CN110627116A - Hydrogen-doped TiO (titanium dioxide)2Phase-change nano material and application thereof - Google Patents
Hydrogen-doped TiO (titanium dioxide)2Phase-change nano material and application thereof Download PDFInfo
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- CN110627116A CN110627116A CN201910839855.6A CN201910839855A CN110627116A CN 110627116 A CN110627116 A CN 110627116A CN 201910839855 A CN201910839855 A CN 201910839855A CN 110627116 A CN110627116 A CN 110627116A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 24
- 239000004408 titanium dioxide Substances 0.000 title claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000001699 photocatalysis Effects 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 239000007787 solid Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 10
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910006069 SO3H Inorganic materials 0.000 claims description 3
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000011065 in-situ storage Methods 0.000 description 7
- 238000007540 photo-reduction reaction Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000004627 transmission electron microscopy Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000013169 thromboelastometry Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/86—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by NMR- or ESR-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses hydrogen-doped TiO2A phase-change nano material and application thereof belong to the field of preparation and application of clean and sustainable novel energy. The method obtains TiO doped with hydrogen of different phases under the condition of low-temperature hydrothermal treatment by mainly regulating and controlling different proportions of organic strong acid and water2A material. The doping increases the light absorption range of the material and improves the efficiency of separating the photon-generated carriers, so that the catalytic activity of the material is greatly improved and the catalytic efficiency of photocatalytic hydrogen production is improved due to the two reasons, and the detailed explanation that the catalytic effect mainly comes from the widening of the light absorption range and the effective separation of the photon-generated carriers is provided.
Description
Technical Field
The invention belongs to the field of clean and sustainable novel energy preparation and application, and particularly relates to hydrogen-doped TiO2Phase-change nano material and application thereof in photocatalytic hydrogen production reaction.
Background
Along with the continuous development of the world economy, energy and environmentThe problem has become one of the problems to be solved urgently at present. Hydrogen, a clean and renewable energy source, is gradually becoming a hot spot for the research of the majority of researchers. Compared with methods for consuming energy such as methane steam reforming, coal gasification and water electrolysis, the method for decomposing water into hydrogen by using inexhaustible natural energy, namely solar energy, is favored. Among the numerous photocatalytic materials, TiO2Due to its good chemical stability, thermal stability, environmental friendliness and suitable energy band position, it is one of the most potential photocatalytic materials and is widely used in the field of photocatalysis.
Well known TiO stabilized in existence2There are three crystal forms: anatase, rutile and brookite, but these three crystalline forms of TiO2But are not all suitable for photocatalytic water splitting. Anatase is generally better than rutile and brookite. Unfortunately, while rutile is not as characteristic as anatase, it has a better absorption range for sunlight than anatase. If the photocatalytic property of rutile is to be improved, the structure of rutile needs to be modified, so that the light utilization rate is further widened and the recombination rate of photon-generated carriers is inhibited under the condition of keeping the original advantages, and the two problems are solved, so that the efficiency of the rutile in the aspect of photocatalysis is greatly promoted.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a hydrogen-doped TiO2Phase-change nano material and is applied to the field of photocatalysis water decomposition catalysis. The hydrogen-doped TiO2The phase-change nano material has the characteristics of low price, simple preparation, high catalytic activity, good stability and the like.
The invention is realized by the following technical scheme: hydrogen-doped TiO (titanium dioxide)2Phase change nanomaterial of hydrogen doped TiO2The phase-change nano material is prepared by the following method:
(1) CF is prepared by3SO3H and water are uniformly mixed according to the volume ratio of 1: 0-1: 1 to obtain CF3SO3H aqueous solution.
(2) 4-10ml of tetrabutyl titanate is added into a polytetrafluoroethylene lined autoclave.
(3) 4ml of the CF obtained in step 1 are taken3SO3And (3) dropwise adding the H aqueous solution into the high-pressure reaction kettle in the step (2), stirring, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the high-pressure reaction kettle after uniform mixing and no precipitation, and carrying out hydrothermal treatment at the temperature of 140-.
(4) After the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed by water for 3 times, the centrifugal speed is 6000-2And (3) nano materials.
Hydrogen-doped TiO (titanium dioxide)2The application of the nano-structure material in the photocatalytic hydrogen production reaction.
Compared with the prior art, the invention has the beneficial effects that: the invention takes organic strong acid as raw material and hydrogen source, and hydrogen is introduced into TiO by the participation of hydrogen in the reaction process2In the crystal lattice and with the TiO formed2Interaction to alter TiO2The structure of (1). The in-situ hydrogen-doped TiO is obtained by a simple low-temperature hydrothermal method2Compared with a hydrogen post-treatment method, the method can obtain a bulk-doped material with good crystallinity. This structure is H-doped TiO in terms of catalytic activity2The absorption range of light is widened, and the effective separation of the material on photon-generated carriers is enhanced, so that the utilization rate of the material on photocatalytic water decomposition is greatly improved.
Drawings
FIG. 1 shows hydrogen-doped TiO according to the invention2XRD pattern of phase change nano material;
FIG. 2 is a schematic representation of the present invention employing 95 vt% CF3SO3Preparation of hydrogen-doped TiO from H aqueous solution2Transmission electron microscope pictures (TEMs);
FIG. 3 is a diagram of the present invention employing 50 vt% CF3SO3Hydrogen doped TiO prepared from H aqueous solution2Transmission Electron Microscopy (TEM) of phase change nanomaterials;
figure 4 is the bookHydrogen-doped TiO prepared by invention2Solid H nuclear magnetism of the phase-change nano material;
FIG. 5 shows hydrogen-doped TiO prepared according to the present invention2A spectral data plot of the phase change nanomaterial;
FIG. 6 shows hydrogen-doped TiO prepared according to the present invention2Phase change nanomaterials compared to the photocatalytic hydrogen production rate of commercial P25.
Detailed Description
The technical solution of the invention is further illustrated below with reference to the accompanying drawings and examples, which are not to be construed as limiting the technical solution.
Example 1
(1) CF is prepared by3SO3Mixing H and water according to the volume ratio of 1:1 to obtain CF3SO3An aqueous solution of H;
(2) adding 10ml of tetrabutyl titanate into a 50ml of high-pressure reaction kettle with a polytetrafluoroethylene lining;
(3) 4ml of the CF mixed in step 1 were taken out3SO3Dropwise adding the H aqueous solution into a high-pressure reaction kettle filled with tetrabutyl titanate, stirring, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the reaction kettle after uniform mixing and no precipitation, and carrying out hydrothermal treatment at 180 ℃ for 16 hours;
(4) after the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed for 3 times by water, the centrifugal condition is 6000rpm/10min, and finally the solid is dried for 8 hours in vacuum at the temperature of 80 ℃ to obtain the hydrogen-doped TiO2And (3) nano materials.
FIG. 1 shows the hydrogen-doped TiO prepared in this example2XRD pattern of phase-change nano material. It can be seen from the figure that 50 vt% water produces hydrogen doped TiO2Is anatase phase. FIG. 2 shows the preparation of hydrogen-doped TiO with 50 vt% water prepared in this example2Transmission Electron Microscopy (TEM) of (A) in which the anatase phase TiO prepared by this process is visible2Is nano-particle of about 10 nm. FIG. 4 shows the preparation of hydrogen-doped TiO with 50% vt water prepared in this example2Solid hydrogen nuclear magnetic field, as can be seen from the figure, this hydrogen doped TiO2The material has many forms of hydrogen. FIG. 5 shows the hydrogen-doped TiO prepared in this example2Spectral data plot of material. From the figure it can be seen that the hydrogen doped TiO with 50 vt% water2The material expands the absorption range of light.
The hydrogen-doped TiO prepared in example 1 was taken230mg of a sample is added into 80ml of 20vt percent methanol aqueous solution, 0.5wt percent platinum chloroplatinic acid solution is added into the solution (in-situ photoreduction) and is connected into a photocatalytic system (GC2014), a 300W xenon lamp is used as a light source for simulating sunlight, firstly, the sample is vacuumized for 30min, secondly, the sample is subjected to photoreduction to generate a Pt cocatalyst in situ, and then, the photocatalytic hydrogen production test is carried out.
FIG. 6 shows the hydrogen-doped TiO prepared in this example2Material versus photocatalytic hydrogen production rate of commercial P25. From the figure, it can be seen that the hydrogen-doped TiO2Compared with commercial P25, the photocatalytic hydrogen production efficiency of the material is improved by about 1.28 times under the same condition. Shows higher catalytic activity.
Example 2
(1) CF is prepared by3SO3H and water are uniformly mixed according to the volume ratio of 1:0.05 to obtain CF3SO3An aqueous solution of H;
(2) adding 10ml of tetrabutyl titanate into a 50ml of high-pressure reaction kettle with a polytetrafluoroethylene lining;
(3) 4ml of the CF mixed in step 1 were taken out3SO3Dropwise adding the H aqueous solution into a high-pressure reaction kettle filled with tetrabutyl titanate, stirring, after uniformly mixing and no precipitation, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the reaction kettle, and carrying out hydrothermal treatment at 200 ℃ for 10 hours;
(4) after the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed for 3 times by water, the centrifugal condition is 8000rpm/10min, and finally the solid is dried for 8 hours in vacuum at the temperature of 80 ℃ to obtain the hydrogen-doped TiO2And (3) nano materials.
The hydrogen-doped TiO prepared in this example is shown in FIG. 12XRD pattern of phase-change nano material, from which it can be seen that 5 vt% water is used to prepare hydrogen-doped TiO2The rutile phase is rod-shaped. FIG. 3 shows the preparation of hydrogen-doped TiO with 5 vt% water prepared in this example2Transmission Electron Microscopy (TEM) of (A) from which it can be seen that the rutile phase TiO produced by this method is in the form of a powder2Is nano-particle of about 10 nm. The preparation of hydrogen doped TiO with 5% vt water prepared in this example is shown in FIG. 42Solid hydrogen Nuclear Magnetic Resonance (NMR), it can be seen from the figure that rutile phase TiO obtained by this method2The solid hydrogen nuclear magnetic spectrum (fig. 4) shows a more enhanced participation in H. The hydrogen-doped TiO prepared in this example is shown in FIG. 52Spectral data plot of material. From the figure it can be seen that the hydrogen doped TiO contains 5 vt% water2The material expands the absorption range of light.
The hydrogen-doped TiO prepared in example 2 was taken230mg of a sample is added into 80ml of 20vt percent methanol aqueous solution, 0.5wt percent platinum chloroplatinic acid solution is added into the solution (in-situ photoreduction) and is connected into a photocatalytic system (GC2014), a 300W xenon lamp is used as a light source for simulating sunlight, firstly, the sample is vacuumized for 30min, secondly, the sample is subjected to photoreduction to generate a Pt cocatalyst in situ, and then, the photocatalytic hydrogen production test is carried out.
As can be seen from fig. 6, the photocatalytic hydrogen production efficiency of the present example is improved by about 1.74 times compared to that of commercial P25. Shows higher catalytic activity.
Example 3
(1) Adding 4ml of tetrabutyl titanate into a 50ml of high-pressure reaction kettle with a polytetrafluoroethylene lining;
(2) take out 4ml of CF3SO3Dropwise adding the H original solution into a high-pressure reaction kettle filled with tetrabutyl titanate, stirring, after uniformly mixing and no precipitation, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the reaction kettle, and carrying out hydrothermal treatment at 140 ℃ for 16 hours;
(4) after the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed for 3 times by water, the centrifugal condition is 8000rpm/10min, and finally the solid is dried for 8 hours in vacuum at the temperature of 80 ℃ to obtain the hydrogen-doped TiO2And (3) nano materials.
Taking the product prepared in example 3Hydrogen doped TiO230mg of a sample is added into 80ml of 20vt percent methanol aqueous solution, 0.5wt percent platinum chloroplatinic acid solution is added into the solution (in-situ photoreduction) and is connected into a photocatalytic system (GC2014), a 300W xenon lamp is used as a light source for simulating sunlight, firstly, the sample is vacuumized for 30min, secondly, the sample is subjected to photoreduction to generate a Pt cocatalyst in situ, and then, the photocatalytic hydrogen production test is carried out.
As can be seen from fig. 6, the photocatalytic hydrogen production efficiency of the present example is improved by about 1.34 times compared with that of commercial P25. Shows higher catalytic activity.
Claims (2)
1. Hydrogen-doped TiO (titanium dioxide)2Phase change nano material, characterized in that the hydrogen doped TiO2The phase-change nano material is prepared by the following method:
(1) CF is prepared by3SO3H and water are uniformly mixed according to the volume ratio of 1: 0-1: 1 to obtain CF3SO3H aqueous solution.
(2) 4-10ml of tetrabutyl titanate is added into a polytetrafluoroethylene lined autoclave.
(3) 4ml of the CF obtained in step 1 are taken3SO3And (3) dropwise adding the H aqueous solution into the high-pressure reaction kettle in the step (2), stirring, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the high-pressure reaction kettle after uniform mixing and no precipitation, and carrying out hydrothermal treatment at the temperature of 140-.
(4) After the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed by water for 3 times, the centrifugal speed is 6000-2And (3) nano materials.
2. The hydrogen-doped TiO of claim 12The application of the nano-structure material in the photocatalytic hydrogen production reaction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116618095A (en) * | 2023-05-29 | 2023-08-22 | 广州大学 | Hydrogen doping WO 3 And Ag nanoparticle-loaded hydrogen doping WO 3 Preparation method of powder and application of powder in photocatalysis field |
| WO2023219397A1 (en) * | 2022-05-10 | 2023-11-16 | 한국세라믹기술원 | Hydrogen-doped reduced titania powder and preparation method therefor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145918A (en) * | 2011-04-18 | 2011-08-10 | 东华大学 | Method for preparing rutile titanium dioxide nanoparticles by using highly strong acid |
| JP2019038713A (en) * | 2017-08-24 | 2019-03-14 | 国立大学法人 鹿児島大学 | Metal oxide nanoparticles and production method thereof |
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- 2019-09-06 CN CN201910839855.6A patent/CN110627116B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145918A (en) * | 2011-04-18 | 2011-08-10 | 东华大学 | Method for preparing rutile titanium dioxide nanoparticles by using highly strong acid |
| JP2019038713A (en) * | 2017-08-24 | 2019-03-14 | 国立大学法人 鹿児島大学 | Metal oxide nanoparticles and production method thereof |
Non-Patent Citations (2)
| Title |
|---|
| GONGMING WANG等: "Hydrogen-Treated TiO2 Nanowire Arrays for Photoelectrochemical Water Splitting", 《NANO LETTERS》 * |
| 孔凡霞: "新型二氧化钛纳米材料的合成与性能研究", 《中国优秀硕士学位论文全文数据库-工程科技1辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023219397A1 (en) * | 2022-05-10 | 2023-11-16 | 한국세라믹기술원 | Hydrogen-doped reduced titania powder and preparation method therefor |
| CN116618095A (en) * | 2023-05-29 | 2023-08-22 | 广州大学 | Hydrogen doping WO 3 And Ag nanoparticle-loaded hydrogen doping WO 3 Preparation method of powder and application of powder in photocatalysis field |
| CN116618095B (en) * | 2023-05-29 | 2023-11-03 | 广州大学 | Hydrogen doping WO 3 And Ag nanoparticle-loaded hydrogen doping WO 3 Preparation method of powder and application of powder in photocatalysis field |
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