CN105148902A - Cavity core-shell structured TiO2/WO3 composite photocatalyst and preparation method therefor and application thereof - Google Patents

Cavity core-shell structured TiO2/WO3 composite photocatalyst and preparation method therefor and application thereof Download PDF

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CN105148902A
CN105148902A CN201510437556.1A CN201510437556A CN105148902A CN 105148902 A CN105148902 A CN 105148902A CN 201510437556 A CN201510437556 A CN 201510437556A CN 105148902 A CN105148902 A CN 105148902A
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catalyst
cavity
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CN105148902B (en
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朱建
李丹
孙兆毅
陆景鹏
李和兴
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Shanghai Normal University
University of Shanghai for Science and Technology
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Abstract

The invention relates to a preparation method for a cavity core-shell structured TiO2/WO3 composite photocatalyst. The preparation method comprises the following steps: (1) dissolving TiCl4 in a mixed alcohol solution so as to obtain a solution A; dissolving WCl6 in ethanol so as to obtain a solution B; and then mixing the solution A and the solution B so as to prepare a raw material solution; and (2) transferring the raw material solution into a polytetrafluoroethylene lined hydrothermal kettle, controlling reaction temperature and time, and carrying out centrifuge washing, thereby preparing the cavity core-shell structured TiO2/WO3 composite photocatalyst. According to the preparation method, the cavity core-shell structured TiO2/WO3 composite photocatalyst can be prepared through changing ingredients of the raw material solution, solvothermal time and temperature based on a solvothermal method. According to the preparation method, the cavity core-shell structured TiO2/WO3 composite photocatalyst is prepared by adopting a one-pot method; and the preparation method does not need a hard template agent, is simple and convenient and is high in controllability. The TiO2/WO3 can be applied to the photocatalytic degradation of indoor pollutant acetaldehyde.

Description

Cavity nucleocapsid structure TiO 2/ WO 3composite photo-catalyst and Synthesis and applications thereof
Technical field
The invention belongs to TiO 2/ WO 3composite photocatalyst material technical field, particularly one adopts one kettle way to prepare cavity nucleocapsid structure TiO 2/ WO 3the method of composite photo-catalyst.
Background technology
In recent years, world wide environment pollution problem is particularly outstanding, in outdoor, more serious with the PM2.5 that in the processes such as daily generating, industrial production, motor vehicle exhaust emission, the residue of discharge is main source through burning.In indoor, the pollution brought due to finishing problem of constantly purchasing house is also very violent, finishing material is nothing more than employing artificial board, filled board, glue, paint, coating, adhesive, granite, marble, ceramic tile and gypsum etc., these materials are more or less all containing the four kinds of pollutants such as formaldehyde, benzene, ammonia, radon do not waited, and the finishing material of no pollution is non-existent.So-called national environmental protection material, just above-mentioned pollutant is within national allowed band.According to the relevent statistics, newly-decorated house air detection qualification rate is very low.Utilizing photocatalysis technology to purify can be harmless carbon dioxide and water by organic pollution decomposition and inversion effectively, reduces room air pollution, convenient and swift, thus is being subject to extensive concern in recent years.
Semiconductor light-catalyst titanium dioxide abundance, nontoxic, but only have ultraviolet catalytic active, tungstic acid band-gap energy is 2.5-2.8eV, can catch the solar spectrum of about 1 12, comprise the visible ray of nearly 500nm.TiO 2/ WO 3composite effectively can improve the separative efficiency of electron-hole pair, expands the absorption region to sunshine.Meanwhile, cavity nucleocapsid structure has the multipath effect to light, effectively can improve the utilization rate to luminous energy.Synthesis has cavity nucleocapsid structure TiO 2/ WO 3composite has potential photocatalytic applications prospect.
At present, nucleocapsid structure is applied comparatively wide in nano-catalytic, and it is large that catalyst with core-casing structure has specific area, can improve the advantage of the utilization rate of light in photocatalysis technology.But it is comparatively complicated to prepare the method that nucleocapsid structure composite photocatalyst generally adopts, mostly be two-step method preparation, first a kind of catalyst is prepared then by dipping, the methods such as photoelectricity deposition adhere to the second catalyst again, cavity structure is generally obtained in conjunction with lithographic technique by template, and program is comparatively loaded down with trivial details.
Summary of the invention
The object of the present invention is to provide a kind of cavity nucleocapsid structure TiO 2/ WO 3the preparation method of composite photo-catalyst, comprises the steps:
(1) by TiCl 4be dissolved in mixed alcohol solution and obtain solution A; By WCl 6be dissolved in ethanol and obtain solution B; Then by solution A and solution B mix and blend 0.5-1.0 hour, obtained material liquid;
(2) material liquid is transferred to polytetrafluoroethylene (PTFE) be liner water heating kettle in, control reaction temperature at 120-200 DEG C of reaction time 12-72h, be cooled to room temperature, obtained cavity nucleocapsid structure TiO after centrifuge washing 2/ WO 3composite photo-catalyst.
Mixed alcohol solution in described step (1) is 1-9:1 mixing by the tert-butyl alcohol, ethylene glycol by volume; Preferably, the tert-butyl alcohol, ethylene glycol are 1-3:1 mixing by volume.
TiCl in described step (1) 4molar concentration in mixed alcohol solution is 0.01-0.15mol/L; Preferably, described TiCl 4molar concentration in mixed alcohol solution is 0.03-0.13mol/L.
WCl in described step (1) 6and TiCl 4mol ratio be 1-10:1.
WCl in described step (1) 6molar concentration is in ethanol 0.025-0.15mol/L; Preferably, described WCl 6molar concentration is in ethanol 0.05-0.12mol/L.
Material liquid in described step (2) accounts for more than 80% of water heating kettle volume.
Reaction temperature in described step (2) is 160 DEG C, reaction time 48h.
Another object of the present invention is to provide a kind of cavity nucleocapsid structure TiO 2/ WO 3composite photo-catalyst, the particle diameter of the catalyst obtained by said method is 1-2um, cavity diameter is 150-200nm, nucleocapsid pattern outer surface homoepitaxial the nano whiskers structure of granule attachment (granule is Ti, W), Ti, W element is evenly distributed in catalyst structure, and the specific area of catalyst reaches 138-203m 2/ g.
Another object of the present invention is to provide described cavity nucleocapsid structure TiO 2/ WO 3the application of composite photo-catalyst in the photocatalytic degradation of indoor pollutant acetaldehyde.
Compared with prior art, good effect of the present invention is as follows:
The present invention is based on solvent thermal process, cavity nucleocapsid structure TiO can be prepared by feed change fluid component, solvent heat time and temperature 2/ WO 3composite photo-catalyst.The present invention prepares cavity nucleocapsid structure TiO by adopting one kettle way 2/ WO 3composite photo-catalyst, this preparation method without the need to hard mould agent, simple and efficient, controllability is strong.Prepare gained TiO 2/ WO 3composite photo-catalyst has larger specific area, Stability Analysis of Structures, and photo-generate electron-hole separative efficiency is high, and photocatalytic-oxidation voltinism is strong, can be applied to the photocatalytic degradation of indoor pollutant acetaldehyde.
Accompanying drawing explanation
The x-ray crystallography of catalyst sample (a) prepared by Fig. 1 embodiment 2 and roasting 3h rear catalyst (b) in 550 DEG C of Muffle furnaces;
The scanning electron microscope diagram (a) of Fig. 2 embodiment 2 sample and transmission electron microscope figure (b); The scanning electron microscope diagram (c) of embodiment 3 sample; The scanning electron microscope diagram (d) of embodiment 5 sample
Nitrogen adsorption desorption isothermal curve (a) of Fig. 3 embodiment 2 sample and graph of pore diameter distribution (b);
Fig. 4 embodiment 2,3,5 samples are to the Photocatalytic activity figure of acetaldehyde.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 20mL tert-butyl alcohol, in 20mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Test result: prepared catalyst pattern is the nucleocapsid structure with cavity, the short grained acicular texture of spherical outer surface growth attachment, nuclear shell ball particle diameter is about 1-2um, and cavity diameter is about 200nm, and catalyst specific surface is about 189m 2/ g, pattern is more homogeneous.
Embodiment 2
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Test result: by the test of SEM and TEM collection of illustrative plates, finds that catalyst pattern is the nucleocapsid structure with cavity, and the short grained acicular texture of spherical outer surface growth attachment, nuclear shell ball particle diameter is about 1-2um, and cavity diameter is about 200nm, and catalyst specific surface is about 203m 2/ g, pattern is more homogeneous.
Embodiment 3
Under water bath condition, the titanium tetrachloride of 280uL (2.54mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 0.5g tungsten hexachloride (1.26mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Test result: observed by SEM (SEM), catalyst is the spherical structure with nucleocapsid, outer surface is granule attachment, and catalyst specific surface is about 165m 2/ g acicular texture disappears.
Embodiment 4
Under water bath condition, the titanium tetrachloride of 560uL (5.08mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Test result: tested by SEM, finds that catalyst pattern is the nucleocapsid structure with cavity, and the short grained acicular texture of spherical outer surface growth attachment, nuclear shell ball particle diameter is about 1-2um, and cavity diameter is about 190nm, and catalyst specific surface is about 138m 2/ g.
Embodiment 5
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 0.5g tungsten hexachloride (1.26mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Test result: prepared catalyst pattern is the nucleocapsid structure with cavity, spherical outer surface growth attachment granule.
Embodiment 6
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 2.0g tungsten hexachloride (5.04mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Embodiment 7
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 0.5g tungsten hexachloride (1.26mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle (accounting for kettle long-pending about 90%), naturally cool to room temperature after keeping 48h at 160 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Embodiment 8
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 72h at 120 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Embodiment 9
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 60h at 140 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Embodiment 10
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 36h at 180 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Embodiment 11
Under water bath condition, the titanium tetrachloride of 140uL (1.27mmol) is joined the 30mL tert-butyl alcohol, in 10mL ethylene glycol, vigorous stirring dissolves formation clear solution completely to titanium tetrachloride, 1.0g tungsten hexachloride (2.52mmol) is dissolved in 50mL absolute ethyl alcohol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettle and (account for kettle long-pending about 90%), naturally cool to room temperature after keeping 12h at 200 DEG C, after centrifuge washing, namely obtain cavity nucleocapsid structure TiO 2/ WO 3composite photocatalyst.
Application Example
Photochemical catalytic oxidation acetaldehyde reacts
To take after synthesis 550 DEG C of roasting 3h, the catalyst 50mg prepared by embodiment 1-13 in Muffle furnace, use 1000 ± 10ppm, 5uL acetaldehyde as analog gas.Open xenon source, carry out Photocatalytic Degradation Process, within every 15 minutes, gather a gaseous sample, carry out content analysis by gas-chromatography.Carry out content analysis to collection gas after 1.0 hours, analysis result is as shown in table 1:
Table 1
Embodiment Acetaldehyde clearance (%) Embodiment Acetaldehyde clearance (%)
1 89 7 48
2 92 8 33
3 40 9 41
4 78 10 38
5 45 11 46
6 62
Blank 2
Tested by the photooxidative degradation of acetaldehyde, result shows, the hud typed photocatalyst surface structure with cavity structure is larger on photocatalysis effect impact, when the acicular texture of spherical outer surface growth attaching particles, degrading activity is optimum, be such a structure increases light multiple reflections utilization rate on a catalyst on the one hand, acicular texture may because the existence of Ti, W hetero-junctions improves the separative efficiency of photo-generate electron-hole on the one hand in addition.
Although preferred embodiment discloses as above by the present invention; so itself and be not used to limit content of the present invention; anyly be familiar with this those skilled in the art; not departing from main spirits of the present invention and context; when doing various change and retouching, the protection domain therefore invented should be as the criterion with the basic right claimed range applied for a patent.

Claims (10)

1. a cavity nucleocapsid structure TiO 2/ WO 3the preparation method of composite photo-catalyst, comprises the steps:
(1) by TiCl 4be dissolved in mixed alcohol solution and obtain solution A; By WCl 6be dissolved in ethanol and obtain solution B; Then by solution A and solution B mix and blend 0.5-1.0 hour, obtained material liquid;
(2) material liquid is transferred to polytetrafluoroethylene (PTFE) be liner water heating kettle in, control reaction temperature 120-200 DEG C of reaction time 12-72h, be cooled to room temperature, obtained cavity nucleocapsid structure TiO after centrifuge washing 2/ WO 3composite photo-catalyst.
2. preparation method according to claim 1, is characterized in that: the mixed alcohol solution in described step (1) is 1-9:1 mixing by the tert-butyl alcohol, ethylene glycol by volume.
3. preparation method according to claim 2, is characterized in that: the mixed alcohol solution in described step (1) is 1-3:1 mixing by the tert-butyl alcohol, ethylene glycol by volume.
4. preparation method according to claim 1, is characterized in that: the TiCl in described step (1) 4molar concentration in mixed alcohol solution is 0.01-0.15mol/L.
5. preparation method according to claim 1, is characterized in that: the WCl in described step (1) 6and TiCl 4mol ratio be 1-10:1.
6. preparation method according to claim 1, is characterized in that: the WCl in described step (1) 6molar concentration is in ethanol 0.025-0.15mol/L.
7. preparation method according to claim 1, is characterized in that: the material liquid in described step (2) accounts for more than 80% of water heating kettle volume.
8. preparation method according to claim 1, is characterized in that: the reaction temperature in described step (2) is 160 DEG C.
9. a cavity nucleocapsid structure TiO 2/ WO 3composite photo-catalyst, obtained by the method preparation described in any one of claim 1-8, the particle diameter of described catalyst is 1-2um, cavity diameter is 150-200nm, nucleocapsid pattern outer surface homoepitaxial the nano whiskers structure of granule attachment, Ti, W element is evenly distributed in catalyst structure, and the specific area of catalyst reaches 138-203m 2/ g.
10. cavity nucleocapsid structure TiO according to claim 9 2/ WO 3the application of composite photo-catalyst in the photocatalytic degradation of indoor pollutant acetaldehyde.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106166498A (en) * 2016-06-20 2016-11-30 同济大学 A kind of nanometer WO3/ TiO2the preparation method of ferrum modified zeolite composite photo-catalyst
CN106311216A (en) * 2016-08-16 2017-01-11 天津大学 Composite photocatalyst with two-dimensional material as oxygen production cocatalyst and preparation method of composite photocatalyst
CN108722394A (en) * 2018-05-25 2018-11-02 东北大学 WO with yolk-eggshell structure3-TiO2Nanocomposite and preparation method thereof
CN110013863A (en) * 2019-03-26 2019-07-16 桂林理工大学 One step solvent-thermal process CuS-WO of one kind3The preparation method of composite material
CN110215925A (en) * 2019-06-09 2019-09-10 桂林理工大学 A kind of homogeneous one-step synthesis CdS-WO3The method of composite material

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106166498A (en) * 2016-06-20 2016-11-30 同济大学 A kind of nanometer WO3/ TiO2the preparation method of ferrum modified zeolite composite photo-catalyst
CN106311216A (en) * 2016-08-16 2017-01-11 天津大学 Composite photocatalyst with two-dimensional material as oxygen production cocatalyst and preparation method of composite photocatalyst
CN108722394A (en) * 2018-05-25 2018-11-02 东北大学 WO with yolk-eggshell structure3-TiO2Nanocomposite and preparation method thereof
CN110013863A (en) * 2019-03-26 2019-07-16 桂林理工大学 One step solvent-thermal process CuS-WO of one kind3The preparation method of composite material
CN110013863B (en) * 2019-03-26 2021-11-16 桂林理工大学 One-step solvothermal synthesis of CuS-WO3Method for preparing composite material
CN110215925A (en) * 2019-06-09 2019-09-10 桂林理工大学 A kind of homogeneous one-step synthesis CdS-WO3The method of composite material
CN110215925B (en) * 2019-06-09 2022-03-22 桂林理工大学 Homogeneous one-step synthesis of CdS-WO3Method for compounding materials

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