2:1 for the mol ratio of hydrochloric acid and butyl titanate.
The pattern of titanium dioxide microballoon sphere when Fig. 2 is 2.6:1 for the mol ratio of hydrochloric acid and butyl titanate.
The pattern of titanium dioxide microballoon sphere when Fig. 3 is 3.3:1 for the mol ratio of hydrochloric acid and butyl titanate.
The pattern of titanium dioxide microballoon sphere when Fig. 4 is 4:1 for the mol ratio of hydrochloric acid and butyl titanate.
Fig. 5 is for adding the pattern of ethanol titanium dioxide microballoon sphere when the mol ratio of water is 111.2:78.8.
Fig. 6 is the N doping microballoon and the P of preparation
25Uv-visible absorption spectra relatively.The mol ratio of hydrochloric acid and butyl titanate is 2.6:1.
Below in conjunction with embodiment the present invention is described further.
The specific embodiment
TiO when the mol ratio of embodiment 1 hydrochloric acid and butyl titanate is respectively 2:1
2
Microballoon
With mol ratio is that the mixed liquor of hydrochloric acid and the butyl titanate of 2:1 is poured in the mixed liquor of urea and second alcohol and water and stirred 2-5 hour.Wherein ethanol, water and urea ratio are 130:0:1.7.Mixed solution is transferred in the Pressure solution bullet 80～160 ℃ of insulations 2～10 hours.Collect bottom precipitation,, obtain the titania-doped microballoon of N 400 ℃ of calcinings 2 hours.As shown in Figure 1, work as M
(HCl): M
(TBT)During for 2:1, most of balling-up, but also have quite a few TiO
2Powder, and the dispersiveness of microballoon is also poor.
TiO when the mol ratio of embodiment 2 hydrochloric acid and butyl titanate is respectively 2.6:1
2
Microballoon
With mol ratio is that the mixed liquor of hydrochloric acid and the butyl titanate of 2.6:1 is poured in the mixed liquor of urea and second alcohol and water and stirred 2-5 hour.Wherein ethanol, water and urea ratio are 130:0:1.7.Mixed solution is transferred in the Pressure solution bullet 80～160 ℃ of insulations 2～10 hours.Collect bottom precipitation,, obtain the titania-doped microballoon of N 400 ℃ of calcinings 2 hours.Work as M
(HCl): M
(TBT)(Fig. 2) obtains the microballoon of good dispersion during for 2.6:1, but some TiO still
2Powder.With ultraviolet-visible absorption spectroscopy paired observation nitrogen doped Ti O
2The spectral response of microballoon and P25 titanium dioxide powder changes (as shown in Figure 6), and though find microballoon that nitrogen mixes ultraviolet region (250～400nm) or visible region (400～650nm) absorption intensity has all surpassed P25.
TiO when the mol ratio of embodiment 3 hydrochloric acid and butyl titanate is respectively 3.3:1
2
Microballoon
With mol ratio is that the mixed liquor of hydrochloric acid and the butyl titanate of 3.3:1 is poured in the mixed liquor of urea and second alcohol and water and stirred 2-5 hour.Wherein ethanol, water and urea ratio are 130:0:1.7.Mixed solution is transferred in the Pressure solution bullet 80～160 ℃ of insulations 2～10 hours.Collect bottom precipitation,, obtain the titania-doped microballoon of N 400 ℃ of calcinings 2 hours.The M that works as as shown in Figure 3
(HCl): M
(TBT)Basically all balling-up during for 3.3:1, particle diameter is compared and has been reduced simultaneously, and dispersed and homogeneity also is improved.
TiO when the mol ratio of embodiment 4 hydrochloric acid and butyl titanate is respectively 4:1
2
Microballoon
With mol ratio is that the mixed liquor of hydrochloric acid and the butyl titanate of 4:1 is poured in the mixed liquor of urea and second alcohol and water and stirred 2-5 hour.Wherein ethanol, water and urea ratio are 130:0:1.7.Mixed solution is transferred in the Pressure solution bullet 80～160 ℃ of insulations 2～10 hours.Collect bottom precipitation,, obtain the titania-doped microballoon of N 400 ℃ of calcinings 2 hours.The M that works as as shown in Figure 4
(H2O): M
(HCl)When being increased to 4:1, though all balling-up, it is many that the fusion between the microballoon becomes, thereby dispersed variation.
The TiO of embodiment 5 ethanol when the mol ratio of water is 111.2:78.8
2
Microballoon
With mol ratio is that the mixed liquor of hydrochloric acid and the butyl titanate of 2.6:1 is poured in the mixed liquor of urea and second alcohol and water and stirred 2-5 hour, and wherein the mol ratio of ethanol, water and urea is 111.2:78.8:1.7.Mixed solution is transferred in the Pressure solution bullet 80～160 ℃ of insulations 2～10 hours.Collect bottom precipitation,, obtain the titania-doped microballoon of N 400 ℃ of calcinings 2 hours.As shown in Figure 5, microspherulite diameter size decreases and surface become coarse.
Claims (3)
1. the preparation method of the titanium dioxide microballoon sphere that mixes of a N; It is characterized in that: the mixed liquor of hydrochloric acid and butyl titanate is poured into stir in the mixed liquor of urea and second alcohol and water and obtained mixed solution; Mixed solution is transferred in the Pressure solution bullet 80～160 ℃ of insulations 2～10 hours; Collect bottom precipitation, will precipitate and obtain the titania-doped microballoon of N after calcining.
2. the preparation method of the titanium dioxide microballoon sphere that N according to claim 1 mixes is characterized in that: ethanol: water: urea: hydrochloric acid: the mol ratio of butyl titanate is (111.2 ~ 130): (0 ~ 78.8): (5 ~ 1): (5 ~ 1): 1.
3. the preparation method of the titanium dioxide microballoon sphere that N according to claim 1 mixes is characterized in that: describedly will precipitate calcining and be meant at 300～500 ℃ and calcined 2 hours down.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240109A (en) * | 2013-03-27 | 2013-08-14 | 天津大学 | High-activity N-doped modified titanium dioxide nanometer photocatalytic material and preparation method thereof |
| CN103346261A (en) * | 2013-05-29 | 2013-10-09 | 许昌学院 | A TiO2 and MEH-PPV hybrid composite heterojunction thin film solar cell and its preparation and application |
| CN103418416A (en) * | 2013-08-30 | 2013-12-04 | 武汉理工大学 | Preparation method of nitrogen doping titanium dioxide powder, prepared titanium dioxide powder material and purpose thereof |
| CN103623800A (en) * | 2013-11-29 | 2014-03-12 | 济南大学 | Method for preparing titanium dioxide ball and obtained product |
| CN104772159A (en) * | 2015-04-07 | 2015-07-15 | 北京化工大学 | Nitrogen-doped anatase TiO2 nanosheet multi-level balls and preparation method thereof |
| CN105870447A (en) * | 2016-05-31 | 2016-08-17 | 中南大学 | Preparation method of nitrogen-doped rutile TiO2/C negative electrode material for sodium ion battery |
| CN106334574A (en) * | 2016-09-26 | 2017-01-18 | 广西科技大学 | Preparation method of high-water-dispersibility nitrogen-doped nano-titanium dioxide |
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2011
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Patent Citations (1)
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| CN1935668A (en) * | 2006-09-30 | 2007-03-28 | 华南理工大学 | Nitrogen-doped titanium dioxide solvent thermal preparation method |
Non-Patent Citations (2)
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240109A (en) * | 2013-03-27 | 2013-08-14 | 天津大学 | High-activity N-doped modified titanium dioxide nanometer photocatalytic material and preparation method thereof |
| CN103346261A (en) * | 2013-05-29 | 2013-10-09 | 许昌学院 | A TiO2 and MEH-PPV hybrid composite heterojunction thin film solar cell and its preparation and application |
| CN103346261B (en) * | 2013-05-29 | 2016-02-03 | 许昌学院 | A kind of TiO 2with MEH-PPV hybridization compounding hetero-junction thin-film solar cell and preparation and application thereof |
| CN103418416A (en) * | 2013-08-30 | 2013-12-04 | 武汉理工大学 | Preparation method of nitrogen doping titanium dioxide powder, prepared titanium dioxide powder material and purpose thereof |
| CN103623800A (en) * | 2013-11-29 | 2014-03-12 | 济南大学 | Method for preparing titanium dioxide ball and obtained product |
| CN103623800B (en) * | 2013-11-29 | 2016-04-13 | 济南大学 | A kind of preparation method of titanium dioxide ball and products obtained therefrom |
| CN104772159A (en) * | 2015-04-07 | 2015-07-15 | 北京化工大学 | Nitrogen-doped anatase TiO2 nanosheet multi-level balls and preparation method thereof |
| CN105870447A (en) * | 2016-05-31 | 2016-08-17 | 中南大学 | Preparation method of nitrogen-doped rutile TiO2/C negative electrode material for sodium ion battery |
| CN105870447B (en) * | 2016-05-31 | 2018-03-27 | 中南大学 | Sodium-ion battery N doping rutile TiO2The preparation method of/C negative materials |
| CN106334574A (en) * | 2016-09-26 | 2017-01-18 | 广西科技大学 | Preparation method of high-water-dispersibility nitrogen-doped nano-titanium dioxide |
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Application publication date: 20120627 |