CN108607596A - A kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance2-xNxCatalyst and its preparation and application - Google Patents
A kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance2-xNxCatalyst and its preparation and application Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000001257 hydrogen Substances 0.000 title claims abstract description 33
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000003054 catalyst Substances 0.000 claims abstract description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910010443 TiO2-xNx Inorganic materials 0.000 claims abstract description 38
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 29
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 229910004339 Ti-Si Inorganic materials 0.000 claims abstract description 16
- 229910010978 Ti—Si Inorganic materials 0.000 claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 49
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- 238000001035 drying Methods 0.000 claims description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000003980 solgel method Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229960002380 dibutyl phthalate Drugs 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 238000005121 nitriding Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 239000000126 substance Substances 0.000 description 13
- 206010013786 Dry skin Diseases 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000001914 filtration Methods 0.000 description 6
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000005406 washing 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1064—Platinum group metal catalysts
- C01B2203/107—Platinum catalysts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1082—Composition of support materials
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance2‑xNxCatalyst and its preparation and application, catalyst are the aggregates constructed by platinum grain and mesoporous nitrogen-doped titanium dioxide；Preparation method includes：Prepared by Ti-Si composite oxide gel, mesoporous TiO2‑xNxPrepared by complex solution, prepared by the suspension of Pt nanoparticle, Composite Pt/TiO2‑xNxCatalyst preparation；Catalyst is applied to using visible light as the photocatalytic hydrogen production by water decomposition of light source.Present invention process and equipment are simple, are easy to get, short preparation period, are easy to mass produce；Obtained specific surface area of catalyst is high, and has higher visible absorption range, and hydrogen production by water decomposition is efficient under visible light.
Description
Technical field
The invention belongs to visible-light photocatalyst and its preparation and application fields, more particularly to a kind of to have visible photocatalysis
The Composite Pt/TiO of water hydrogen manufacturing performance2-xNxCatalyst and its preparation and application.
Background technology
Hydrogen Energy is generally acknowledged clean energy resource, is being shown one's talent as low-carbon and the zero carbon energy.21 century, China and U.S.
State, Japan, Canada, European Union etc. have all formulated Hydrogen Energy development plan, and China achieves in many ways in Hydrogen Energy field at present
The progress in face is expected to become Hydrogen Technology in the near future and applies leading one of country.In addition, current routine used
The energy belongs to non-renewable resources and increasingly depleted, it is therefore necessary to find the new energy.Hydrogen is exactly such a in routine
While the appearance of energy crisis and exploitation new secondary energy sources, new secondary energy sources that people expect.It is grinding countries in the world
Study carefully how a large amount of and cheap production hydrogen.Using solar energy come to decompose water be a main direction of studying, under the action of light
Hydrogen and oxygen are split water into, key is to find a kind of suitable catalyst.Nano-titanium dioxide is a kind of highly effective
Photochemical catalyst, but there is also can only absorb ultraviolet light, cannot be utilized to the visible light of sunlight accounting 40%.Nitrogen
After oxygen in equal nonmetalloids substitution titanium dioxide, the photoresponse range of titanium dioxide can be extended to visible light by ultraviolet light
Area, and show visible light catalysis activity.Immersion reduction method may be used in the deposition of semiconductor surface in noble metal.Noble metal
Deposition can greatly improve the transfer efficiency of light induced electron, and inhibit the compound of light induced electron and hole, and the light for improving semiconductor is urged
Change efficiency.Reported noble metal mainly including Pt, Ag, Ir, Au, Ru, Pd, Rh etc., wherein the report in relation to Pt is most, is imitated
Fruit is preferably also.
Invention content
Technical problem to be solved by the invention is to provide a kind of Composite Pt/ with visible photocatalysis water hydrogen manufacturing performance
TiO2-xNxCatalyst and its preparation and application, the preparation method is simple, and technological parameter is easy to control, and obtained catalyst compares table
Area is high, and has higher visible absorption range, and hydrogen production by water decomposition is efficient under visible light.
A kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance of the present invention2-xNxCatalyst, the catalysis
Agent is the aggregate constructed by platinum grain and mesoporous nitrogen-doped titanium dioxide, and wherein the load capacity of platinum is 0.5wt%-3wt%.
A kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance of the present invention2-xNxThe preparation side of catalyst
Method, specific implementation can be divided into three big steps：The first step prepares mesoporous TiO2-xNxComplex solution；Second step is prepared with microwave method
The suspension of Pt nanoparticle；Third step is to prepare Composite Pt/TiO2-xNxCatalyst to obtain there is visible light light to urge
Change the nitrogen-doped titanium dioxide mesoporous material for the platinum load for decomposing water characteristic.It specifically includes：
(1) mesoporous TiO2-xNxThe preparation of complex solution：Ti-Si composite oxide gel, titanium are prepared with sol-gel method
Si composite oxide gel nitrogenizes after drying, crushing, sieving and calcining (removing remaining organic matter), under ammonia atmosphere (to be made
Titania part nitrogenizes), lye washes (dissolve therein silica, excess nitrogen), washes, dry, obtains mesoporous TiO2-xNx
Compound, by mesoporous TiO2-xNxCompound is mixed with solvent, and ultrasound obtains mesoporous TiO2-xNxComplex solution, wherein 0<x<2,
Mesoporous TiO2-xNxThe mass ratio of compound and solvent is 1:10~200；
(2) suspension of Pt nanoparticle is prepared with microwave method：Compound containing platinum is dissolved in solvent, platiniferous chemical combination is obtained
Object solution, adjusting pH value of solution are 7-12 (alkali is added to adjust), are subsequently placed in microwave heating in micro-wave oven, cooling, obtain platinum nanometer
The ratio of the suspension of particle, wherein compound containing platinum and solvent is 20-60mg:80-110mL；
(3) Composite Pt/TiO is prepared2-xNxCatalyst：By step (1) intermediary hole TiO2-xNxComplex solution is added to step
Suddenly in (2) in the suspension of Pt nanoparticle, stirring, adjusting pH value of solution is 1-6, continues to stir, and is filtered, and is washed, dry, is obtained
Composite Pt/TiO2-xNxCatalyst, the wherein load capacity of platinum are 0.5wt%-3wt%.
Sol-gel method prepares Ti-Si composite oxide gel and is in the step (1)：By Butyl Phthalate and positive silicic acid second
Ester obtains Ti-Si composite oxide gel respectively as the presoma of titanium dioxide and silica by two step hydrolysis method,
The molar ratio of titanium and silicon is 1 in middle Ti-Si composite oxide gel:3-2:1, the concrete component of Ti-Si composite oxide gel is：
TiO2:3SiO2、TiO2:2SiO2、TiO2:SiO2、2TiO2:SiO2Deng 4 kinds.
Drying temperature is 50-110 DEG C in the step (1).
Lye is 2mol/L in the step (1), and the aqueous slkali washing compound using 2mol/L is to dissolve it
In silica, excessive concentration can be such that the photocatalysis performance of titanium dioxide declines, and concentration is too low to be not achieved dissolving titanium dioxide
The purpose of silicon.
Solvent is ethyl alcohol, ethylene glycol or isopropanol in the step (1), (2)；Alkali is sodium hydroxide or hydroxide
Potassium.
Solvent is consistent with solvent in step (1) in the step (2).
Calcination temperature is 400-600 DEG C in the step (1), calcination time 1-3h.
Ultrasonic time is 5min-1h in the step (1).The purpose of ultrasonic disperse is in order to avoid TiO2-xNxCompound
Reunion, make its dispersion evenly.
The flow of ammonia is 100-400 ml/mins in the step (1)；Nitriding temperature is 800-1000 DEG C, when nitridation
Between be 4-6h.
Compound containing platinum is chloroplatinic acid, platinic sodium chloride or potassium chloroplatinate in the step (2).
Microwave heating power is 500-1000W in the step (2), and microwave heating temperature is 50~200 DEG C, microwave heating
Time is 1-10min.Change the size of the platinum grain generated by adjusting the power of micro-wave oven, temperature and heating time.
It is to use hydrochloric acid, sulfuric acid or nitric acid that pH value of solution is adjusted in the step (3) as 1-6.
Mixing time is 1-5min in the step (3)；Continuation whipping temp is room temperature, and continuation mixing time is 1-48h.
When the load capacity of platinum is 2wt% in the step (3), Composite Pt/TiO2-xNxThe catalytic performance of catalyst is most
It is good.
A kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance of the present invention2-xNxCatalyst be applied to
Visible light is the photocatalytic hydrogen production by water decomposition of light source.
The present invention combines sol-gel method and Microwave reduction method, is prepared for a kind of high performance Composite Pt/TiO2- xNxVisible-light photocatalyst.
The N doping mesopore titania photocatalyst of platinum load prepared by the present invention, uniform component, large specific surface area, and
The separative efficiency that electron hole pair can be effectively improved between platinum, to improve photo-quantum efficiency.N doping and metal platinum
Load can increase absorption of the catalyst to visible light simultaneously, and material is made to have preferable visible light catalysis activity.Using visible light as light
Source, formic acid are sacrifice agent, carry out photocatalytic hydrogen production by water decomposition test and achieve good catalysis compared to business photochemical catalyst
Effect.
Advantageous effect
(1) present invention process and equipment are simple, are easy to get, short preparation period, are easy to mass produce；
(2) specific surface area of catalyst that the present invention obtains is high, and has higher visible absorption range, under visible light
Hydrogen production by water decomposition it is efficient.
Description of the drawings
Fig. 1 is Composite Pt/TiO prepared by embodiment 12-xNxThe UV-vis DRS light of catalyst and business P25
Spectrum；
Fig. 2 is Composite Pt/TiO prepared by embodiment 22-xNxThe XRD diagram of catalyst；
Fig. 3 is Composite Pt/TiO prepared by embodiment 22-xNxThe transmission electron microscope picture of catalyst；
Fig. 4 is Composite Pt/TiO prepared by embodiment 32-xNxThe Photocatalyzed Hydrogen Production of catalyst and commercial titanium dioxide P25
Curve.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) it is 1 toward 90ml volume ratios：The ethanol solution of 1 ethyl orthosilicate enters the ethyl alcohol of 4.3ml 0.1M nitric acid in adding
Solution, 70 degrees Celsius are flowed back 2 hours, are cooled to room temperature.Above-mentioned solution 90ml is taken, it is 1 that 44ml volume ratios, which are then added,：1 titanium
The ethanol solution of acid butyl ester and stirring.Be gradually added 9.2ml 0.1M nitals again, make the substance of water amount be titanium and
Twice of the sum of the amount of substance of silicon.Stand to gel is formed, obtain Ti-Si composite oxide gel, 110 DEG C of dryings, crushing,
Sieving, 600 degrees Celsius are calcined two hours.2 grams are weighed after cooling, is placed in tube furnace, and flow velocity is the flowing of 400 ml/mins
In ammonia, 900 degrees Celsius nitrogenize 5 hours, and room temperature is cooled in nitrogen protection.2.0M sodium hydroxide solutions 70 are subsequently placed in take the photograph
Family name's degree washs 12 hours, is washed to 110 degrees Celsius of drying after neutrality, obtains the mesoporous TiO of grey powder2-xNxCompound (0<x<
2) it, takes 1g grey powder to be dissolved in ultrasound 30min in 50ml ethylene glycol solutions, obtains mesoporous TiO2-xNxComplex solution.
(2) 53mg chloroplatinic acids are dissolved into 100ml ethylene glycol solutions, pH to 10 is adjusted with sodium hydroxide.It then will be upper
It states solution to be placed in micro-wave oven, 5min is heated at the power of 800W and 130 DEG C, cooled to room temperature obtains platinum nanometer
The suspension of grain.
(3) by step (1) intermediary hole TiO2-xNxComplex solution is mixed with the suspension of Pt nanoparticle in step (2),
5min is stirred, sulfuric acid is used in combination to adjust pH to 2, is then stirred at room temperature for 24 hours, through filtering, is repeatedly washed to neutrality, 80 DEG C of dryings
After obtain Composite Pt/TiO2-xNxCatalyst.
Fig. 1 shows：The Composite Pt/TiO that the present embodiment obtains2-xNxCatalyst is substantially better than business to visible absorption
TiO2(P25)。
Embodiment 2
(1) it is 1 toward 90ml volume ratios：The ethyl alcohol of 4.3ml 0.1M nitric acid is added in the ethanol solution of 1 ethyl orthosilicate
Solution, 70 degrees Celsius are flowed back 2 hours, are cooled to room temperature.Above-mentioned solution 60ml is taken, it is 1 that 44ml volume ratios, which are then added,：1 titanium
The ethanol solution of acid butyl ester and stirring.Be gradually added 9.2ml 0.1M nitals again, make the substance of water amount be titanium and
Twice of the sum of the amount of substance of silicon.Stand to gel is formed, obtain Ti-Si composite oxide gel, 110 DEG C of dryings, crushing,
Sieving, 600 degrees Celsius are calcined two hours.2 grams are weighed after cooling, is placed in tube furnace, and flow velocity is the flowing of 400 ml/mins
In ammonia, 900 degrees Celsius nitrogenize 5 hours, and room temperature is cooled in nitrogen protection.2.0M sodium hydroxide solutions 70 are subsequently placed in take the photograph
Family name's degree washs 12 hours, is washed to 110 degrees Celsius of drying after neutrality, obtains the mesoporous TiO of grey powder2-xNxCompound (0<x<
2) it, takes 1g grey powder to be dissolved in ultrasound 30min in 50ml ethylene glycol solutions, obtains mesoporous TiO2-xNxComplex solution.
(2) 53mg chloroplatinic acids are dissolved into 100ml ethylene glycol solutions, pH to 10 is adjusted with sodium hydroxide.It then will be upper
It states solution to be placed in micro-wave oven, 5min is heated at the power of 800W and 130 DEG C, cooled to room temperature obtains platinum nanometer
The suspension of grain.
(3) by step (1) intermediary hole TiO2-xNxComplex solution is mixed with the suspension of Pt nanoparticle in step (2),
3min is stirred, sulfuric acid is used in combination to adjust pH to 2, is then stirred at room temperature for 24 hours, through filtering, is repeatedly washed to neutrality, 80 DEG C of dryings
After obtain Composite Pt/TiO2-xNxCatalyst.
Fig. 2 shows：Under the calcining of 900 DEG C of high temperature, the Composite Pt/TiO that is prepared2-xNxCatalyst is still sharp
Titanium ore phase TiO2, there is no transformation of the Anatase to Rutile Type occurs.
Fig. 3 shows：The Composite Pt/TiO that the present embodiment is prepared2-xNxCatalyst has apparent pore space structure, than
Surface area is larger.
Embodiment 3
(1) it is 1 toward 90ml volume ratios：The ethyl alcohol of 4.3ml 0.1M nitric acid is added in the ethanol solution of 1 ethyl orthosilicate
Solution, 70 degrees Celsius are flowed back 2 hours, are cooled to room temperature.Above-mentioned solution 30ml is taken, it is 1 that 44ml volume ratios, which are then added,：1 titanium
The ethanol solution of acid butyl ester and stirring.Be gradually added 9.2ml 0.1M nitals again, make the substance of water amount be titanium and
Twice of the sum of the amount of substance of silicon.Stand to gel is formed, obtain Ti-Si composite oxide gel, 110 DEG C of dryings, crushing,
Sieving, 600 degrees Celsius are calcined two hours.2 grams are weighed after cooling, is placed in tube furnace, and flow velocity is the flowing of 400 ml/mins
In ammonia, 900 degrees Celsius nitrogenize 5 hours, and room temperature is cooled in nitrogen protection.2.0M sodium hydroxide solutions 70 are subsequently placed in take the photograph
Family name's degree washs 12 hours, is washed to 110 degrees Celsius of drying after neutrality, obtains the mesoporous TiO of grey powder2-xNxCompound (0<x<
2) it, takes 1g grey powder to be dissolved in ultrasound 30min in 50ml ethylene glycol solutions, obtains mesoporous TiO2-xNxComplex solution.
(2) 53mg chloroplatinic acids are dissolved into 100ml ethylene glycol solutions, pH to 10 is adjusted with sodium hydroxide.It then will be upper
It states solution to be placed in micro-wave oven, 5min is heated at the power of 800W and 130 DEG C, cooled to room temperature obtains platinum nanometer
The suspension of grain.
(3) by step (1) intermediary hole TiO2-xNxComplex solution is mixed with the suspension of Pt nanoparticle in step (2),
5min is stirred, sulfuric acid is used in combination to adjust pH to 2, is then stirred at room temperature for 24 hours, through filtering, is repeatedly washed to neutrality, 80 DEG C of dryings
After obtain Composite Pt/TiO2-xNxCatalyst.
The Composite Pt/TiO that the present embodiment is prepared2-xNxThe load capacity of platinum is 2wt% in catalyst, and Fig. 4 shows it
Water H2-producing capacity is decomposed under visible light is significantly better than business TiO2(P25)。
Embodiment 4
(1) it is 1 toward 90ml volume ratios：The ethyl alcohol of 4.3ml 0.1M nitric acid is added in the ethanol solution of 1 ethyl orthosilicate
Solution, 70 degrees Celsius are flowed back 2 hours, are cooled to room temperature.Above-mentioned solution 60ml is taken, it is 1 that 44ml volume ratios, which are then added,：1 titanium
The ethanol solution of acid butyl ester and stirring.Be gradually added 9.2ml 0.1M nitals again, make the substance of water amount be titanium and
Twice of the sum of the amount of substance of silicon.Stand to gel is formed, obtain Ti-Si composite oxide gel, 110 DEG C of dryings, crushing,
Sieving, 600 degrees Celsius are calcined two hours.2 grams are weighed after cooling, is placed in tube furnace, and flow velocity is the flowing of 400 ml/mins
In ammonia, 900 degrees Celsius nitrogenize 5 hours, and room temperature is cooled in nitrogen protection.2.0M sodium hydroxide solutions 70 are subsequently placed in take the photograph
Family name's degree washs 12 hours, is washed to 110 degrees Celsius of drying after neutrality, obtains the mesoporous TiO of grey powder2-xNxCompound (0<x<
2) it, takes 2g grey powder to be dissolved in ultrasound 30min in 50ml ethylene glycol solutions, obtains mesoporous TiO2-xNxComplex solution.
(2) 53mg chloroplatinic acids are dissolved into 100ml ethylene glycol solutions, pH to 10 is adjusted with sodium hydroxide.It then will be upper
It states solution to be placed in micro-wave oven, 5min is heated at the power of 800W and 130 DEG C, cooled to room temperature obtains platinum nanometer
The suspension of grain.
(3) by step (1) intermediary hole TiO2-xNxComplex solution is mixed with the suspension of Pt nanoparticle in step (2),
1min is stirred, sulfuric acid is used in combination to adjust pH to 2, is then stirred at room temperature for 24 hours, through filtering, is repeatedly washed to neutrality, 80 DEG C of dryings
After obtain Composite Pt/TiO2-xNxCatalyst.
Embodiment 5
(1) it is 1 toward 90ml volume ratios：The ethyl alcohol of 4.3ml 0.1M nitric acid is added in the ethanol solution of 1 ethyl orthosilicate
Solution, 70 degrees Celsius are flowed back 2 hours, are cooled to room temperature.Above-mentioned solution 30ml is taken, it is 1 that 44ml volume ratios, which are then added,：1 titanium
The ethanol solution of acid butyl ester and stirring.Be gradually added 9.2ml 0.1M nitals again, make the substance of water amount be titanium and
Twice of the sum of the amount of substance of silicon.Stand to gel is formed, obtain Ti-Si composite oxide gel, 110 DEG C of dryings, crushing,
Sieving, 600 degrees Celsius are calcined two hours.2 grams are weighed after cooling, is placed in tube furnace, and flow velocity is the flowing of 400 ml/mins
In ammonia, 900 degrees Celsius nitrogenize 5 hours, and room temperature is cooled in nitrogen protection.2.0M sodium hydroxide solutions 70 are subsequently placed in take the photograph
Family name's degree washs 12 hours, is washed to 110 degrees Celsius of drying after neutrality, obtains the mesoporous TiO of grey powder2-xNxCompound (0<x<
2) it, takes 1g grey powder to be dissolved in ultrasound 30min in 50ml ethylene glycol solutions, obtains mesoporous TiO2-xNxComplex solution.
(2) 26.5mg chloroplatinic acids are dissolved into 100ml ethylene glycol solutions, pH to 10 is adjusted with sodium hydroxide.Then will
Above-mentioned solution is placed in micro-wave oven, and 5min is heated at the power of 1000W and 120 DEG C, and cooled to room temperature obtains platinum nanometer
The suspension of particle.
(3) by step (1) intermediary hole TiO2-xNxComplex solution is mixed with the suspension of Pt nanoparticle in step (2),
5min is stirred, sulfuric acid is used in combination to adjust pH to 2, is then stirred at room temperature for 24 hours, through filtering, is repeatedly washed to neutrality, 80 DEG C of dryings
After obtain Composite Pt/TiO2-xNxCatalyst.
Embodiment 6
(1) it is 1 toward 90ml volume ratios：The ethyl alcohol of 4.3ml 0.1M nitric acid is added in the ethanol solution of 1 ethyl orthosilicate
Solution, 70 degrees Celsius are flowed back 2 hours, are cooled to room temperature.Above-mentioned solution 30ml is taken, it is 1 that 44ml volume ratios, which are then added,：1 titanium
The ethanol solution of acid butyl ester and stirring.Be gradually added 9.2ml 0.1M nitals again, make the substance of water amount be titanium and
Twice of the sum of the amount of substance of silicon.Stand to gel is formed, obtain Ti-Si composite oxide gel, 110 DEG C of dryings, crushing,
Sieving, 600 degrees Celsius are calcined two hours.2 grams are weighed after cooling, is placed in tube furnace, and flow velocity is the flowing of 400 ml/mins
In ammonia, 900 degrees Celsius nitrogenize 5 hours, and room temperature is cooled in nitrogen protection.2.0M sodium hydroxide solutions 70 are subsequently placed in take the photograph
Family name's degree washs 12 hours, is washed to 110 degrees Celsius of drying after neutrality, obtains the mesoporous TiO of grey powder2-xNxCompound (0<x<
2) it, takes 1g grey powder to be dissolved in ultrasound 30min in 50ml ethylene glycol solutions, obtains mesoporous TiO2-xNxComplex solution.
(2) 53mg potassium chloroplatinates are dissolved into 100ml ethylene glycol solutions, pH to 10 is adjusted with sodium hydroxide.Then will
Above-mentioned solution is placed in micro-wave oven, and 5min is heated at the power of 800W and 130 DEG C, and cooled to room temperature obtains platinum nanometer
The suspension of particle.
(3) by step (1) intermediary hole TiO2-xNxComplex solution is mixed with the suspension of Pt nanoparticle in step (2),
5min is stirred, hydrochloric acid is used in combination to adjust pH to 2, is then stirred at room temperature for 24 hours, through filtering, is repeatedly washed to neutrality, 80 DEG C of dryings
After obtain Composite Pt/TiO2-xNxCatalyst.
Claims (10)
1. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance2-xNxCatalyst, which is characterized in that the catalysis
Agent is the aggregate constructed by platinum grain and mesoporous nitrogen-doped titanium dioxide, and wherein the load capacity of platinum is 0.5wt%-3wt%.
2. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance2-xNxThe preparation method of catalyst, including：
(1) Ti-Si composite oxide gel is prepared with sol-gel method, Ti-Si composite oxide gel is through drying, crushing, sieving
It after calcining, is nitrogenized under ammonia atmosphere, lye is washed, and is washed, dry, obtains mesoporous TiO2-xNxCompound, by mesoporous TiO2-xNxIt is multiple
It closes object to mix with solvent, ultrasound obtains mesoporous TiO2-xNxComplex solution, wherein 0<x<2, mesoporous TiO2-xNxCompound with it is molten
The mass ratio of agent is 1:10~200；
(2) compound containing platinum is dissolved in solvent, obtains compound containing platinum solution, adjusting pH value of solution is 7-12, and then microwave adds
Heat, it is cooling, the suspension of Pt nanoparticle is obtained, the wherein ratio of compound containing platinum and solvent is 20-60mg:80-110mL；
(3) by step (1) intermediary hole TiO2-xNxComplex solution is added in step (2) in the suspension of Pt nanoparticle, is stirred
It mixes, adjusting pH value of solution is 1-6, continues to stir, and is filtered, and is washed, dry, obtains Composite Pt/TiO2-xNxCatalyst, wherein platinum
Load capacity be 0.5wt%-3wt%.
3. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that sol-gel method prepares Ti-Si composite oxide and is in the step (1)：By Butyl Phthalate
With ethyl orthosilicate respectively as the presoma of titanium dioxide and silica, titanium silicon combined oxidation is obtained by two step hydrolysis method
Object gel, the molar ratio of titanium and silicon is 1 wherein in Ti-Si composite oxide gel:3-2:1.
4. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that solvent is ethyl alcohol, ethylene glycol or isopropanol in the step (1), (2)；Alkali is hydrogen-oxygen
Change sodium or potassium hydroxide.
5. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that in the step (1) calcination temperature be 400-600 DEG C, calcination time 1-3h；When ultrasonic
Between be 5min-1h.
6. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that in the step (1) concentration of lye be 2mol/L；The flow of ammonia be 100-400 milliliters/
Minute；Nitriding temperature is 800-1000 DEG C, nitridation time 4-6h.
7. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that in the step (2) compound containing platinum be chloroplatinic acid, platinic sodium chloride or potassium chloroplatinate.
8. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that in the step (2) microwave heating power be 500-1000W, microwave heating temperature be 50~
200 DEG C, microwave heating time 1-10min.
9. a kind of Composite Pt/TiO with visible photocatalysis water hydrogen manufacturing performance according to claim 22-xNxCatalyst
Preparation method, which is characterized in that it is to use hydrochloric acid, sulfuric acid or nitric acid that pH value of solution is adjusted in the step (3), which is 1-6,；Stirring
Time is 1-5min；Continuation whipping temp is room temperature, and continuation mixing time is 1-48h.
10. a kind of Composite Pt/TiO as described in claim 1 with visible photocatalysis water hydrogen manufacturing performance2-xNxCatalyst
Using, which is characterized in that it is applied to using visible light as the photocatalytic hydrogen production by water decomposition of light source.
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