CN103240072B - Core-shell structure nanoribbon photocatalyst and preparation method thereof - Google Patents
Core-shell structure nanoribbon photocatalyst and preparation method thereof Download PDFInfo
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- CN103240072B CN103240072B CN201310207737.6A CN201310207737A CN103240072B CN 103240072 B CN103240072 B CN 103240072B CN 201310207737 A CN201310207737 A CN 201310207737A CN 103240072 B CN103240072 B CN 103240072B
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- 238000002360 preparation method Methods 0.000 title claims description 20
- 239000002074 nanoribbon Substances 0.000 title abstract 8
- 239000011258 core-shell material Substances 0.000 title abstract 4
- 239000011941 photocatalyst Substances 0.000 title abstract 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 29
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000003054 catalyst Substances 0.000 claims description 19
- 239000002127 nanobelt Substances 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 6
- 238000003746 solid phase reaction Methods 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 3
- 229910010251 TiO2(B) Inorganic materials 0.000 abstract 3
- 230000002194 synthesizing effect Effects 0.000 abstract 2
- 229910020293 Na2Ti3O7 Inorganic materials 0.000 abstract 1
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract 1
- 238000005242 forging Methods 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 6
- 229910002115 bismuth titanate Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
The invention discloses a TiO2(B)@Bi20TiO32 core-shell structure nanoribbon photocatalyst, wherein the core-shell structure nanoribbon has the width size of 100nm-150nm, and the length of 10 micron-990 micron, and the nanoribbon is internally provided with TiO2(B), and is externally provided with Bi20TiO32. The photocatalyst provided by the invention is synthesized through low-temperature solid phase reaction, namely, Na2Ti3O7 is adopted within the nanoscale range as a reaction template and a reaction raw material, and is sufficiently mixed with pentahydrate bismuth nitrate hydrolysis suspension with certain concentration; and firstly a hybrid precursor nanoribbon is synthesized by utilizing electrostatic attraction among granules, and finally the TiO2(B)@Bi20TiO32 core-shell structure nanoribbon photocatalyst is obtained through low-temperature forging and synthesizing. Because the solid phase reaction is completed once at low temperature, and the technology device is simple, the obtained nanoribbon is narrow in width distribution, is controllable in length, is short in reaction cycle, has good repeatability, has a wide development prospect, and provides a simple and feasible synthesizing line for preparing other titanate nanoribbon materials by a solid phase reaction method.
Description
Technical field
The present invention relates to a kind of TiO
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst and preparation method thereof.
Background technology
The control that environment in recent years is polluted more and more comes into one's own with administering, and the environmental problem going from bad to worse is in the urgent need to a kind of more environmental protection, the cheap technology pollutant in atmosphere and water body of degrading.Photocatalysis performance is one of special performance of Nano semiconductor.Nano semiconductor material, under the irradiation of light, by being chemical energy light energy conversion, impelling the synthetic of compound or makes the process of compound (organic matter, inorganic matter) degraded be referred to as catalysis material.From then on, with TiO
2for the semiconductor light-catalyst representing starts to grow up.But TiO
2photocatalysis efficiency not high, and photoresponse scope is at ultraviolet region, sunshine utilization rate is low, has restricted its development.
Bi
2o
3and TiO
2be compounded to form the composite oxides with multiple crystal phase structure: as Bi
4ti
3o
12, Bi
2ti
2o
7, Bi
2ti
4o
11, Bi
12tiO
20, Bi
20tiO
32deng, be referred to as bismuth titanates compound.By studying these bismuth titanates compounds and P-25(anatase TiO
2nano-powder) ultraviolet～visible scattered reflection spectrum discovery, the energy gap of these several bismuth titanates materials is all less than 3eV, and ABSORPTION EDGE is 400～580nm, and TiO
2energy gap be 3.2eV, ABSORPTION EDGE is 387.5nm, by contrast, there is " red shift " phenomenon in the ABSORPTION EDGE of bismuth titanates material, makes it in visible wavelength range, have good photocatalytic effect.Bi wherein
20tiO
32because thering is high N-shaped photoconduction and high carrier mobility, and possesses good ultraviolet～visible light catalytic effect.
Up to now, there is not yet relevant Bi
20tiO
32report prepared by nanobelt.[Hefeng Cheng, Baibiao Huang, the Ying Dai et al.Visible-light photocatalytic activity of the metastable Bi such as Hefeng Cheng
20tiO
32synthesized by a high-temperature quenching method[J] .Journal of Solid State Chemistry.2009,182:2274-2278.] by solid reaction process, at 1000 ℃, prepared Bi
20tiO
32nano particle, and its visible light catalytic performance is studied, Bi shown
20tiO
32in visible wavelength range, methyl orange is had to good catalytic effect; [the Tengfei Zhou and Juncheng Hu.Mass Production and Photocatalytic Activity of Highly Crystalline Metastable Single-Phase Bi such as Tengfei Zhou
20tiO
32nanosheets[J] .Environ.Sci.Technol.2010,44:8698 – 8703.] by sol-gal process, prepared Bi
20tiO
32nanometer sheet etc.But the Bi preparing
20tiO
32powder because of its pattern be that nano particle is difficult for recycling, and these methods or high to equipment requirement, equipment and instrument is more expensive; Utilization rate to raw material is very little; Or complex process, manufacturing cycle is long, repeatable poor.In order to reach practical object, the necessary Bi that Development and Production cost is low, simple to operate, the cycle is short
20tiO
32the preparation technology of nanobelt.
Summary of the invention
For the deficiencies in the prior art, the present invention requires the problem solving to be to provide a kind of TiO
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst and preparation method thereof.
TiO of the present invention
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst, is characterized in that: described photochemical catalyst is that width dimensions is 100nm～150nm, and length is the TiO of 10 μ m～990 μ m
2(B)@Bi
20tiO
32nuclear shell structure nano band, wherein nanobelt the inside is TiO
2(B), outside is Bi
20tiO
32.
Described TiO of the present invention
2(B)@Bi
20tiO
32the preparation method of nuclear shell structure nano band photochemical catalyst, step is:
(1) the nano titanium oxide P25 of reacting dose is dissolved in the NaOH solution of 10M, ultrasonic, stir each 0.5h and fall back in thermal response still, compactedness is controlled at 60～80% of reactor volume; Then seal hydrothermal reaction kettle, put it in drying box, make hydrothermal temperature be controlled at 200 ± 10 ℃, the reaction time is controlled at 24h～72h, after reaction finishes, naturally cools to room temperature, and gained powder rinses repeatedly by deionized water, and then suction filtration, makes Na
2ti
3o
7powder, stand-by;
(2) by analytically pure five water bismuth nitrate (Bi (NO
3)
35H
2o) add in distilled water, and constantly stir, be mixed with Bi
3+concentration is the suspension of 2.5mmol/L～10mmol/L, and gained solution is designated as A solution;
(3) to Na in molar ratio in A solution
+: Bi
3+the ratio of=1:1 adds above-mentioned Na
2ti
3o
7powder, and constantly stir, forming precursor solution, gained solution is designated as B solution; By after the B solution left standstill 48h of preparation, gained powder rinses repeatedly by deionized water, and then suction filtration, will make powder and be placed in 60 ± 5 ℃ of dry 10～15h of drying box;
(4) the dried powder of step (3) is put into Muffle furnace and calcine 2～3h at 450 ± 10 ℃, then cool to room temperature with the furnace, make TiO free from foreign meter
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst.
Above-mentioned TiO
2(B)@Bi
20tiO
32in the preparation method of nuclear shell structure nano band photochemical catalyst: the described Bi of step (2)
3+concentration is preferably 2.5mmol/L～7mmol/L.
Above-mentioned TiO
2(B)@Bi
20tiO
32in the preparation method of nuclear shell structure nano band photochemical catalyst: the described powder of step (4) is put into Muffle furnace and preferably calcined 2h at 450 ℃.
The present invention adopts simple low-temperature solid phase reaction method, has prepared wide about 100nm-150nm, and length is at tens of TiO to hundreds of micrometer ranges
2(B)@Bi
20tiO
32nuclear shell structure nano band.Because this nanobelt is TiO
2(B)@Bi
20tiO
32nucleocapsid structure, the feature of this nuclear shell structure nano band is that the inside is TiO
2(B), outside is Bi
20tiO
32, be more conducive to the separation of carrier, effectively raise the photocatalysis performance of this nanobelt, make its degradation rate to methyl orange under the ultraviolet radiation of 50min reach 96.89%.
TiO of the present invention
2(B)@Bi
20tiO
32nuclear shell structure nano band is to adopt Na in nanoscale scope
2ti
3o
7for reaction template, by low-temperature solid phase reaction, synthesize.Adopt in this way and can prepare rapidly wide about 100nm-150nm, length is at tens of TiO to hundreds of micrometer ranges
2(B)@Bi
20tiO
32nuclear shell structure nano band.Na in preparation
2ti
3o
7nanobelt, for reaction titanium source, had been both again nanobelt reaction template.Five water bismuth nitrate (Bi (NO
3)
35H
2o) add in distilled water, both generated BiONO
3precipitation, as reaction raw materials, produces again a large amount of H simultaneously
+, for replacing Na
2ti
3o
7in Na
+, kill two birds with one stone.Because this solid phase reaction once completes at low temperatures, and process equipment is simple, gained nanobelt width distribution is narrow, length is controlled, reaction time is short, reproducible, therefore there is vast potential for future development, for solid reaction process is prepared the synthetic route that other titanate nanobelt materials provide a simple possible.
To sum up, the invention has the beneficial effects as follows:
1. the TiO that the inventive method makes
2(B)@Bi
20tiO
32nuclear shell structure nano band, is conducive to the separation of carrier more, effectively raises the photocatalysis performance of this nanobelt.
2. this nanobelt width dimensions narrowly distributing (100nm-150nm), length controlled (at tens of microns between hundreds of micrometer ranges).
3. technique preparation of the present invention is simple, and easy to operate, raw material is easy to get, and preparation cost is lower.
Accompanying drawing explanation
Fig. 1 is TiO prepared by low-temperature solid-phase method
2(B)@Bi
20tiO
32the X-ray diffraction of nanobelt (XRD) collection of illustrative plates.
Fig. 2 is TiO prepared by low-temperature solid-phase method
2(B)@Bi
20tiO
32the field emission scanning electron microscope of nanobelt (FESEM) photo.
Fig. 3 is TiO prepared by low-temperature solid-phase method
2(B)@Bi
20tiO
32the transmission electron microscope of nanobelt (TEM) photo.
Fig. 4 is TiO prepared by low-temperature solid-phase method
2(B)@Bi
20tiO
32nanobelt is the degraded figure to methyl orange under UV-irradiation.
The specific embodiment
Embodiment 1:
1. the nano titanium oxide P25 of 0.3g is dissolved in the NaOH solution of 60ml10M, ultrasonic, stir each 0.5h and pour in hydrothermal reaction kettle, compactedness is controlled at 80%; Then seal hydrothermal reaction kettle, put it in drying box.Hydrothermal temperature is controlled at 200 ℃, and the reaction time is controlled at 72h, after reaction finishes, naturally cools to room temperature, and gained powder rinses repeatedly by deionized water, and then suction filtration, makes Na
2ti
3o
7powder, stand-by.
2. by analytically pure five water bismuth nitrate (Bi (NO
3)
35H
2o) add in distilled water, and constantly stir, be mixed with Bi
3+concentration is the solution of 2.5mmol/L, and gained solution is designated as A solution.
3. to the Na that adds step 1. to prepare in A solution
2ti
3o
7powder, and constantly stir, forming precursor solution, gained solution is designated as B solution.By after the B solution left standstill 48h of preparation, gained powder rinses repeatedly by deionized water, and suction filtration then, by gained powder 60 ℃ of dry 10h in drying box.
4. dried powder is put into Muffle furnace and calcine 2h at 450 ℃, finally cool to room temperature with the furnace, make TiO free from foreign meter
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst.
By the TiO of gained
2(B)@Bi
20tiO
32german Brooker D8X-x ray diffractometer x analytic sample for nanobelt, finds that product is the tetragonal crystal system Bi that JCPDS is numbered 42-0202
20tiO
32(Fig. 1).This sample is observed with field emission scanning electron microscope (Fig. 2) and the Japanese JEOL company's production JEM2100 type transmission electron microscope (Fig. 3) of HITACHI S-4800, from photo, can be found out prepared TiO
2(B)@Bi
20tiO
32the width distribution of nanobelt is narrow, is about 100-150nm; Distribution of lengths wider range, for tens of microns are to hundreds of microns.The nuclear shell structure nano band of preparation is degraded (Fig. 4) to methyl orange under UV-irradiation, and after 50min irradiates, degradation rate can reach 96.89%.
Embodiment 2:
1. the nano titanium oxide P25 of 0.3g is dissolved in the NaOH solution of 60ml10M, ultrasonic, stir each 0.5h and fall back in thermal response still, compactedness is controlled at 70%; Then seal hydrothermal reaction kettle, put it in drying box.Hydrothermal temperature is controlled at 200 ℃, and the reaction time is controlled at 60h, after reaction finishes, naturally cools to room temperature, gained Na
2ti
3o
7powder is stand-by after deionized water is rinsed suction filtration repeatedly.
2. by analytically pure five water bismuth nitrate (Bi (NO
3)
35H
2o) add in distilled water, and constantly stir, be mixed with Bi
3+concentration is the solution of 4mmol/L, and gained solution is designated as A solution.
3. to the Na that adds step 1. to prepare in A solution
2ti
3o
7powder, and constantly stir, forming precursor solution, gained solution is designated as B solution.By after the B solution left standstill 48h of preparation, through deionized water, repeatedly rinse suction filtration, by gained powder 60 ℃ of dry 10h in drying box.
4. dried powder is put into Muffle furnace and calcine 2h at 450 ℃, finally cool to room temperature with the furnace, make TiO free from foreign meter
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst.
Embodiment 3:
1. the nano titanium oxide P25 of 0.3g is dissolved in the NaOH solution of 60ml10M, ultrasonic, stir each 0.5h and fall back in thermal response still, compactedness is controlled at 60%; Then seal hydrothermal reaction kettle, put it in drying box.Hydrothermal temperature is controlled at 200 ℃, and the reaction time is controlled at 48h, after reaction finishes, naturally cools to room temperature, gained Na
2ti
3o
7powder is stand-by after deionized water is rinsed suction filtration repeatedly.
2. by analytically pure five water bismuth nitrate (Bi (NO
3)
35H
2o) add in distilled water, and constantly stir, be mixed with Bi
3+concentration is the solution of 7mmol/L, and gained solution is designated as A solution.
3. to the Na that adds step 1. to prepare in A solution
2ti
3o
7powder, and constantly stir, forming precursor solution, gained solution is designated as B solution.By after the B solution left standstill 48h of preparation, through deionized water, repeatedly rinse suction filtration, by gained powder 60 ℃ of dry 10h in drying box.
4. dried powder is put into Muffle furnace and calcine 2h at 450 ℃, finally cool to room temperature with the furnace, make TiO free from foreign meter
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst.
Claims (4)
1. a TiO
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst, is characterized in that: described photochemical catalyst is that width dimensions is 100nm～150nm, and length is the TiO of 10 μ m～990 μ m
2(B)@Bi
20tiO
32nuclear shell structure nano band, wherein nanobelt the inside is TiO
2(B), outside is Bi
20tiO
32.
2. TiO described in claim 1
2(B)@Bi
20tiO
32the preparation method of nuclear shell structure nano band photochemical catalyst, step is:
(1) the nano titanium oxide P25 of reacting dose is dissolved in the NaOH solution of 10M, ultrasonic, stir each 0.5h and fall back in thermal response still, compactedness is controlled at 60～80% of reactor volume; Then seal hydrothermal reaction kettle, put it in drying box, make hydrothermal temperature be controlled at 200 ± 10 ℃, the reaction time is controlled at 24h～72h, after reaction finishes, naturally cools to room temperature, and gained powder rinses repeatedly by deionized water, and then suction filtration, makes Na
2ti
3o
7powder, stand-by;
(2) by analytically pure five water bismuth nitrate (Bi (NO
3)
35H
2o) add in distilled water, and constantly stir, be mixed with Bi
3+concentration is the suspension of 2.5mmol/L～10mmol/L, and gained solution is designated as A solution;
(3) to Na in molar ratio in A solution
+: Bi
3+the ratio of=1:1 adds above-mentioned Na
2ti
3o
7powder, and constantly stir, forming precursor solution, gained solution is designated as B solution; By after the B solution left standstill 48h of preparation, gained powder rinses repeatedly by deionized water, and then suction filtration, will make powder and be placed in 60 ± 5 ℃ of dry 10～15h of drying box;
(4) the dried powder of step (3) is put into Muffle furnace and calcine 2～3h at 450 ± 10 ℃, then cool to room temperature with the furnace, make TiO free from foreign meter
2(B)@Bi
20tiO
32nuclear shell structure nano band photochemical catalyst.
3. TiO as claimed in claim 2
2(B)@Bi
20tiO
32the preparation method of nuclear shell structure nano band photochemical catalyst, is characterized in that: the described Bi of step (2)
3+concentration is 2.5mmol/L～7mmol/L.
4. TiO as claimed in claim 2
2(B)@Bi
20tiO
32the preparation method of nuclear shell structure nano band photochemical catalyst, is characterized in that: the described powder of step (4) is put into Muffle furnace and calcine 2h at 450 ℃.
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| JP2007290887A (en) * | 2006-04-24 | 2007-11-08 | Fuji Ceramics:Kk | Bismuth titanate-based nanoparticle, piezoelectric ceramic using the same, and methods for producing them |
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| Title |
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| Zhenhuan Zhao et al."UV-visible-light-activated photocatalysts based on Bi2O3/Bi4Ti3O12/TiO2 double-heterostructured TiO2 nanobelts".《Journal of Materials Chemistry》.2012,第22卷全文. |
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