CN105214648A - A kind of exposure { 001}TiO 2/ Bi 2wO 6the preparation method of catalysis material - Google Patents
A kind of exposure { 001}TiO 2/ Bi 2wO 6the preparation method of catalysis material Download PDFInfo
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- CN105214648A CN105214648A CN201510760705.8A CN201510760705A CN105214648A CN 105214648 A CN105214648 A CN 105214648A CN 201510760705 A CN201510760705 A CN 201510760705A CN 105214648 A CN105214648 A CN 105214648A
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Abstract
The invention discloses a kind of exposure { 001}TiO
2/ Bi
2wO
6the preparation method of catalysis material, butyl titanate, hydrofluoric acid and deionized water are stirred in vessel, after adding reactor hydro-thermal reaction hour, deionized water is repeatedly cleaned post-drying and is obtained { the TiO in 001} face
2; Bismuth nitrate and sodium tungstate are added middle stirring, in the process of stirring, slowly instills red fuming nitric acid (RFNA), continue to stir, form white Bi
2wO
6suspension; Suspension is added the { TiO in 001} face prepared
2, add reactor hydro-thermal reaction after magnetic agitation, repeatedly clean by deionized water and obtain TiO
2/ Bi
2wO
6composite; By the TiO of preparation
2/ Bi
2wO
6composite is being calcined, { the TiO in 001} face needed for namely obtaining
2/ Bi
2wO
6photochemical catalyst.The present invention adopts hydro-thermal method to prepare the { TiO in 001} face
2/ Bi
2wO
6composite, makes full use of the Uv and visible light part of sunshine in light-catalysed process, in addition, and TiO
2/ Bi
2wO
6form semiconductor heterostructure, can effective separate electronic-hole pair, oxidation-reduction quality is provided, reduces its probability of recombination, thus improve its photocatalytic activity.
Description
Technical field
The present invention relates to a kind of nano photo catalyzed oxidation, in particular a kind of exposure { 001}TiO
2/ Bi
2wO
6the preparation method of catalysis material.
Background technology
Nano-TiO
2be a kind of N-type semiconductor material, because it has, nontoxic, physics and chemistry stability is strong, catalytic activity high, has huge application prospect in the organic pollutant in the photocatalytic degradation aqueous solution.But, TiO
2normally with stable, { form of 101} exposure exists, and the recombination rate of its higher electron-hole pair inhibits its photocatalysis performance.
Inorganic pollution in industrial wastewater mainly contains heavy metal ion, as the ion of Hg, Cr, Pb etc.Large quantifier elimination shows, many inorganic matters are at TiO
2surface has photocatalytic activity.Cr6+ concentration be 80mg/L, volume is in the waste water of 100mL, adds 0.7gSiO
2-TiO
2be glass as photochemical catalyst, the clearance of illumination reaction system 3h, Cr6+ reaches 99.9%.
Active high { the TiO in 001} face of preparation
2can improve its photocatalysis performance in UV light region, but in the process utilizing sunshine, ultraviolet light only accounts for about 5% of total light intensity, accounts for the most visible light part of light intensity and is not fully utilized.Bi
2wO
6that there is visible light-responded semiconductor light-catalyst.In addition, Bi in the process of illumination
2wO
6also there is the problem that electron-hole pair recombination rate is high.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of exposure { 001}TiO
2/ Bi
2wO
6the preparation method of catalysis material, improve its photocatalytic activity.
The present invention is achieved by the following technical solutions, and the present invention (1) is by after butyl titanate, hydrofluoric acid and deionized water and stirring, and after adding reactor hydro-thermal reaction, deionized water is repeatedly cleaned post-drying and obtained { the TiO in 001} face
2;
(2) bismuth nitrate and sodium tungstate are added deionized water for stirring, in the process of stirring, slowly instill red fuming nitric acid (RFNA), continue to stir, form white Bi
2wO
6suspension;
(3) suspension of step (2) is added the preparation-obtained { TiO in 001} face of step (1)
2, after adding reactor hydro-thermal reaction after magnetic agitation, repeatedly clean by deionized water and obtain TiO
2/ Bi
2wO
6composite;
(4) by the TiO prepared by step (3)
2/ Bi
2wO
6composite calcines 2 ~ 4h at 300 ~ 400 DEG C, { the TiO in 001} face needed for namely obtaining
2/ Bi
2wO
6photochemical catalyst.
As one of preferred embodiment of the present invention, in described step (1), after stirring 8 ~ 15min after the 25:6:9 mixing by volume of butyl titanate, hydrofluoric acid and deionized water in vessel, hydro-thermal reaction is after 20 ~ 30 hours at 150 ~ 250 DEG C to add reactor, and deionized water is repeatedly cleaned post-drying and obtained { the TiO in 001} face
2.
As one of preferred embodiment of the present invention, in described step (1), butyl titanate, hydrofluoric acid and deionized water stir in plastic ware.Avoid hydrofluoric acid etching glass vessel.
As one of preferred embodiment of the present invention, in described step (2), bismuth nitrate and sodium tungstate in molar ratio 2:1 add 100ml deionized water, and the amount adding the concentrated sulfuric acid is 1ml.
As one of preferred embodiment of the present invention, in described step (2), the stir speed (S.S.) 1000 turns/min of bismuth nitrate and sodium tungstate.
As one of preferred embodiment of the present invention, in described step (3), after magnetic agitation 8 ~ 15min, add reactor hydro-thermal reaction 15 ~ 25 hours at 150 ~ 200 DEG C.
As one of preferred embodiment of the present invention, in described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 5 ~ 1:1, obtain the TiO of different mol ratio
2/ Bi
2wO
6composite.
In described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 5:1.
In described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 2:1.
In described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 1:1.
The present invention has the following advantages compared to existing technology: the present invention adopts hydro-thermal method to prepare the { TiO in 001} face
2/ Bi
2wO
6composite, makes full use of the Uv and visible light part of sunshine in light-catalysed process, in addition, and TiO
2/ Bi
2wO
6form semiconductor heterostructure, can effective separate electronic-hole pair, oxidation-reduction quality is provided, reduces its probability of recombination, thus improve its photocatalytic activity.
Accompanying drawing explanation
Fig. 1 is preparation { 001} face TiO
2and TiO
2/ Bi
2wO
6the XRD figure of composite;
Fig. 2 is preparation { 001} face TiO
2and TiO
2/ Bi
2wO
6sEM figure and the TEM figure of composite;
Fig. 3 is TiO
2/ Bi
2wO
6for the composite of 5:1 and commercial P25 are to the photocatalysis result schematic diagram of methyl orange solution.
Detailed description of the invention
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment utilizes hydro-thermal method to prepare the { TiO in 001} face
2/ Bi
2wO
6photochemical catalyst, detailed process is as follows:
(1) by the deionized water (H of the butyl titanate (C16H36O4Ti) of 25ml, the hydrofluoric acid (HF) of 6ml and 9ml
2o), after stirring 10min in plastic ware, hydro-thermal reaction is after 24 hours at 200 DEG C for the reactor adding 50ml, and deionized water is repeatedly cleaned post-drying and obtained { the TiO in 001} face
2;
(2) by the bismuth nitrate (Bi (NO of 6mmol
3)
35H
2and the sodium tungstate (Na of 3mmol O)
2wO
42H
2o) add the deionized water for stirring (stir speed (S.S.) 1000 turns/min) of 100ml, in the process of stirring, slowly instill 1ml red fuming nitric acid (RFNA) (HNO
3), continue stirring 2 hours, form white suspension;
(3) get the white suspension that the step (2) of 1/3 volume is obtained, add { the TiO in 001} face of 5mmol prepared by step (1)
2, the reactor hydro-thermal reaction at 180 DEG C adding 50ml after magnetic agitation 10min, after 20 hours, is repeatedly cleaned by deionized water and is obtained TiO
2/ Bi
2wO
6composite;
(4) by the TiO prepared by step (3)
2/ Bi
2wO
6composite calcines 2 ~ 4h at 300 ~ 400 DEG C, { the TiO in 001} face needed for namely obtaining
2/ Bi
2wO
6photochemical catalyst.
Embodiment 2
In the present embodiment, in step (3), get the white suspension that the step (2) of 1/3 volume is obtained, add { the TiO in 001} face of 2mmol prepared by step (1)
2, the reactor hydro-thermal reaction at 180 DEG C adding 50ml after magnetic agitation 10min, after 20 hours, is repeatedly cleaned by deionized water and is obtained TiO
2/ Bi
2wO
6composite.
Other embodiments are identical with embodiment 1.
Embodiment 3
In the present embodiment, in step (3), get the white suspension that the step (2) of 1/3 volume is obtained, add { the TiO in 001} face of 1mmol prepared by step (1)
2, the reactor hydro-thermal reaction at 180 DEG C adding 50ml after magnetic agitation 10min, after 20 hours, is repeatedly cleaned by deionized water and is obtained TiO
2/ Bi
2wO
6composite.
Other embodiments are identical with embodiment 1.
Photochemical catalyst obtained for above-described embodiment 1 ~ 3 is carried out XRD detection, and as shown in Figure 1, wherein (a) is pure { 001} face TiO to result
2; (b) TiO
2: Bi
2wO
6=5:1 (mol ratio); (c) TiO
2: Bi
2wO
6=2:1 (mol ratio); (d) TiO
2: Bi
2wO
6=1:1 (mol ratio); (e) Bi
2wO
6.
Photochemical catalyst obtained for above-described embodiment 1 ~ 3 is carried out SEM and TEM detect, as shown in Figure 2, (a) is { 001} face TiO
2, as can be seen from the figure, sample is the flake that size is about 100nm; (b) and (c) TiO
2: Bi
2wO
6be respectively SEM figure (mol ratio) of 5:1 and 2:1; As can be seen from the figure along with Bi
2wO
6the increase of ratio, TiO
2be assembled into TiO together
2/ Bi
2wO
6nano flower; D () is TiO
2/ Bi
2wO
6the TEM figure of composite, can find out and define heterojunction structure.
Fig. 3 is the TiO2:Bi2WO6 that photocatalysis efficiency is the highest is the TiO of 5:1
2/ Bi
2wO
6composite and commercial P25 are to the photocatalysis result of methyl orange solution.As can be seen from the results, through half an hour darkroom adsorption experiment, two kinds of samples all can be ignored to the absorption of methyl orange, through the photocatalysis experiment of 90 minutes, and TiO
2/ Bi
2wO
699.1% and 67.5% is respectively with the photocatalysis efficiency of P25.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. an exposure { 001}TiO
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, comprise the following steps:
(1), by after butyl titanate, hydrofluoric acid and deionized water and stirring, after adding reactor hydro-thermal reaction, deionized water is repeatedly cleaned post-drying and is obtained { the TiO in 001} face
2;
(2) bismuth nitrate and sodium tungstate are added deionized water for stirring, in the process of stirring, slowly instill red fuming nitric acid (RFNA), continue to stir, form white Bi
2wO
6suspension;
(3) suspension of step (2) is added the preparation-obtained { TiO in 001} face of step (1)
2, after adding reactor hydro-thermal reaction after magnetic agitation, repeatedly clean by deionized water and obtain TiO
2/ Bi
2wO
6composite;
(4) by the TiO prepared by step (3)
2/ Bi
2wO
6composite calcines 2 ~ 4h at 300 ~ 400 DEG C, { the TiO in 001} face needed for namely obtaining
2/ Bi
2wO
6photochemical catalyst.
2. a kind of exposure { 001}TiO according to claim 1
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (1), after stirring 8 ~ 15min after the 25:6:9 mixing by volume of butyl titanate, hydrofluoric acid and deionized water in vessel, hydro-thermal reaction is after 20 ~ 30 hours at 150 ~ 250 DEG C to add reactor, and deionized water is repeatedly cleaned post-drying and obtained { the TiO in 001} face
2.
3. a kind of exposure { 001}TiO according to claim 1
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (1), butyl titanate, hydrofluoric acid and deionized water stir in plastic ware.
4. a kind of exposure { 001}TiO according to claim 1
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (2), bismuth nitrate and sodium tungstate in molar ratio 2:1 add 100ml deionized water, and the amount adding the concentrated sulfuric acid is 1ml.
5. a kind of exposure { 001}TiO according to claim 1
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (2), the stir speed (S.S.) 1000 turns/min of bismuth nitrate and sodium tungstate.
6. a kind of exposure { 001}TiO according to claim 1
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (3), after magnetic agitation 8 ~ 15min, add reactor hydro-thermal reaction 15 ~ 25 hours at 150 ~ 200 DEG C.
7. a kind of exposure { 001}TiO according to claim 1
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 5 ~ 1:1, obtain the TiO of different mol ratio
2/ Bi
2wO
6composite.
8. a kind of exposure { 001}TiO according to claim 5
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 5:1.
9. a kind of exposure { 001}TiO according to claim 5
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 2:1.
10. a kind of exposure { 001}TiO according to claim 5
2/ Bi
2wO
6the preparation method of catalysis material, it is characterized in that, in described step (3), { TiO in 001} face obtained by step (1)
2with the Bi of step (2)
2wO
6mix according to mol ratio 1:1.
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Cited By (2)
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| CN106984312A (en) * | 2017-04-24 | 2017-07-28 | 福州大学 | A kind of composite photocatalyst and preparation method thereof |
| CN116726908A (en) * | 2023-08-14 | 2023-09-12 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Bismuth-doped high-performance electrocatalytic composite material, preparation method and application |
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| CN116726908B (en) * | 2023-08-14 | 2023-11-10 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Bismuth-doped high-performance electrocatalytic composite material, preparation method and application |
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