CN108499582A - A kind of preparation method of composite photo-catalyst - Google Patents
A kind of preparation method of composite photo-catalyst Download PDFInfo
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- CN108499582A CN108499582A CN201810293695.5A CN201810293695A CN108499582A CN 108499582 A CN108499582 A CN 108499582A CN 201810293695 A CN201810293695 A CN 201810293695A CN 108499582 A CN108499582 A CN 108499582A
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 41
- 239000010936 titanium Substances 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 35
- 235000019441 ethanol Nutrition 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012153 distilled water Substances 0.000 claims abstract description 23
- 238000013019 agitation Methods 0.000 claims abstract description 21
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 21
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 19
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005864 Sulphur Substances 0.000 claims abstract description 13
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 10
- 239000011737 fluorine Substances 0.000 claims abstract description 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 238000002604 ultrasonography Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 claims description 10
- 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 description 7
- -1 Titanium alkoxides Chemical class 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- PQJCUFBNSPVIEG-UHFFFAOYSA-N [O-2].[Cd+2].[O-2].[Ti+4] Chemical compound [O-2].[Cd+2].[O-2].[Ti+4] PQJCUFBNSPVIEG-UHFFFAOYSA-N 0.000 claims description 6
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 6
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 5
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 235000013878 L-cysteine Nutrition 0.000 claims description 4
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000004201 L-cysteine Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 125000001153 fluoro group Chemical group F* 0.000 claims 1
- 235000015424 sodium Nutrition 0.000 claims 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052980 cadmium sulfide Inorganic materials 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 10
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract 2
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000000975 dye Substances 0.000 abstract 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 13
- 230000035484 reaction time Effects 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical group S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- AJVCUHHHRPBRHU-UHFFFAOYSA-N cadmium nitric acid Chemical compound [Cd].[N+](=O)(O)[O-] AJVCUHHHRPBRHU-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 150000008538 L-cysteines Chemical class 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000003483 aging Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910000331 cadmium sulfate Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- SGJUCMOYVKXLDY-UHFFFAOYSA-N acetic acid;cadmium Chemical compound [Cd].CC(O)=O.CC(O)=O SGJUCMOYVKXLDY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910000238 buergerite Inorganic materials 0.000 description 1
- HUKFCVYEXPZJJZ-UHFFFAOYSA-N cadmium;hydrate Chemical compound O.[Cd] HUKFCVYEXPZJJZ-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- B01J35/40—
-
- B01J35/51—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of preparation methods of composite photo-catalyst, belong to field of material technology；This method first dissolves graphene with titanium source with ethyl alcohol, and Fluorine source is dissolved in distilled water, is allowed to be uniformly dispersed by ultrasonic agitation after the two is mixed, the Fluorin doped titanium dioxide graphene of high-energy surface must be exposed using microwave solvothermal legal system；Then by cadmium source and sulphur source difference spent glycol dissolving, the Fluorin doped titanium dioxide graphene that gained is exposed to high-energy surface is mixed under the conditions of ultrasonic agitation, and the Fluorin doped titanium dioxide wurtzite-type cadmium sulfide graphene composite photocatalyst of high-energy surface must be exposed by microwave solvothermal legal system；The present invention has many advantages, such as that simple for process, preparation time is short, efficient, safe and reliable, synthesized composite photo-catalyst has the characteristics that morphology controllable and high-specific surface area, organic matter that can be in efficient absorption waste water from dyestuff is simultaneously broken down into water and carbon dioxide under visible light, has application prospect in sewage treatment field.
Description
Technical field
The invention belongs to the technical fields of graphene composite photocatalyst material preparation method, are related to a kind of exposed high-energy surface
Fluorin doped titanium dioxide-cadmium sulfide-graphene composite photocatalyst material preparation method.
Background technology
The environmental problem caused by waste water and exhaust gas by the industry such as the consumption and printing and dyeing of fossil energy, papermaking at
For current urgent problem to be solved.Photocatalysis technology is due to its energy source is green, environmentally friendly in production hydrogen, water pollution control
Equal fields are by numerous studies.Titanium dioxide（TiO2）It is to grind at present because it is with Strong oxdiative ability and nontoxic, chemical property stabilization
Study carefully one of conductor photocatalysis material most, that use scope is most wide.But pure TiO2Due to energy gap（3.2 eV）It is wider, and
It is low to the utilization rate of sunlight.Cadmium sulfide（CdS）Although energy gap（2.4 eV）It is relatively narrow, to visible light-responded wider range,
But single CdS easily reunites, there are photoetch, be oxidized easily, chemical stability is poor and limits its actual use.It is existing
Some research confirms CdS loading to TiO2Surface can overcome CdS and TiO to a certain extent2Respective disadvantage and effectively enhance
Photocatalytic activity.The features such as due to special electronic conductivity energy, high mechanical strength, large specific surface area, catalyst is loaded to
Graphene surface can effective limiting catalyst particle size and caking, further guide electron-hole pair according to certain road
Line migrates, and promotes absorption of the catalyst to visible light, and then improve the photochemical properties of catalyst.
106215920 A of Chinese patent application discloses a kind of porous graphene carried titanium dioxide composite material and its system
Titanium source is dissolved in dilute sulfuric acid by Preparation Method, this method first, with graphene quantum dot suspension ultrasonic mixing, heating, ageing, clear
After washing, drying, then handled with microwave-hydrothermal method to obtain the graphene quantum of carried titanium dioxide.Then with water, acetone or
Dimethyl sulfoxide (DMSO) is that solvent newly configures graphene dispersion solution, then the graphene quantum dot of previous gained carried titanium dioxide is added
Enter into graphene dispersing solution, then handles through hydro-thermal method to obtain product.This method is in the mistake for preparing graphene quantum dot suspension
The reagents such as the concentrated sulfuric acid, acetone are used in journey, the wherein concentrated sulfuric acid has certain risk, more demanding to working condition；Wherein
Acetone and dimethyl sulfoxide (DMSO) are toxic reagent, and acetone, the concentrated sulfuric acid, potassium permanganate belong to controlled easily toxicant processed；It should
Method be related to mixing, heating, ageing and etc., the process is more complicated.105688937 A of Chinese patent application discloses one kind two
The preparation method of titanium oxide-graphene-sulfur cadmium composite material, this method directly disperse finished product titanium dioxide in ethanol,
It flows back a few hours after adding silane coupling agent, titanium dioxide graphene oxide is mixed to obtain with graphite oxide dispersion after washed
Compound.Then in ethanol by gained titanium dioxide graphene oxide compound, four water cadmium nitrates, sulphur powder dispersion, xenon lamp shines
Through washing, centrifugation, drying after penetrating 2 hours, titanium dioxide-graphene-sulfur cadmium composite material is finally obtained.This method is directly adopted
With finished titanium dioxide synthesizing graphite alkene titanium dioxide, obtained catalysis material caking, particle is uneven, particle size is larger,
Its structure, pattern, dimensional controllability be not strong；In addition, this method is related to the processes such as heating, reflux, although technique is relatively easy,
Compare that preparation time is longer, combined coefficient is low with two step microwave solvothermal methods.
Invention content
The object of the present invention is to provide a kind of Fluorin doped of exposed high-energy surface titanium dioxide-cadmium sulfide-graphene complex lights
The preparation method of catalyst, to solve for the disadvantage and the deficiencies in the prior art present in single semiconductor, this method exists
It is efficiently easy-to-use in industrial process.
Fluorin doped titanium dioxide-cadmium sulfide-graphene composite photocatalyst that the present invention exposes high-energy surface is with graphene
For catalyst carrier, cadmium sulfide and titanium dioxide are active component, are made using two step microwave solvothermal methods；
Preparation method is as follows：
（1）0.003-0.006 mol titanium sources and 10-25mg graphene oxides is taken to be distributed in absolute ethyl alcohol under ultrasound condition,
It takes the Fluorine source of 0.003-0.006 mol to be dissolved in distilled water, Fluorine source solution is then added drop-wise to the mixed of titanium source and graphene oxide
It closes in liquid, ultrasonic agitation is allowed to uniformly mix after being added dropwise to complete；Then by mixed liquor dislocation in focusing in single mold microwave synthesizer
It is reacted, waits filtering sample after the completion of reacting, wash, be dried in vacuo the Fluorin doped titanium dioxide for obtaining exposing high-energy surface
Titanium-graphene complex；
（2）It is distributed to second two respectively under ultrasound condition by the mol cadmiums sources 0.003-0.006 and by 0.005-0.015 mol sulphur sources
In alcohol, sulphur source solution is added drop-wise in the solution of cadmium source under the conditions of ultrasonic agitation, then by step（1）Fluorin doped titanium dioxide-
Graphene complex is distributed in above-mentioned solution, and ultrasonic agitation is allowed to uniformly mix after the completion of all reagent mixing；After mixing
Solution moves into focus to react in single mold microwave synthesizer, waits filtering sample after the completion of reacting, wash, being dried in vacuo and obtain
Fluorin doped titanium dioxide-wurtzite-type cadmium sulfide-graphene composite photocatalyst of exposure high-energy surface.
The step（1）Middle titanium source is one kind in titanium tetrachloride, Titanium Nitrate, Titanium alkoxides；Fluorine source is ammonium fluoride, calcirm-fluoride
In one kind；The drop rate of Fluorine source solution is 5 mL/ 30min, and the ultrasonic agitation time is 5 ~ 30 min, and supersonic frequency is
30 ~ 50 kHz, it is 250 ~ 450 W to focus microwave power in single mold microwave synthesizer, and reaction temperature is 100 ~ 150 DEG C,
Reaction time is 30 ~ 60 min, and suction filtration is filtered using miillpore filter, and washing washs 3 respectively using ethyl alcohol and distilled water
Secondary, vacuum drying temperature is 60 ~ 90 DEG C.
The step（2）Middle cadmium source is one kind in cadmium sulfate, cadmium nitrate, cadmium acetate；Sulphur source is vulcanized sodium, thiosulfuric acid
One kind in sodium, L-cysteine；The drop rate of sulphur source solution is 5 mL/30 min, and the ultrasonic agitation time is 5 ~ 30
Min, it is 30 ~ 50 kHz to focus supersonic frequency in single mold microwave synthesizer, and microwave power is 250 ~ 450 W, reaction temperature
Be 100 ~ 150 DEG C, the reaction time be 30 ~ 60 min, suction filtration filtered using miillpore filter, washing using ethyl alcohol with
Distilled water washs 3 times respectively, and vacuum drying temperature is 60 ~ 90 DEG C.
The advantage of the invention is that：
Source chemicals and preparation method selected by the present invention be simple and efficient it is easy-to-use, can the structure of Effective Regulation catalyst, pattern,
Particle size.Obtained by titanium dioxide-cadmium sulfide-graphene composite photocatalyst material and other methods obtained by the present invention
Composite material is compared, and structure is the nanoporous nucleocapsid of cadmium sulfide cladding titanium dioxide；Its titania additive fluorine member
Element；Its titanium dioxide exposes high-energy surface（001）Crystal face；Its cadmium sulfide is wurtzite-type crystalline phase.Nanoporous nucleocapsid has
The high feature of large specific surface area, photocatalysis performance；Fluorin doped titania structure is conducive to catalyst light compared to pure titinium dioxide
Chemism；Titanium dioxide exposes under normal conditions（101）Crystal face, the present invention obtained by titanium dioxide expose high-energy surface
（001）Crystal face has better photocatalytic activity；Buergerite phase cadmium sulfide is conducive to photocatalysis compared to a cube mine phase cadmium sulfide.
Description of the drawings
Fig. 1 is the Fluorin doped titanium dioxide-for the exposure high-energy surface that differential responses temperature and time synthesizes in embodiment 3 and 5
Wurtzite-type cadmium sulfide-graphene composite photocatalyst is to methylene blue（MB）Degradation curve；
Fig. 2 is Fluorin doped titanium dioxide-wurtzite-type cadmium sulfide-graphite of exposure high-energy surface prepared by 3 present invention of the present embodiment
The transmission electron microscope picture of alkene composite photocatalyst material；
Fig. 3 is Fluorin doped titanium dioxide-wurtzite-type cadmium sulfide-graphite of exposure high-energy surface prepared by 3 present invention of the present embodiment
The transmission electron microscope picture of alkene composite photocatalyst material；
Fig. 4 is Fluorin doped titanium dioxide-wurtzite-type cadmium sulfide-graphite of exposure high-energy surface prepared by 3 present invention of the present embodiment
The scanning electron microscope (SEM) photograph of alkene composite photocatalyst material.
Fig. 5 is Fluorin doped titanium dioxide-wurtzite-type cadmium sulfide-of exposure high-energy surface prepared by 3 present invention of the present embodiment
The scanning power spectrum and constituent content figure of graphene composite photocatalyst material.
Specific implementation mode
Below by drawings and examples, invention is further described in detail, but protection scope of the present invention is not limited to
In the content.
Embodiment 1
It takes 0.003 mol Titanium Nitrates and 10 mg graphene oxides to be distributed in ethyl alcohol under ultrasound environments, takes 0.003 mol's
Ammonium fluoride is dissolved in distilled water, and ammonium fluoride solution is then added drop-wise to Titanium Nitrate and oxidation with the rate of addition of 5 mL/30 min
In the mixed liquor of graphene, 5 min are stirred by ultrasonic after being added dropwise to complete and are allowed to uniformly mix, supersonic frequency is 30 kHz, then will
Mixed liquor, which moves into, to be focused in single mold microwave synthesizer, sets microwave power to 250 W, and reaction temperature is 100 DEG C, when reaction
Between be 40min, wait for that reaction is finished and filtered to sample with miillpore filter, washed respectively 3 times, 60 DEG C using distilled water and ethyl alcohol
Lower freeze-day with constant temperature obtains exposing Fluorin doped titanium dioxide-graphene complex of high-energy surface；By 0.003 mol cadmium sulfates and incite somebody to action
0.005 mol sodium thiosulfate is distributed in ethylene glycol respectively under ultrasound environments；By thiosulfuric acid under the conditions of ultrasonic agitation
Sodium solution is added drop-wise to the rate of addition of 5 mL/30 min in cadmium sulfate solution, and by step（1）Middle gained exposure high-energy surface
In Fluorin doped titanium dioxide-graphene dispersion to above-mentioned solution, 5 min of ultrasonic agitation are allowed to uniform after the completion of all reagent mixing
Mixing, supersonic frequency are 30 kHz；Then acquired solution is moved into and is focused in single mold microwave synthesizer, sets microwave power to
250 W, reaction temperature are 100 DEG C, and the reaction time is 40 min, wait for that reaction is finished and are filtered to sample with miillpore filter, are adopted
Fluorin doped titanium dioxide-fibre zinc that freeze-day with constant temperature at 3 times, 60 DEG C obtains exposing high-energy surface is washed respectively with distilled water and ethyl alcohol
Mine type cadmium sulfide-graphene composite photocatalyst.
Embodiment 2
0.004 mol titanium tetrachlorides and 15 mg graphene oxides is taken to be distributed in ethyl alcohol under ultrasound environments.Take 0.005 mol
Ammonium fluoride be dissolved in distilled water.Then with the rate of addition of 10mL/30 min by ammonium fluoride solution be added drop-wise to titanium tetrachloride and
In the mixed liquor of graphene oxide, 10 min are stirred by ultrasonic after being added dropwise to complete and are allowed to uniformly mix, supersonic frequency is 30 kHz.With
Mixed liquor is moved into afterwards and is focused in single mold microwave synthesizer, sets microwave power to 300 W, reaction temperature is 110 DEG C, instead
It is 35 min between seasonable, waits for that reaction is finished and sample is filtered with miillpore filter, 3 are washed respectively using distilled water and ethyl alcohol
Secondary, freeze-day with constant temperature obtains exposing Fluorin doped titanium dioxide-graphene complex of high-energy surface at 65 DEG C.By 0.004 mol nitric acid
Cadmium and 0.008 mol sodium thiosulfate is distributed in ethylene glycol respectively under ultrasound environments；By sulphur under the conditions of ultrasonic agitation
Sodium thiosulfate solution is added drop-wise to the rate of addition of 5 mL/30 min in nitric acid cadmium solution, and by step（1）Middle gained exposure is high
In the Fluorin doped titanium dioxide-graphene dispersion to above-mentioned solution in energy face, 10 min are stirred by ultrasonic after the completion of all reagents mixing
It is allowed to uniformly mix, supersonic frequency is 30 kHz.Then acquired solution is moved into and is focused in single mold microwave synthesizer, by microwave work(
Rate is set as 300 W, and reaction temperature is 110 DEG C, and the reaction time is 35 min, wait for reaction finish with miillpore filter to sample into
Row filters, and the Fluorin doped dioxy that freeze-day with constant temperature at 3 times, 65 DEG C obtains exposing high-energy surface is washed respectively using distilled water and ethyl alcohol
Change titanium-wurtzite-type cadmium sulfide-graphene composite photocatalyst.
Embodiment 3
0.005 mol Titanium alkoxides and 20 mg graphene oxides are taken to be distributed in ethyl alcohol under ultrasound environments.Take 0.006 mol's
Calcirm-fluoride is dissolved in distilled water.Then calcium fluoride melt solution is added drop-wise to by Titanium alkoxides and oxidation with the rate of addition of 15 mL/30 min
In the mixed liquor of graphene, 15 min are stirred by ultrasonic after being added dropwise to complete and are allowed to uniformly mix, supersonic frequency is 35 kHz.Then will
Mixed liquor, which moves into, to be focused in single mold microwave synthesizer, sets microwave power to 300 W, and reaction temperature is 120 DEG C, when reaction
Between be 40 min, wait for that reaction is finished and filtered to sample with miillpore filter, 3 times washed respectively using distilled water and ethyl alcohol, 70
Freeze-day with constant temperature obtains exposing Fluorin doped titanium dioxide-graphene complex of high-energy surface at DEG C.By 0.004 mol cadmium nitrates and incite somebody to action
0.01 mol L-cysteines are distributed in ethylene glycol respectively under ultrasound environments.By half Guang ammonia of L- under the conditions of ultrasonic agitation
Acid solution is added drop-wise to the rate of addition of 15 mL/30 min in nitric acid cadmium solution, and by step（1）Middle gained exposes high-energy surface
Fluorin doped titanium dioxide-graphene dispersion to above-mentioned solution in, 15 min of ultrasonic agitation are allowed to after the completion of the mixing of all reagents
Uniformly mixing, supersonic frequency are 35 kHz.Then acquired solution is moved into and is focused in single mold microwave synthesizer, microwave power is set
300 W are set to, reaction temperature is 120 DEG C, and the reaction time is 40 min, waits for that reaction is finished and is taken out to sample with miillpore filter
Filter washs the Fluorin doped titanium dioxide-that freeze-day with constant temperature at 3 times, 70 DEG C obtains exposing high-energy surface respectively using distilled water and ethyl alcohol
Wurtzite-type cadmium sulfide-graphene composite photocatalyst.Cadmium sulfide, titanium dioxide, graphene are mutually tied as can see from Figure 2
Conjunction forms tri compound structure, and titanium dioxide life is box structure, mainly exposes its high-energy surface（001）Crystal face；It can be with from Fig. 3
See that cadmium sulfide is coated on titanium dioxide surface and forms nanoporous nucleocapsid；Be in Fig. 4 obtained composite catalyst
Pattern under large scale and structure；Fig. 5 is the content of the middle each component element of obtained composite catalyst.
Embodiment 4
0.006 mol Titanium alkoxides and 25 mg graphene oxides are taken to be distributed in ethyl alcohol under ultrasound environments.Take 0.003 mol's
Ammonium fluoride is dissolved in distilled water.Then ammonium fluoride solution is added drop-wise to by Titanium alkoxides and oxidation with the rate of addition of 20 mL/30 min
In the mixed liquor of graphene, 20 min are stirred by ultrasonic after being added dropwise to complete and are allowed to uniformly mix, supersonic frequency is 40 kHz.Then will
Mixed liquor, which moves into, to be focused in single mold microwave synthesizer, sets microwave power to 350 W, and reaction temperature is 130 DEG C, when reaction
Between be 45 min, wait for that reaction is finished and filtered to sample with miillpore filter, 3 times washed respectively using distilled water and ethyl alcohol, 70
Freeze-day with constant temperature obtains exposing Fluorin doped titanium dioxide-graphene complex of high-energy surface at DEG C.By 0.006 mol cadmium nitrates and incite somebody to action
0.015 mol vulcanized sodium is distributed in ethylene glycol respectively under ultrasound environments.Under the conditions of ultrasonic agitation by sodium sulfide solution with
The rate of addition of 25mL/30 min is added drop-wise in nitric acid cadmium solution, and by step（1）The Fluorin doped two of middle gained exposure high-energy surface
In titanium oxide-graphene dispersion to above-mentioned solution, 20 min of ultrasonic agitation are allowed to uniformly mix after the completion of all reagent mixing, surpass
Acoustic frequency is 40 kHz.Then acquired solution is moved into and is focused in single mold microwave synthesizer, sets microwave power to 350 W,
Reaction temperature is 130 DEG C, and the reaction time is 45 min, waits for that reaction is finished and is filtered to sample with miillpore filter, using distillation
Water and ethyl alcohol wash Fluorin doped titanium dioxide-wurtzite-type vulcanization that freeze-day with constant temperature at 3 times, 70 DEG C obtains exposing high-energy surface respectively
Cadmium-graphene composite photocatalyst.
Embodiment 5
0.003 mol titanium tetrachlorides and 25 mg graphene oxides is taken to be distributed in ethyl alcohol under ultrasound environments.Take 0.006 mol
Calcirm-fluoride be dissolved in distilled water.Then with the rate of addition of 5 mL/30 min by calcium fluoride melt solution be added drop-wise to titanium tetrachloride and
In the mixed liquor of graphene oxide, 25 min are stirred by ultrasonic after being added dropwise to complete and are allowed to uniformly mix, supersonic frequency is 40 kHz.With
Mixed liquor is moved into afterwards and is focused in single mold microwave synthesizer, sets microwave power to 350 W, reaction temperature is 140 DEG C, instead
It is 50 min between seasonable, waits for that reaction is finished and sample is filtered with miillpore filter, 3 are washed respectively using distilled water and ethyl alcohol
Secondary, freeze-day with constant temperature obtains exposing Fluorin doped titanium dioxide-graphene complex of high-energy surface at 80 DEG C.By 0.003 mol acetic acid
Cadmium and 0.015 mol vulcanized sodium is distributed under ultrasound environments respectively in 25 mL ethylene glycol.By sulphur under the conditions of ultrasonic agitation
Change sodium solution to be added drop-wise in cadmium acetate solution with the rate of addition of 5 mL/30 min, and by step（1）Middle gained exposes high-energy surface
Fluorin doped titanium dioxide-graphene dispersion to above-mentioned solution in, 25 min of ultrasonic agitation are allowed to after the completion of the mixing of all reagents
Uniformly mixing, supersonic frequency are 40 kHz.Then acquired solution is moved into and is focused in single mold microwave synthesizer, microwave power is set
350 W are set to, reaction temperature is 140 DEG C, and the reaction time is 50 min, waits for that reaction is finished and is taken out to sample with miillpore filter
Filter washs the Fluorin doped titanium dioxide-that freeze-day with constant temperature at 3 times, 80 DEG C obtains exposing high-energy surface respectively using distilled water and ethyl alcohol
Wurtzite-type cadmium sulfide-graphene composite photocatalyst.
Embodiment 6
0.006 mol Titanium Nitrates and 10 mg graphene oxides is taken to be distributed in ethyl alcohol under ultrasound environments.Take 0.003 mol's
Calcirm-fluoride is dissolved in distilled water.Then calcium fluoride melt solution is added drop-wise to by Titanium Nitrate and oxidation with the rate of addition of 5 mL/30 min
In the mixed liquor of graphene, 30 min are stirred by ultrasonic after being added dropwise to complete and are allowed to uniformly mix, supersonic frequency is 50 kHz.Then will
Mixed liquor, which moves into, to be focused in single mold microwave synthesizer, sets microwave power to 450 W, and reaction temperature is 150 DEG C, when reaction
Between be 60 min, wait for that reaction is finished and filtered to sample with miillpore filter, 3 times washed respectively using distilled water and ethyl alcohol, 90
Freeze-day with constant temperature obtains exposing Fluorin doped titanium dioxide-graphene complex of high-energy surface at DEG C.By 0.006 mol cadmium acetates and incite somebody to action
0.015 mol L-cysteines are distributed under ultrasound environments respectively in 25 mL ethylene glycol.By L- under the conditions of ultrasonic agitation
Cysteine solution is added drop-wise to the rate of addition of 5 mL/30 min in cadmium acetate solution, and by step（1）Middle gained exposure is high
In the Fluorin doped titanium dioxide-graphene dispersion to above-mentioned solution in energy face, 30 min are stirred by ultrasonic after the completion of all reagents mixing
It is allowed to uniformly mix, supersonic frequency is 50 kHz.Then acquired solution is moved into and is focused in single mold microwave synthesizer, by microwave work(
Rate is set as 450 W, and reaction temperature is 150 DEG C, and the reaction time is 60 min, wait for reaction finish with miillpore filter to sample into
Row filters, and the Fluorin doped dioxy that freeze-day with constant temperature at 3 times, 90 DEG C obtains exposing high-energy surface is washed respectively using distilled water and ethyl alcohol
Change titanium-wurtzite-type cadmium sulfide-graphene composite photocatalyst.
Embodiment 7
Synthesized Fluorin doped titanium dioxide-graphene intermediate, Fluorin doped titanium dioxide-cadmium sulfide-in Example 3 and 5
Graphene composite photocatalyst, graphene oxide, blank control group are to methylene blue（MB）Solution carries out Visible Light Induced Photocatalytic.Using
PLS-LAX500ADJ types（Beijing Bo Feilai Instrument Ltd.）Xenon long-arc lamp is as light source.It is put in special purpose reactor first
The MB solution for entering a concentration of 10 mg/L of 200 mL is added 100 mg catalyst samples, will first be mixed before light-catalyzed reaction thereto
It closes uniform catalyst and MB solution is placed in 30 min in dark, so that catalyst is reached absorption/desorption equilibrium with MB, then in room
Temperature is lower to carry out photocatalytic degradation reaction, and the reaction time amounts to 90 min.When light-catalyzed reaction, a sample is taken every 10 min, is used
After centrifuge, supernatant liquor is taken to survey its absorbance value at the nm of λ=665 in ultraviolet-visible spectrophotometer, according to
The degradation rate of MB is calculated according to following formula：
In formula,ηFor degradation rate；A0To reach the absorbance of solution after adsorption/desorption balances after dark reaction；AtFor different samplings when
Between solution absorbance.The result shows that 120 DEG C of reaction temperature, 40 min of reaction time, graphene content are catalyzed when being 15 %
The photocatalysis effect of agent is best, sees Fig. 1.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution, improvement and etc. done should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of composite photo-catalyst, which is characterized in that include the following steps：
（1）0.003-0.006 mol titanium sources and 10-25mg graphene oxides is taken to be distributed in absolute ethyl alcohol under ultrasound condition,
It takes the Fluorine source of 0.003-0.006 mol to be dissolved in distilled water, Fluorine source solution is then added drop-wise to the mixed of titanium source and graphene oxide
It closes in liquid, ultrasonic agitation is allowed to uniformly mix after being added dropwise to complete；Then by mixed liquor dislocation in focusing in single mold microwave synthesizer
It is reacted, waits filtering sample after the completion of reacting, wash, be dried in vacuo the Fluorin doped titanium dioxide for obtaining exposing high-energy surface
Titanium-graphene complex；
（2）It is distributed to second two respectively under ultrasound condition by the mol cadmiums sources 0.003-0.006 and by 0.005-0.015 mol sulphur sources
In alcohol, sulphur source solution is added drop-wise in the solution of cadmium source under the conditions of ultrasonic agitation, then by step（1）Fluorin doped titanium dioxide-
Graphene complex is distributed in above-mentioned solution, and ultrasonic agitation is allowed to uniformly mix after the completion of all reagent mixing；After mixing
Solution moves into focus to react in single mold microwave synthesizer, waits filtering sample after the completion of reacting, wash, being dried in vacuo and obtain
Fluorin doped titanium dioxide-cadmium sulfide-graphene composite photocatalyst of exposure high-energy surface.
2. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Step（1）Middle titanium source is four
One kind in titanium chloride, Titanium Nitrate, Titanium alkoxides.
3. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Step（1）Middle Fluorine source is fluorine
Change one kind in ammonium, calcirm-fluoride.
4. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Step（2）Middle cadmium source is sulphur
One kind in sour cadmium, cadmium nitrate, cadmium acetate.
5. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Step（2）Middle sulphur source is sulphur
Change one kind in sodium, sodium thiosulfate, L-cysteine.
6. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：The drop rate of solution is 5
mL/30 min。
7. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Ultrasonic agitation is to be in frequency
5 ~ 30 min of ultrasound under 30 ~ 50 kHz.
8. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Focus single mold microwave synthesizer
Middle reaction is 30 ~ 60 min of progress at 250 ~ 450 W of microwave power, 100 ~ 150 DEG C.
9. the preparation method of composite photo-catalyst according to claim 1, it is characterised in that：Filter using miillpore filter into
Row filters, and washing is washed 3 times respectively successively using ethyl alcohol and distilled water, and vacuum drying temperature is 60 ~ 90 DEG C.
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Application publication date: 20180907 |