CN105148902B - Cavity core shell structure TiO2/WO3Composite photo-catalyst and its preparation and application - Google Patents
Cavity core shell structure TiO2/WO3Composite photo-catalyst and its preparation and application Download PDFInfo
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- CN105148902B CN105148902B CN201510437556.1A CN201510437556A CN105148902B CN 105148902 B CN105148902 B CN 105148902B CN 201510437556 A CN201510437556 A CN 201510437556A CN 105148902 B CN105148902 B CN 105148902B
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Abstract
The present invention relates to a kind of cavity core shell structure TiO2/WO3The preparation method of composite photo-catalyst, comprises the following steps：(1) by TiCl4It is dissolved in mixing alcoholic solution and obtains solution A；By WCl6It is dissolved in ethanol and obtains solution B；Then solution A and solution B are mixed to prepare material liquid；(2) material liquid is transferred to using polytetrafluoroethylene (PTFE) in the water heating kettle of liner, controlling reaction temperature and time, cavity core shell structure TiO to be made after centrifuge washing2/WO3Composite photo-catalyst.The present invention is based on solvent thermal process, and cavity core shell structure TiO can be prepared by feed change liquid component, solvent heat time and temperature2/WO3Composite photo-catalyst.The present invention prepares cavity core shell structure TiO by using one kettle way2/WO3Composite photo-catalyst, the preparation method is without hard mould agent, simple and efficient, controllability is strong.The TiO2/WO3It can be applied to the photocatalytic degradation of indoor pollutant acetaldehyde.
Description
Technical field
The invention belongs to TiO2/WO3Composite photocatalyst material technical field, it is more particularly to a kind of that sky is prepared using one kettle way
Chamber core shell structure TiO2/WO3The method of composite photo-catalyst.
Background technology
In recent years, world wide environment pollution is particularly problematic, in outdoor, with daily generating, industrial production, automobile
The residue discharged during exhaust emissions etc. by burning is more serious for the PM 2.5 of main source.Indoors, due to
Constantly the pollution that brings of house-purchase finishing problem also very acutely, finishing material nothing more than using artificial board, filled board, glue, paint,
Coating, adhesive, granite, marble, ceramic tile and gypsum etc., these materials more or less containing not wait formaldehyde, benzene,
Four kinds of pollutants such as ammonia, radon, the finishing material of no pollution are not present.So-called national environmental protection material, simply above-mentioned pollution
Thing is within national allowed band.According to the relevent statistics, newly-decorated house air detection qualification rate is very low.Utilize photocatalysis skill
Organic pollution decomposition and inversion can be effectively harmless carbon dioxide and water by art purification, reduce room air pollution, side
Just it is quick, so as to receive significant attention in recent years.
Semiconductor light-catalyst titanium dioxide abundance, it is nontoxic, but only ultraviolet catalytic activity, tungstic acid band gap
It can be 2.5-2.8eV, about 1 12 solar spectrum can be captured, include nearly 500nm visible ray.TiO2/WO3It is compound
Material can effectively improve the separative efficiency of electron-hole pair, expand the absorption region to sunshine.Meanwhile cavity nucleocapsid knot
Structure has the multipath effect to light, can effectively improve the utilization rate to luminous energy.Synthesis has cavity core shell structure TiO2/WO3
Composite has potential photocatalytic applications prospect.
At present, core shell structure is using relatively wide in nano-catalytic, and catalyst with core-casing structure has that specific surface area is big, Neng Gouti
In high photocatalysis technology the advantages of the utilization rate of light.But prepare method that core shell structure composite photocatalyst typically uses compared with
The methods of for complexity, mostly prepared by two-step method, prepares a kind of catalyst first and then by dipping, and photoelectricity deposits adheres to the again
Two kinds of catalyst, cavity structure are typically obtained by template combination lithographic technique, and program is relatively complicated.
The content of the invention
It is an object of the invention to provide a kind of cavity core shell structure TiO2/WO3The preparation method of composite photo-catalyst, bag
Include following steps：
(1) by TiCl4It is dissolved in mixing alcoholic solution and obtains solution A；By WCl6It is dissolved in ethanol and obtains solution B；Then
Solution A and solution B are mixed into 0.5-1.0 hours, material liquid is made；
(2) material liquid is transferred to using polytetrafluoroethylene (PTFE) as in the water heating kettle of liner, controlling reaction temperature is at 120-200 DEG C
Reaction time 12-72h, is cooled to room temperature, and cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photo-catalyst.
Mixing alcoholic solution in the step (1) is 1-9 by volume by the tert-butyl alcohol, ethylene glycol:1 mixing；Preferably, uncle
Butanol, ethylene glycol are 1-3 by volume:1 mixing.
TiCl in the step (1)4Molar concentration in alcoholic solution is mixed is 0.01-0.15mol/L；Preferably,
The TiCl4Molar concentration in alcoholic solution is mixed is 0.03-0.13mol/L.
WCl in the step (1)6And TiCl4Mol ratio be 1-10:1.
WCl in the step (1)6Molar concentration in ethanol is 0.025-0.15mol/L；Preferably, the WCl6
Molar concentration in ethanol is 0.05-0.12mol/L.
Material liquid in the step (2) accounts for more than the 80% of water heating kettle volume.
Reaction temperature in the step (2) is 160 DEG C, reaction time 48h.
Another object of the present invention is to provide a kind of cavity core shell structure TiO2/WO3Composite photo-catalyst, by above-mentioned
The particle diameter of catalyst made from method is 1-2um, and cavity diameter 150-200nm, nucleocapsid pattern outer surface homoepitaxial small
The nano whiskers structure of particle attachment (little particle Ti, W), Ti, W element are evenly distributed in catalyst structure, catalyst
Specific surface area reaches 138-203m2/g。
It is still another object of the present invention to provide the cavity core shell structure TiO2/WO3Composite photo-catalyst pollutes indoors
Application in the photocatalytic degradation of thing acetaldehyde.
Compared with prior art, the positive effect of the present invention is as follows：
The present invention is based on solvent thermal process, and cavity core can be prepared by feed change liquid component, solvent heat time and temperature
Shell structure TiO2/WO3Composite photo-catalyst.The present invention prepares cavity core shell structure TiO by using one kettle way2/WO3Complex light
Catalyst, the preparation method is without hard mould agent, simple and efficient, controllability is strong.Prepare gained TiO2/WO3Composite photo-catalyst has
There is larger specific surface area, Stability Analysis of Structures, photo-generate electron-hole separative efficiency is high, and photochemical catalytic oxidation is strong, can be applied to
The photocatalytic degradation of indoor pollutant acetaldehyde.
Brief description of the drawings
Catalyst sample (a) prepared by Fig. 1 embodiments 2 and the x- through 550 DEG C of Muffle kiln roasting 3h rear catalysts (b) are penetrated
Line crystallogram；
The scanning electron microscope diagram (a) and transmission electron microscope figure (b) of the sample of Fig. 2 embodiments 2；The sample of embodiment 3
Scanning electron microscope diagram (c)；The scanning electron microscope diagram (d) of the sample of embodiment 5
The nitrogen adsorption desorption isothermal curve (a) and graph of pore diameter distribution (b) of the sample of Fig. 3 embodiments 2；
Photocatalytic activity figure of the sample of Fig. 4 embodiments 2,3,5 to acetaldehyde.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 20mL tert-butyl alcohols, in 20mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Test result：Prepared catalyst pattern is the core shell structure with cavity, and spherical outer surface growth adheres to small
The acicular texture of grain, nuclear shell ball particle diameter about 1-2um, cavity diameter about 200nm, catalyst specific surface about 189m2/ g, pattern are more equal
One.
Embodiment 2
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Test result：Tested by SEM and TEM collection of illustrative plates, it is found that catalyst pattern is the core shell structure with cavity, it is spherical
Short grained acicular texture, nuclear shell ball particle diameter about 1-2um, cavity diameter about 200nm, catalyst specific surface are adhered in outer surface growth
About 203m2/ g, pattern are more uniform.
Embodiment 3
Under water bath condition, 280uL (2.54mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 0.5g tungsten hexachlorides (1.26mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Test result：Observed by SEM (SEM), catalyst is the spherical structure with nucleocapsid, appearance
Face is adhered to for little particle, and catalyst specific surface is about 165m2/ g acicular textures disappear.
Embodiment 4
Under water bath condition, 560uL (5.08mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Test result：Tested by SEM, it is the core shell structure with cavity to find catalyst pattern, and spherical outer surface is given birth to
The long short grained acicular texture of attachment, nuclear shell ball particle diameter about 1-2um, cavity diameter about 190nm, catalyst specific surface are about
138m2/g。
Embodiment 5
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 0.5g tungsten hexachlorides (1.26mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Test result：Prepared catalyst pattern is the core shell structure with cavity, and spherical outer surface growth adheres to small
Grain.
Embodiment 6
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 2.0g tungsten hexachlorides (5.04mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Embodiment 7
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 0.5g tungsten hexachlorides (1.26mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles (accounting for kettle product about 90%), in 160 DEG C of guarantors
Room temperature is naturally cooled to after holding 48h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Embodiment 8
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 120 DEG C of guarantors
Room temperature is naturally cooled to after holding 72h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Embodiment 9
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 140 DEG C of guarantors
Room temperature is naturally cooled to after holding 60h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Embodiment 10
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 180 DEG C of guarantors
Room temperature is naturally cooled to after holding 36h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Embodiment 11
Under water bath condition, 140uL (1.27mmol) titanium tetrachloride is added to the 30mL tert-butyl alcohols, in 10mL ethylene glycol,
It is stirred vigorously to titanium tetrachloride to be completely dissolved to form clear solution, it is anhydrous that 1.0g tungsten hexachlorides (2.52mmol) are dissolved in into 50mL
In ethanol, then above-mentioned mixed solution is transferred in 100mL polytetrafluoroethylkettle kettles and (accounts for kettle product about 90%), in 200 DEG C of guarantors
Room temperature is naturally cooled to after holding 12h, cavity core shell structure TiO is made after centrifuge washing2/WO3Composite photocatalyst.
Application Example
Photochemical catalytic oxidation acetaldehyde reacts
Weigh after synthesizing through 550 DEG C of roasting 3h in Muffle furnace, the catalyst 50mg prepared by embodiment 1-13, use 1000
± 10ppm, 5uL acetaldehyde are as simulation gas.Xenon source is opened, carries out Photocatalytic Degradation Process, collection in every 15 minutes is once
Gaseous sample, content analysis is carried out with gas-chromatography.Content analysis, analysis result such as table 1 are carried out to collection gas after 1.0 hours
It is shown：
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 control | 2 |
Tested by the photooxidative degradation of acetaldehyde, the results showed that, the hud typed photocatalyst surface knot with cavity structure
Structure has a great influence to photocatalysis effect, and when the acicular texture of spherical outer surface growth attaching particles, degrading activity is optimal, a side
Face is that multiple reflections utilization rate, still further aspect acicular texture may be because Ti, W on a catalyst such a structure increases light
The presence of hetero-junctions improves the separative efficiency of photo-generate electron-hole.
Although the present invention discloses preferred embodiment as above, so it is not limited to present disclosure, any ripe
Know this those skilled in the art, do not departing from the present invention main spirits and context in, when can make it is various change and retouching, therefore invent
Protection domain should be defined by the basic right claimed range applied for a patent.
Claims (7)
- A kind of 1. cavity core shell structure TiO2/WO3The preparation method of composite photo-catalyst, comprises the following steps：(1) by TiCl4It is dissolved in mixing alcoholic solution and obtains solution A；By WCl6It is dissolved in ethanol and obtains solution B；Then will be molten Liquid A and solution B mix 0.5-1.0 hours, and material liquid is made；Wherein, described mixing alcoholic solution is by the tert-butyl alcohol, ethylene glycol It is 1-9 by volume:1 mixing；Described TiCl4Molar concentration in alcoholic solution is mixed is 0.01-0.15mol/L；It is described WCl6And TiCl4Mol ratio be 1-10:1；(2) material liquid is transferred to using polytetrafluoroethylene (PTFE) as in the water heating kettle of liner, during 120-200 DEG C of reaction of controlling reaction temperature Between 12-72h, be cooled to room temperature, cavity core shell structure TiO be made after centrifuge washing2/WO3Composite photo-catalyst.
- 2. preparation method according to claim 1, it is characterised in that：Mixing alcoholic solution in the step (1) is by tertiary fourth Alcohol, ethylene glycol are 1-3 by volume:1 mixing.
- 3. preparation method according to claim 1, it is characterised in that：WCl in the step (1)6Mole in ethanol Concentration is 0.025-0.15mol/L.
- 4. preparation method according to claim 1, it is characterised in that：Material liquid in the step (2) accounts for hydro-thermal kettle Long-pending more than 80%.
- 5. preparation method according to claim 1, it is characterised in that：Reaction temperature in the step (2) is 160 DEG C.
- A kind of 6. cavity core shell structure TiO2/WO3Composite photo-catalyst, prepared by the method described in claim any one of 1-5 And obtain, the particle diameter of the catalyst is 1-2um, cavity diameter 150-200nm, and nucleocapsid pattern outer surface homoepitaxial small The nano whiskers structure of grain attachment, Ti, W element are evenly distributed in catalyst structure, and the specific surface area of catalyst reaches 138- 203m2/g。
- 7. cavity core shell structure TiO according to claim 62/WO3The light of composite photo-catalyst pollutant acetaldehyde indoors Application in catalytic degradation.
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| CN106166498B (en) * | 2016-06-20 | 2019-01-25 | 同济大学 | A kind of nanometer of WO3/TiO2The preparation method of iron 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 |
| CN108722394B (en) * | 2018-05-25 | 2020-05-19 | 东北大学 | WO having a yolk-eggshell structure3-TiO2Nanocomposite and method for preparing same |
| 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 |
| 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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| CN101791545A (en) * | 2010-03-02 | 2010-08-04 | 上海师范大学 | Method for preparing (001) surface-exposed micrometer laminar titanium dioxide photocatalyst |
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