CN105289565A - TiO<2>@SiO<2> photocatalyst and application of same to photocatalytic reduction for CO<2> - Google Patents
TiO<2>@SiO<2> photocatalyst and application of same to photocatalytic reduction for CO<2> Download PDFInfo
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- CN105289565A CN105289565A CN201510715539.XA CN201510715539A CN105289565A CN 105289565 A CN105289565 A CN 105289565A CN 201510715539 A CN201510715539 A CN 201510715539A CN 105289565 A CN105289565 A CN 105289565A
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Abstract
The invention belongs to the field of photocatalyst preparation and particularly relates to a TiO<2>@SiO<2> photocatalyst and application of the same to photocatalytic reduction for CO<2>. A preparation method of the photocatalyst comprises the steps that Degussa P25-TiO<2> serves as the material core, the material core is wrapped with a SiO<2> thin layer through a simple sol-gel method, and the TiO<2>@SiO<2> photocatalyst which is of a core-shell structure and different in SiO<2> mass content is obtained. According to the TiO<2>@SiO<2> photocatalyst and the application of the same to photocatalytic reduction for CO<2>, the TiO<2>@SiO<2> photocatalyst is applied to gaseous phase photocatalysis CO<2> reduction for the first time, and the regulation effects of SiO<2> wrapping on activity and selectivity of TiO<2> photocatalytic reduction for CO<2> are explored. The catalyst is simple in preparation method, low in cost, convenient to prepare in an amplified mode and environmentally friendly, when the photocatalyst is used for reduction for CO<2> through photocatalysis, the greenhouse effect can be alleviated, reduction products can be used as fuel, and sustainable development of the environment and energy is facilitated.
Description
Technical field
The invention belongs to the sustainable development field of catalyst preparing and environment and the energy, be specifically related to a kind of TiO
2siO
2photochemical catalyst and photo catalytic reduction CO thereof
2.
Background technology
The continuous increase of the CO2 emissions in the day by day exhausted and air of fossil fuel reserves make current global environment and energy problem more and more outstanding.Artificial photosynthesis, being converted into regenerative resource by carbon dioxide in air by light-catalysed method is that solution environment and energy problem provide new way.But the transformation efficiency of current this artificial photosynthesis is also very low, based on this, large quantifier elimination is devoted to improve the photoresponse of traditional photochemical catalyst and the separative efficiency of carrier to improve catalytic performance, such as semiconductors coupling, noble metal loading, element doping etc.But nearest research report, by improving photochemical catalyst CO absorption
2ability be further improve its photocatalysis CO
2reducing power provides another kind of possibility.
The method of sol-gel silica parcel be improve embedding substance surface area and increase adsorption capacity and provide a green effective method, and its preparation method is simple, is easy to amplify, with low cost and environmentally friendly.It is worth mentioning that, the method for Silicon dioxide sol-gel parcel shows in the research in thermocatalytic field, and parcel catalytic active species can prevent it from assembling and increase surface area to strengthen adsorption capacity, thus improves reactivity.But the report being improved its photocatalysis performance by Silica-coated semiconductor light-catalyst is but also extremely lacked, particularly it is to gas-phase photocatalysis CO
2the probing into of impact of reducing activity does not also cause certain concern.
We are with Degussa P25-TiO that is nontoxic, cheap, stable chemical nature
2for base material, prepare the TiO with nucleocapsid structure by a kind of simple sol-gel process
2siO
2composite, have studied its photo catalytic reduction CO under simulated solar illumination
2performance.Result shows, by this simple SiO
2parcel TiO
2method can greatly increase it to CO
2adsorption capacity, and the formation of Ti-O-Si key facilitates the separative efficiency of its photo-generated carrier, finally achieves it to photocatalysis CO
2the regulation and control of the activity and selectivity of reduction.
Summary of the invention
The object of the present invention is to provide a kind of TiO
2siO
2photochemical catalyst and photo catalytic reduction CO thereof
2, this catalyst is easy to preparation, with low cost, environmentally friendly; This TiO
2siO
2catalyst is at photo catalytic reduction CO
2aspect has to be applied well, TiO
2siO
2to CO
2the activity of reduction improves, and especially significantly improves the selective of CO product, wherein TiO
230%SiO
2selectively reach 72.4%, be blank TiO
2(25.2%) nearly three times.
For achieving the above object, the present invention adopts following technical scheme:
A kind of TiO
2siO
2photochemical catalyst: with Degussa P25-TiO
2for core, be wrapped with SiO at it
2the catalyst with core-casing structure of thin layer; Wherein, SiO
2mass content be 5% ~ 50%.
In described catalyst, SiO
2mass content be 30%.
A kind of TiO as above
2siO
2the application of photochemical catalyst: for gas-phase photocatalysis CO
2reduction.
Described TiO
2siO
2photochemical catalyst is used for photo catalytic reduction CO
2, under simulated solar irradiation, irradiate 8h, compared to blank TiO
2, it is to CO
2the activity of reduction improves, and especially significantly improves the selective of CO product, wherein TiO
230%SiO
2reaching 72.4% to the selective of CO, is blank TiO
2(25.2%) nearly three times.
One prepares TiO as above
2siO
2the method of catalyst, comprises the following steps:
(1) by the hydrochloric acid solution of tetraethyl orthosilicate, ethanol and 1M according to volume ratio 1:2:1 mixing and stirring, obtain the hydrolyzate of tetraethyl orthosilicate;
(2) by TiO
2in 1ml water, ultrasonic disperse is even, then with the hydrolyzate of tetraethyl orthosilicate according to certain ratio mixing and stirring, obtain mixing suspension;
(3) in mixing suspension, slowly drip the sodium hydroxide solution of 1M, to mixed liquor dehydration plastic, close storage 24h and make colloid aging, finally dry and obtain TiO
2siO
2photochemical catalyst.
Catalyst photo catalytic reduction CO of the present invention
2concrete steps as follows:
(1) a certain amount of TiO is got
2siO
2photochemical catalyst is in the crystal reaction tube of 25ml at volume, and this reaction tube is filled with pure carbon dioxide gas after being vacuumized by mechanical pump, and repeats three times; Afterwards, the aqueous water syringe that vacuumizes of 0.5ml is expelled in the 5ml sample cell that hangs in crystal reaction tube by the barrier film on reaction tube, keep CO
2final pressure be 8kPa;
(2) above-mentioned system simulated solar irradiation (luxuriant and rich with fragrance Lay is moored in 300W xenon lamp, Beijing) illumination, after 8 hours, is taken out the reactant gas of 0.3ml, analyzed by gas-chromatography from reaction tube with sampling probe;
(3) this reacted mist (CO
2, H
2, CO and CH
4) adopt carbon molecular sieve (TDX-01) post to be separated, afterwards, H
2be analyzed by TCD detector, CO is further converted to CH by methanation converter
4after analyzed by fid detector, CH
4directly analyzed by fid detector.Remaining CO
2gone out by six-way valve blowback.
remarkable advantage of the present invention is:
(1) the present invention is by TiO
2siO
2photochemical catalyst is used for gas-phase photocatalysis reduction CO
2, demonstrate sol-gel SiO
2wrap up regulation and control TiO
2photo catalytic reduction CO
2activity and optionally feasibility; TiO
230%SiO
2reaching 72.4% to the selective of CO, is blank TiO
2(25.2%) nearly three times, effect is very outstanding;
(2) TiO
2siO
2the preparation method of photochemical catalyst is simple, with low cost, is convenient to amplify to produce and environmentally friendly.
Accompanying drawing explanation
Fig. 1 is TiO
230%SiO
2transmission electron microscope (TEM) figure of composite;
Fig. 2 is TiO
230%SiO
2x-ray diffraction (XPS) figure of composite, (Fig. 2-A is Si, Fig. 2-B is Ti);
Fig. 3 is each ratio TiO
2siO
2composite and blank TiO
2fourier transform infrared spectroscopy (FT-IR) figure;
Fig. 4 is each ratio TiO
2siO
2composite and blank TiO
2to CO
2energy of adsorption try hard to;
Fig. 5 is each ratio TiO
2siO
2composite and blank TiO
2fluorescence spectrum (PL) figure;
Fig. 6 is TiO
2, TiO
25%SiO
2, TiO
210%SiO
2, TiO
230%SiO
2, TiO
250%SiO
2catalyst photo catalytic reduction CO
2product distribution map (Fig. 6-A), CO
2conversion ratio and selective figure (Fig. 6-B) to product C O.
Detailed description of the invention
Illustrate content of the present invention further below in conjunction with specific embodiment, but these embodiments do not limit the scope of the invention.
embodiment 1
By 20mgTiO
2photochemical catalyst is placed in the crystal reaction tube that volume is 25ml, is filled with pure carbon dioxide gas after being vacuumized by reaction tube, and repeats three times; Afterwards, 0.5ml vacuumized aqueous water injector to inject to quartz ampoule, keep CO
2final pressure be 8kPa; After above-mentioned system illumination (simulated solar irradiation) 8h, from reaction tube, take out the reactant gas of 0.3ml with sampling probe, analyzed by gas-chromatography; Calculate, H
2generating rate be 2.17 μm of olg
-1h
-1, the generating rate of CO is 1.79 μm of olg
-1h
-1, CH
4generating rate be 0.77 μm of olg
-1h
-1, CO
2conversion ratio be 2.62 μm of olg
-1h
-1, be 25.23% to the selective of CO.
embodiment 2
By hydrochloric acid solution (HCl) mixing and stirring of 2ml tetraethyl orthosilicate (TEOS), 4ml ethanol (ETOH) and 2ml1M, obtain the hydrolyzate of TEOS; By 0.1gTiO
2in 1ml water, ultrasonic disperse is even, the then above-mentioned TEOS hydrolyzate mixing and stirring with 0.08ml; The sodium hydroxide solution (NaOH) slowly dripping 1M in above-mentioned mixing suspension, to mixed liquor dehydration plastic, is closed storage 24h and is made colloid aging, finally dry and obtain gel; Gel abrasive is obtained TiO
25%SiO
2powder sample.
By 20mgTiO
25%SiO
2photochemical catalyst is placed in the crystal reaction tube that volume is ~ 25ml, is filled with pure carbon dioxide gas, and repeats three times after being vacuumized by reaction tube; Afterwards, 0.5ml vacuumized aqueous water injector to inject to quartz ampoule, keep CO
2final pressure be 8KPa; After above-mentioned system illumination (simulated solar irradiation) 8h, from reaction tube, take out the reactant gas of 0.3ml with sampling probe, analyzed by gas-chromatography; Calculate, H
2generating rate be 1.21 μm of olg
-1h
-1, the generating rate of CO is 2.76 μm of olg
-1h
-1, CH
4generating rate be almost 0, CO
2conversion ratio be 2.76 μm of olg
-1h
-1, be 69.54% to the selective of CO.
embodiment 3
By hydrochloric acid solution (HCl) mixing and stirring of 2ml tetraethyl orthosilicate (TEOS), 4ml ethanol (ETOH) and 2ml1M, obtain the hydrolyzate of TEOS; By 0.1gTiO
2in 1ml water, ultrasonic disperse is even, the then above-mentioned TEOS hydrolyzate mixing and stirring with 0.15ml; The sodium hydroxide solution (NaOH) slowly dripping 1M in above-mentioned mixing suspension, to mixed liquor dehydration plastic, is closed storage 24h and is made colloid aging, finally dry and obtain gel; Gel abrasive is obtained TiO
210%SiO
2powder sample.By 20mgTiO
210%SiO
2photochemical catalyst is placed in the crystal reaction tube that volume is 25ml, is filled with pure carbon dioxide gas after being vacuumized by reaction tube, and repeats three times; Afterwards, 0.5ml vacuumized aqueous water injector to inject to quartz ampoule, keep CO
2final pressure be 8KPa; After above-mentioned system illumination (simulated solar irradiation) 8h, from reaction tube, take out the reactant gas of 0.3ml with sampling probe, analyzed by gas-chromatography; Calculate, H
2generating rate be 1.25 μm of olg
-1h
-1, the generating rate of CO is 2.93 μm of olg
-1h
-1, CH
4generating rate be almost 0, CO
2conversion ratio be 2.93 μm of olg
-1h
-1, be 72.11% to the selective of CO.
embodiment 4
By hydrochloric acid solution (HCl) mixing and stirring of 2ml tetraethyl orthosilicate (TEOS), 4ml ethanol (ETOH) and 2ml1M, obtain the hydrolyzate of TEOS; By 0.1gTiO
2in 1ml water, ultrasonic disperse is even, the then above-mentioned TEOS hydrolyzate mixing and stirring with 0.67ml; The sodium hydroxide solution (NaOH) slowly dripping 1M in above-mentioned mixing suspension, to mixed liquor dehydration plastic, is closed storage 24h and is made colloid aging, finally dry and obtain gel; Gel abrasive is obtained TiO
230%SiO
2powder sample; By 20mgTiO
230%SiO
2photochemical catalyst is placed in the crystal reaction tube that volume is 25ml, is filled with pure carbon dioxide gas after being vacuumized by reaction tube, and repeats three times; Afterwards, 0.5ml vacuumized aqueous water injector to inject to quartz ampoule, keep CO
2final pressure be 8KPa.After above-mentioned system illumination (simulated solar irradiation) 8h, from reaction tube, take out the reactant gas of 0.3ml with sampling probe, analyzed by gas-chromatography.Calculate, H
2generating rate be 1.19 μm of olg
-1h
-1, the generating rate of CO is 3.13 μm of olg
-1h
-1, CH
4generating rate be almost 0, CO
2conversion ratio be 3.13 μm of olg
-1h
-1, be 72.39% to the selective of CO.
embodiment 5
By hydrochloric acid solution (HCl) mixing and stirring of 2ml tetraethyl orthosilicate (TEOS), 4ml ethanol (ETOH) and 2ml1M, obtain the hydrolyzate of TEOS.By 0.1gTiO
2in 1ml water, ultrasonic disperse is even, the then above-mentioned TEOS hydrolyzate mixing and stirring with 1.53ml.The sodium hydroxide solution (NaOH) slowly dripping 1M in above-mentioned mixing suspension, to mixed liquor dehydration plastic, is closed storage 24h and is made colloid aging, finally dry and obtain gel.Gel abrasive is obtained TiO
250%SiO
2powder sample; By 20mgTiO
250%SiO
2photochemical catalyst is placed in the crystal reaction tube that volume is ~ 25ml, is filled with pure carbon dioxide gas, and repeats three times after being vacuumized by reaction tube; Afterwards, 0.5ml vacuumized aqueous water injector to inject to quartz ampoule, keep CO
2final pressure be 8kPa; After above-mentioned system illumination (simulated solar irradiation) 8h, from reaction tube, take out the reactant gas of 0.3ml with sampling probe, analyzed by gas-chromatography.Calculate, H
2generating rate be 1.2 μm of olg
-1h
-1, the generating rate of CO is 2.66 μm of olg
-1h
-1, CH
4generating rate be almost 0, CO
2conversion ratio be 2.66 μm of olg
-1h
-1, be 68.83% to the selective of CO.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. a TiO
2siO
2photochemical catalyst, is characterized in that: with Degussa P25-TiO
2for core, be wrapped with SiO at it
2the catalyst with core-casing structure of thin layer; Wherein, SiO
2mass content be 5% ~ 50%.
2. TiO according to claim 1
2siO
2photochemical catalyst, is characterized in that: in described catalyst, SiO
2mass content be 30%.
3. a TiO as claimed in claim 1 or 2
2siO
2the application of photochemical catalyst, is characterized in that: for gas-phase photocatalysis CO
2reduction.
4. prepare TiO as claimed in claim 1 for one kind
2siO
2the method of catalyst, is characterized in that: comprise the following steps:
(1) by the hydrochloric acid solution of tetraethyl orthosilicate, ethanol and 1M according to volume ratio 1:2:1 mixing and stirring, obtain the hydrolyzate of tetraethyl orthosilicate;
(2) by TiO
2in 1ml water, ultrasonic disperse is even, then with the hydrolyzate of tetraethyl orthosilicate according to certain ratio mixing and stirring, obtain mixing suspension;
(3) in mixing suspension, slowly drip the sodium hydroxide solution of 1M, to mixed liquor dehydration plastic, close storage 24h and make colloid aging, finally dry and obtain TiO
2siO
2photochemical catalyst.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105771950A (en) * | 2016-04-26 | 2016-07-20 | 中国石油大学(华东) | Preparation method of one-dimensional TiO2/SiO2 nano photocatalytic material |
CN105836703A (en) * | 2016-03-18 | 2016-08-10 | 浙江大学 | Method for preparing synthetic gas through photo-thermal chemical circulation decomposition of carbon dioxide |
CN108479855A (en) * | 2018-03-28 | 2018-09-04 | 北京工业大学 | A kind of nucleocapsid metal organic framework base composite photocatalyst and preparation method thereof |
CN108786792A (en) * | 2018-06-25 | 2018-11-13 | 福州大学 | A kind of metal/semiconductor composite photo-catalyst and its preparation and application |
CN109126791A (en) * | 2018-07-24 | 2019-01-04 | 福州大学 | A kind of Cu (II)-mTiO2Loaded photocatalyst and its preparation and application |
CN110605134A (en) * | 2019-08-30 | 2019-12-24 | 浙江迈实科技有限公司 | Hollow core-shell structure nitrogen-doped TiO2Method for preparing microspheres |
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US20030104198A1 (en) * | 2001-08-08 | 2003-06-05 | Degussa Ag | Metal oxide particles coated with silicon dioxide |
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BI-JIN LIU ET AL.: "Effect of solvents on photocatalytic reduction of carbon dioxide using TiO2 nanocrystal photocatalyst embedded in SiO2 matrices", 《JOURNAL OF PHOTOCHEMISTRY AND PHOTOBIOLOGY A: CHEMISTRY》 * |
LIANJUN LIU ET AL.: "Understanding the Reaction Mechanism of Photocatalytic Reduction of CO2 with H2O on TiO2-Based Photocatalysts: A Review", 《AEROSOL AND AIR QUALITY RESEARCH》 * |
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Cited By (8)
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---|---|---|---|---|
CN105836703A (en) * | 2016-03-18 | 2016-08-10 | 浙江大学 | Method for preparing synthetic gas through photo-thermal chemical circulation decomposition of carbon dioxide |
CN105771950A (en) * | 2016-04-26 | 2016-07-20 | 中国石油大学(华东) | Preparation method of one-dimensional TiO2/SiO2 nano photocatalytic material |
CN108479855A (en) * | 2018-03-28 | 2018-09-04 | 北京工业大学 | A kind of nucleocapsid metal organic framework base composite photocatalyst and preparation method thereof |
CN108479855B (en) * | 2018-03-28 | 2020-07-03 | 北京工业大学 | Core-shell structure metal organic framework-based composite photocatalyst and preparation method thereof |
CN108786792A (en) * | 2018-06-25 | 2018-11-13 | 福州大学 | A kind of metal/semiconductor composite photo-catalyst and its preparation and application |
CN108786792B (en) * | 2018-06-25 | 2021-03-26 | 福州大学 | Metal/semiconductor composite photocatalyst and preparation and application thereof |
CN109126791A (en) * | 2018-07-24 | 2019-01-04 | 福州大学 | A kind of Cu (II)-mTiO2Loaded photocatalyst and its preparation and application |
CN110605134A (en) * | 2019-08-30 | 2019-12-24 | 浙江迈实科技有限公司 | Hollow core-shell structure nitrogen-doped TiO2Method for preparing microspheres |
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