CN106238043A - The preparation of titanium dichloride load high dispersive platinum composite photocatalyst material and application process - Google Patents
The preparation of titanium dichloride load high dispersive platinum composite photocatalyst material and application process Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 title claims abstract description 15
- 230000008569 process Effects 0.000 title claims abstract description 8
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 title abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 128
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 63
- 239000002055 nanoplate Substances 0.000 claims abstract description 50
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002096 quantum dot Substances 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 230000001699 photocatalysis Effects 0.000 claims abstract description 13
- 238000007146 photocatalysis Methods 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000009833 condensation Methods 0.000 claims abstract description 9
- 230000005494 condensation Effects 0.000 claims abstract description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000011238 particulate composite Substances 0.000 claims abstract description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 16
- 229940043267 rhodamine b Drugs 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- VSQYNPJPULBZKU-UHFFFAOYSA-N mercury xenon Chemical compound [Xe].[Hg] VSQYNPJPULBZKU-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 14
- 238000006731 degradation reaction Methods 0.000 abstract description 14
- 239000003054 catalyst Substances 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000000975 dye Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 229910000510 noble metal Inorganic materials 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000007857 degradation product Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- -1 platinum ion Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical compound C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- VKFAUCPBMAGVRG-UHFFFAOYSA-N dipivefrin hydrochloride Chemical compound [Cl-].C[NH2+]CC(O)C1=CC=C(OC(=O)C(C)(C)C)C(OC(=O)C(C)(C)C)=C1 VKFAUCPBMAGVRG-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000002351 wastewater Substances 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—
-
- B01J35/399—
-
- B01J35/40—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The preparation of a kind of titanium dichloride load high dispersive platinum composite photocatalyst material and application process, belong to field of titanium dioxide photocatalysis.Butyl titanate is stirred together with Fluohydric acid. by the method at normal temperatures, puts into 150～220 DEG C of reactions 15～24h in hydrothermal reaction kettle, obtains titanium dioxide nanoplate after separating, washing, drying；Titanium dioxide nanoplate is dispersed in without in water glycol again, 10～60min are stirred at 80～150 DEG C of reflux condensation modes, add polyvinylpyrrolidone and chloroplatinic acid, continue reflux condensation mode stirring 3～10h at 80～150 DEG C, after separating, washing, drying, obtain titanium dioxide nanoplate supported platinum nano particulate composite.The method can obtain the titanium dioxide nanoplate that pattern is easily-controllable, by ethylene glycol as reducing agent be readily available even particle size distribution, have polymolecularity 2～3nm platinum quantum dot, preparation parameter is easily controllable, reproducible.The catalyst prepared is particularly well-suited to ultraviolet light and irradiates lower catalytic degradation organic dyestuff, reaches the highest degradation rate.
Description
Technical field
The present invention relates to field of titanium dioxide photocatalysis, particularly to titanium dioxide nanoplate carried noble metal composite
Field.The catalyst that the method is prepared is particularly well-suited to ultraviolet light and irradiates lower catalytic degradation organic dyestuff (such as: rhodamine B),
Reach the highest degradation rate.
Background technology
At present, titanium dioxide optical catalyst causes domestic and international researcher because having the advantage such as stable, nontoxic, inexpensive
Extensive concern, has broad application prospects in fields such as waste water process, air cleaning, antibacterial and deodouring, automatically cleanings.Anatase
Single crystal titanium dioxide nanometer sheet has obtained the biggest concern due to high energy active face (001) large percentage.Theory and experimentation
Show compared to other active face, (001) face can more efficiently adsorption reaction thing molecule, promote the carrying out of catalytic reaction.
But relatively low photo-quantum efficiency and slower reaction rate limit the actual application of titanium dioxide.Photoproduction current-carrying
The migration of son, capture and be compound between competition determine titanium dioxide nanoplate light-catalyzed reaction quantum efficiency height and
The speed of reaction rate, and titanium dioxide-noble metal compound system is because having special contact interface structure and chemistry and electronics
Character and be widely applied in catalytic reaction.
Titanium dioxide-noble metal systems has two kinds of complex methods: the titanium that (1) precious metal atom replaces in titanium dioxide is former
Son；(2) noble metal loading is at titanium dioxide surface.The method that noble metal loading is conventional has photoreduction met hod and conventional impregnation reduction
Method.Photoreduction met hod is quasiconductor to be immersed in precious metal salt and sacrifices the molten of Organic substance (free radical aceeptor, such as acetic acid, methanol etc.)
In liquid, under ultraviolet light irradiates, noble metal is reduced and is deposited on titanium dioxide surface；Conventional impregnation reducing process is by dioxy
Change titanium to be immersed in the solution containing precious metal salt, under inert gas shielding, then use hydrogen high temperature reduction.Your conventional gold
Owner to include Pt, Ag, Au, Pd, Ru etc. of the 3rd main group, and wherein the report about supporting Pt is most, and effect is preferably also.
Etc. (Zhang Jinlong, security positive, the research in propine photocatalysis hydrolysis of the noble-metal-supported photocatalyst,
SCI) use aqueous impregnation method that P25 adsorbs platinum ion, after being evaporated by solvent, put into Muffle furnace
Middle high-temperature hot reduction platinum ion is to reach the purpose of loading platinum on P25 nano-particle.The method is relatively complicated, energy
Amount consumes more, and platinum is skewness on P25.
(Wang Yan, Chen Xuanli, Wen Lixiong, Chen Jianfeng, the preparation of mesoporous silicon oxide coated with silver nano-particle and antibacterial such as king
Performance, natural science report) use the method for sodium hypophosphite liquid-phase reduction to be prepared for nano silver colloidal sol, with cetyl trimethyl bromine
Change ammonium is template, grows silica shell with tetraethyl orthosilicate at Argent grain surface in situ, finally utilizes solution extraction
Remove organic formwork agent again.But the method is relatively complicated, uses reagent consumption many, put in production application the biggest
Distance.
The present invention combines the work of forefathers, uses the method for solution impregnation to be prepared for a kind of polymolecularity platinum quantum dot uniform
The high-effect photocatalyst being supported on titanium dioxide nanoplate.
Summary of the invention
The invention provides the preparation of a kind of titanium dioxide nanoplate load high dispersive platinum quantum dot composite photocatalyst material
Method, makes the titanium dioxide nanoplate catalyst of Supported Pt Nanoparticles have the visible light photocatalysis performance of excellence.
A kind of titanium dioxide nanoplate load polymolecularity platinum quantum dot composite photocatalyst material preparation method, including with
Lower step:
1) butyl titanate is stirred together with Fluohydric acid. at normal temperatures, put in hydrothermal reaction kettle 150～220 DEG C
Reaction 15～24h, obtains titanium dioxide nanoplate after separating, washing, drying.
2) by step 1) in titanium dioxide nanoplate be dispersed in without in water glycol, 80～150 DEG C of returned cold
Solidifying stirring 10～60min, adds polyvinylpyrrolidone and chloroplatinic acid, continues stirring 3～10h at 80～150 DEG C, separated,
Wash, obtain titanium dioxide nanoplate supported platinum nano particulate composite after drying.
Step 1) in, as preferably, described butyl titanate, Fluohydric acid. mass ratio are 1:0.1～0.3:.Be conducive to
Different and the preferable titanium dioxide nanoplate of crystallinity to size, so that the titanium dioxide nanoplate load of final preparation
Polymolecularity platinum quantum dot composite material has preferable photocatalysis performance.Further preferably, described butyl titanate, hydrogen fluorine
The mass ratio of acid is 1:0.2～0.25.Be conducive to obtaining size difference and the preferable titanium dioxide nanoplate of crystallinity, thus
The titanium dioxide nanoplate finally prepared load polymolecularity platinum quantum dot composite material is made to have more preferable photocatalysis performance.
As preferably, 150～220 DEG C of reactions 15～24h in pyroreaction still, by the method for Hydrothermal Synthesis, at this
Reacting under optimum condition, be conducive to obtaining crystallinity preferable, pattern is than more uniform titanium dioxide nanoplate.Further preferably, exist
200～220 DEG C of reactions 20～22h in pyroreaction still, it is possible to obtain crystallinity more preferable, be conducive to obtaining pattern more uniform
Titanium dioxide nanoplate.
Step 2) in, as preferably, described titanium dioxide nanoplate, without water glycol, polyvinylpyrrolidone, chlorine platinum
The mass ratio of acid is 1:270～300:0.8～1.0:0.1～0.15, is conducive to obtaining higher being combined of platinum quantum dot dispersibility
Material, thus embody good photocatalytic activity.Further preferably, described titanium dioxide nanoplate, without water glycol, poly-
Vinylpyrrolidone, the mass ratio of chloroplatinic acid are 1:285～290:0.9～0.95:0.13～0.14.Be conducive to obtaining high dispersive
Property platinum quantum dot composite material, thus embody more preferable photocatalytic activity.
As preferably, continue reflux condensation mode stirring 3～10h at 80～150 DEG C, react under this optimum condition, be conducive to
The growth of suppression metal platinum, promotes the formation of platinum quantum dot.Further preferably, reflux condensation mode stirring 5 is continued at 100～115 DEG C
～6h, advantageously form pattern uniform, there is the optic catalytic composite material of polymolecularity platinum point distribution.
Titanium dioxide nanoplate load high dispersive platinum quantum dot composite photo-catalyst prepared by the present invention is applied to photocatalysis
Degradation experiment, with ultraviolet light as light source, rhodamine B is that target degradation product carries out photocatalytic degradation process, achieves well fall
Solve effect.
The titanium dioxide nanoplate composite photo-catalyst that the high dispersive platinum quantum dot using the present invention to prepare loads, dioxy
Change the separation efficiency that can effectively improve electron-hole between titanium and platinum quantum dot, thus improve photo-quantum efficiency.Noble metal
The load of platinum can increase the catalyst absorption to visible ray, makes material have stronger photocatalytic activity.This preparation method energy
Enough well obtain, by simple hydro-thermal reaction, the titanium dioxide nanoplate that pattern is easily-controllable, by ethylene glycol as reducing agent very
Be readily available even particle size distribution, have polymolecularity 2～3nm platinum quantum dot, preparation parameter is easily controllable, repeatability
Good.
Catalyst carrier of the present invention is the titanium dioxide nanoplate utilizing hydro-thermal reaction method to prepare, size be about 70～
80nm, for Anatase structure, with chloroplatinic acid for platinum source, utilizes reduction of ethylene glycol to obtain platinum quantum dot and is highly dispersed at titanium dioxide
Composite in titanium nanometer sheet, platinum quantum dot size is about 2～3nm.Dioxy by the high dispersive platinum quantum dot load of preparation
Changing titanium nanosheet photocatalyst and be applied to photocatalytic degradation experiment, with ultraviolet light as light source, rhodamine B is that target degradation product is carried out
Photocatalytic degradation processes, and compared to business photocatalyst, achieves good degradation effect.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture (TEM) of the titanium dioxide nanoplate of embodiment 1 preparation
Fig. 2 is the transmission electron microscope of the titanium dioxide nanoplate load high dispersive platinum quantum dot composite material of embodiment 1 preparation
Figure (TEM)
Fig. 3 is the titanium dioxide nanoplate load high dispersive platinum quantum dot composite material high-resolution transmission of embodiment 1 preparation
Electronic Speculum figure (HRTEM)
Fig. 4 is the EDS figure of the titanium dioxide nanoplate load high dispersive platinum quantum dot composite material of embodiment 1 preparation
Fig. 5 is the photocatalysis fall of the titanium dioxide nanoplate load high dispersive platinum quantum dot composite material of embodiment 1 preparation
Solution curve.
Detailed description of the invention
Below in conjunction with example, the method for the present invention is further described.These examples have further described and demonstrated this
Embodiment in invention scope.The purpose that the example be given is merely to illustrate, does not constitute any restriction, is not carrying on the back the present invention
Under conditions of spirit and scope of the invention, it can be carried out various change.
Embodiment 1
(1) being added by the Fluohydric acid. that 5ml mass fraction is 40% in the butyl titanate of 25ml, at 25 DEG C, stirring is all
Even, put in the autoclave of 100ml, 200 DEG C of reaction 20h.After question response terminates, with deionized water and ethanol purge in
Property, obtain titanium dioxide nanoplate powder after drying.
(2) ethylene glycol measuring 10ml heats 30min in round-bottomed flask in 110 DEG C of oil bath pans, and condensing reflux removes
Unnecessary water.Then weigh the titanium dioxide nanoplate powder that 0.25g prepares, be distributed in 5ml ethylene glycol use ultrasonic disperse
Uniformly, being subsequently adding 110 DEG C of heating 30min in above-mentioned round-bottomed flask, condensing reflux removes unnecessary water.Weigh 0.033g simultaneously
Chloroplatinic acid and 0.225g polyvinylpyrrolidone, be then respectively adding in 1ml ethylene glycol solution, ultrasonic 30min, by chloroplatinic acid
It is simultaneously introduced in the ethylene glycol solution containing titanium dioxide nanoplate with polyvinylpyrrolidone, condensing reflux, 110 DEG C of reactions
5h。
The scanned Electronic Speculum of products obtained therefrom (SEM) analyze show, the size of titanium dioxide prepared by this method be about 70～
80nm, uniform sheet shape structure, surface is relatively smooth.The rear surface of deposition platinum quantum dot becomes coarse, can from transmission electron microscope
Knowing, the platinum grain of deposition is 2～about 3nm, and distribution height is uniform, does not has agglomeration to occur.
The titanium dioxide nanoplate load high dispersive platinum quantum dot composite catalyst weighing the above-mentioned preparation of 0.02g carries out light and urges
Changing the experiment of rhodamine B degradation, rhodamine B concentration is 5mg L-1, after ultraviolet light irradiation 80min, the degradation rate of rhodamine B is
97.0%.
Embodiment 2
High dispersive platinum quantum dot carried titanium dioxide nanometer sheet method for preparing composite catalyst, step is with embodiment 1, different
Part is: the quality of chloroplatinic acid used is 0.017g
The titanium dioxide nanoplate load high dispersive platinum quantum dot composite catalyst weighing the above-mentioned preparation of 0.02g carries out light and urges
Changing the experiment of rhodamine B degradation, rhodamine B concentration is 5mg L-1, after ultraviolet light irradiation 80min, the degradation rate of rhodamine B is
91.0%.
Embodiment 3
High dispersive platinum quantum dot carried titanium dioxide nanometer sheet method for preparing composite catalyst, step is with embodiment 1, different
Part is: the quality of chloroplatinic acid used is 0.083g.
The titanium dioxide nanoplate load high dispersive platinum quantum dot composite catalyst weighing the above-mentioned preparation of 0.02g carries out light and urges
Changing the experiment of rhodamine B degradation, rhodamine B concentration is 5mg L-1, after ultraviolet light irradiation 80min, the degradation rate of rhodamine B is
66.4%.
Embodiment 4
The preparation method of high dispersive platinum quantum dot carried titanium dioxide nanosheet photocatalyst, step is with embodiment 1, different
Part is: the quality of chloroplatinic acid used is 0.008g.
The titanium dioxide nanoplate load high dispersive platinum quantum dot composite catalyst weighing the above-mentioned preparation of 0.02g carries out light and urges
Changing the experiment of rhodamine B degradation, rhodamine B concentration is 5mg L-1, after ultraviolet light irradiation 80min, the degradation rate of rhodamine B is
85.9%.
Claims (8)
1. the preparation method of titanium dioxide nanoplate load high dispersive platinum composite photocatalyst material, it is characterised in that include with
Lower step:
1) butyl titanate is stirred together with Fluohydric acid. at normal temperatures, put into 150～220 DEG C of reactions in hydrothermal reaction kettle
15～24h, obtain titanium dioxide nanoplate after separating, washing, drying；
2) by step 1) in titanium dioxide nanoplate be dispersed in without in water glycol, stir at 80～150 DEG C of reflux condensation modes
Mix 10～60min, add polyvinylpyrrolidone and chloroplatinic acid, continue reflux condensation mode stirring 3～10h at 80～150 DEG C, through dividing
From, washing, obtain titanium dioxide nanoplate supported platinum nano particulate composite after drying；
Wherein step 1) in, described butyl titanate, Fluohydric acid. mass ratio are 1:0.1～0.3.
The preparation method of titanium dioxide nanoplate the most according to claim 1 load high dispersive platinum composite photocatalyst material,
It is characterized in that, described butyl titanate, Fluohydric acid. 1:0.2～0.25.
The preparation method of titanium dioxide nanoplate the most according to claim 1 load high dispersive platinum composite photocatalyst material,
It is characterized in that, step 1) in, 150～220 DEG C of reactions 15～24h in hydrothermal reaction kettle.
The preparation method of titanium dioxide nanoplate the most according to claim 3 load high dispersive platinum composite photocatalyst material,
It is characterized in that, 200～210 DEG C of reactions 20～21h in hydrothermal reaction kettle.
The preparation method of titanium dioxide nanoplate the most according to claim 1 load high dispersive platinum composite photocatalyst material,
It is characterized in that, step 2) described in titanium dioxide nanoplate, without water glycol, polyvinylpyrrolidone, the matter of chloroplatinic acid
Amount ratio is 1:270～300:0.8～1.0:0.1～0.15.
Preparation method the most according to claim 5, it is characterised in that described titanium dioxide nanoplate, without water glycol,
Polyvinylpyrrolidone, the mass ratio of chloroplatinic acid are 1:285～290:0.9～0.95:0.13～0.14.
The preparation method of titanium dioxide nanoplate the most according to claim 1 load high dispersive platinum composite photocatalyst material,
It is characterized in that, continue reflux condensation mode stirring 5～6h at 100～115 DEG C.
8. the titanium dioxide nanoplate load high dispersive platinum photocatalysis prepared according to method described in any one of claim 1～7 is multiple
Application process in condensation material photocatalysis, it is characterised in that be by multiple for 20mg titanium dioxide nanoplate load high dispersive platinum quantum dot
Condensation material adds in the rhodamine B aqueous solution that concentration is 5mg/L, and ultrasonic disperse uniformly rear dark reaction 40min, absorption to be achieved is put down
During weighing apparatus, it is positioned over 300w wavelength and carries out light-catalyzed reaction less than under the xenon-mercury lamp of 420nm.
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