CN106824246B - A kind of TiO2/g-C3N4The preparation method of composite visible light catalyst - Google Patents
A kind of TiO2/g-C3N4The preparation method of composite visible light catalyst Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010936 titanium Substances 0.000 claims abstract description 24
- 235000019441 ethanol Nutrition 0.000 claims abstract description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 48
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 9
- 229920000877 Melamine resin Polymers 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229910010342 TiF4 Inorganic materials 0.000 claims description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 25
- 230000001699 photocatalysis Effects 0.000 abstract description 18
- 238000003786 synthesis reaction Methods 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 18
- 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 12
- 239000013078 crystal Substances 0.000 description 12
- 229960000907 methylthioninium chloride Drugs 0.000 description 12
- 238000007146 photocatalysis Methods 0.000 description 12
- 229960004756 ethanol Drugs 0.000 description 11
- 239000002245 particle Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000000985 reflectance spectrum Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000010748 Photoabsorption Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010298 TiOSO4 Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011218 binary composite Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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—
-
- B01J35/39—
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- 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
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of TiO2/g‑C3N4Titanium source and nitrogen source are first uniformly dispersed by the preparation method of composite visible light catalyst in ethanol, and water is then added dropwise into ethyl alcohol and obtains mixed material；Mixed material is evaporated to obtain presoma under stirring；Then the presoma of preparation is transferred in Muffle furnace, calcines 0.5~12h at 300 DEG C~800 DEG C in Muffle furnace, obtains TiO2/g‑C3N4Composite visible light catalyst.The present invention is in preparation TiO2And g-C3N4While be made TiO2/g‑C3N4Composite visible light catalyst, by TiO2And g-C3N4The synthesis of both compounds and the preparation of composite catalyst, which are placed in a step, to be realized；Simple process, it is easy to accomplish industrialized production.Composite visible light catalyst photocatalytic activity center of the invention is more, and absorptivity and photocatalytic activity are higher, and the photocatalytic activity of organic matter is higher.
Description
The application is application No. is 201410621237.1, and the applying date is on November 6th, 2014, and invention and created name is
“TiO2/g-C3N4The divisional application of the application for a patent for invention of the preparation method of composite visible light catalyst ".
Technical field
The present invention relates to a kind of preparation methods of visible light catalyst, and in particular to a kind of TiO2/g-C3N4Composite visible light
The preparation method of catalyst.
Background technique
Semiconductor light-catalyst has been a concern in the past few decades.It is obtained because it is widely used in direct hydrolysis
Obtain the environmental protection of renewable energy hydrogen and organic polluting water.
In numerous semiconductors, TiO2Since its nontoxic, inexpensive, high stability and excellent photo-catalysis capability become
Most study and most promising semiconductor material.But due to big (such as Detitanium-ore-type TiO of its energy gap2 3.2
EV), can only be using the part ultraviolet light (UV) for accounting for sunlight 3%~4%, and quantum efficiency is low, to limit TiO2Answer
With.Therefore, the methods of doping, metal deposit and preparation of composite material are applied to TiO2Modification, with expectation improve its can
Light-exposed photocatalytic activity.
In recent years, a kind of new function material-graphitic carbon nitride (g-C3N4) due to nonmetal character, high electronics
The characteristics of mobility, low band gap (2.73eV) and be caused extensive concern.g-C3N4With superior reducing power, photoresponse
Wavelength is expanded to visible-range up to 450nm.But its oxidability ratio TiO2It is weak, in addition, in the photocatalytic process
Electron-hole pair separation rate needs further increase.
In order to overcome TiO2And g-C3N4Respective disadvantage combines the advantages of the two, and researcher synthesizes
TiO2/g-C3N4Composite material.Synthetic composite material TiO at present2/g-C3N4Method mainly grind, hydro-thermal or calcining.
Such as 103736512 A(application number 201410003651.6 of Chinese patent literature CN) disclose a kind of TiO2It is situated between
Hole monocrystalline microballoon and g-C3N4The preparation method of heterojunction photocatalyst, the method are the means processing titanium source and g-C with water-bath3N4
Mixture after obtain composite photo-catalyst.The g-C for first obtaining calcining when prepared by the patent document3N4Powder is placed in TiCl4It is brilliant
In kind solution, centrifugal drying obtains the g-C of pre- plantation crystal seed after water bath with thermostatic control 2 hours3N4；By the g-C of pre- plantation crystal seed3N4With
TiOSO4Solution moves into autoclave jointly, is sealed in 100 DEG C of heat preservation 48h of air dry oven, filters out powder after reaction, washing
TiO is obtained after drying2Mesoporous single crystals microballoon and g-C3N4Heterojunction photocatalyst.The preparation method is with g-C3N4For nitrogen source,
TiCl4For titanium source, g-C is first prepared3N4, and preparation process will use high-tension apparatus, and the reaction time is long.
103230808 A (application number 201310198704.X) of Chinese patent literature CN discloses a kind of Pt- C3N4-
TiO2Melamine is first calcined in Muffle furnace and obtains g-C by the preparation method of ternary visible photochemical catalyst3N4Powder；It weighs
TiO2Four parts of solid powder are placed in four beakers, dehydrated alcohol are respectively added, then add g-C respectively3N4Powder, ultrasonic mixing is extremely
Powder is completely dispersed, and 80 DEG C of dry 5h are placed in Muffle furnace after grinding to be evaporated powder and calcine 2h at 400 DEG C, Temperature fall is cold
But binary composite photo-catalyst TiO is obtained to taking-up after room temperature2/g-C3N4.The preparation method is with g-C3N4For nitrogen source, TiO2For titanium
Source, it is necessary to first prepare g-C respectively3N4And TiO2It just can be carried out the preparation of next step, and g-C3N4And TiO2It needs by cumbersome
Preparation process could obtain, this can prevent TiO2/g-C3N4Large-scale production and application.
102962088 A(application number 201210439866.3 of Chinese patent literature CN) disclose a kind of TiO2Microballoon with
g-C3N4Composite visible light catalyst and preparation method and application, the titanium sheet cleaned up is placed in melamine and ammonium fluoride
Hydro-thermal reaction is carried out in mixed aqueous solution, after reaction solution is cooling, collects the sediment in reaction solution, washing and drying is simultaneously forged
It burns, obtains TiO2Microballoon and g-C3N4Composite visible light catalyst.Ammonium fluoride used in the preparation process of the preparation method is
Extremely toxic substance, to operator there are security risk and to high operation requirements.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of simple processes, it is easy to accomplish the TiO of industrialized production2/
g-C3N4The preparation method of composite visible light catalyst.
The technical solution for realizing the object of the invention is a kind of TiO2/g-C3N4The preparation method of composite visible light catalyst, packet
Include following steps:
1. titanium source and nitrogen source are uniformly dispersed by the preparation of presoma in ethanol, then the Xiang Hanyou again under stirring
Water is added dropwise in the ethyl alcohol of titanium source and nitrogen source and obtains mixed material；Mixed material is evaporated to obtain presoma under stirring；Institute
Stating titanium source is Ti (OBu)4Or TiF4, nitrogen source is melamine or urea.
2. 1. presoma that step is prepared is transferred in Muffle furnace, calcined at 300 DEG C~800 DEG C in Muffle furnace
0.5~12h obtains TiO2/g-C3N4Composite visible light catalyst.
1. the mass ratio of middle titanium source and nitrogen source is 0.0001~1000 to above-mentioned steps.
Further, step 1. in after titanium source and nitrogen source be uniformly dispersed in ethanol, the concentration of titanium source is 0.0001g/mL
~1.5g/mL, the concentration of nitrogen source are 0.0001g/mL~1g/mL.
Further, step 1. in water dripping quantity be ethyl alcohol volume 10%~500%.
Above-mentioned steps 1. in ethyl alcohol temperature be 0 DEG C~78 DEG C.
Preferably, step 1. in ethyl alcohol temperature be 15 DEG C~35 DEG C.
Above-mentioned steps 1. in by mixed material in 40 DEG C~100 DEG C of water-bath, be evaporated to obtain forerunner under stirring
Body.
Preferably, step 1. in mixed material is evaporated in 70 DEG C~85 DEG C of water-bath, under stirring
To presoma.
The present invention has the effect of positive: (1) present invention is in preparation TiO2/g-C3N4When composite visible light catalyst, do not have
First prepare TiO2Or g-C3N4, then by TiO2With melamine or g-C3N4Composite catalyst or g-C is made by technique3N4
With titanium source or TiO2Composite catalyst is made by technique；But in preparation TiO2And g-C3N4While be made TiO2/g-C3N4
Composite visible light catalyst, by TiO2And g-C3N4The synthesis of both compounds and the preparation of composite catalyst are placed on a step
Middle realization；Simple process, it is easy to accomplish industrialized production.
(2) TiO prepared by the present invention2/g-C3N4Composite visible light catalyst has apparent graphite laminated structure, product
TEM map show nano-TiO2Uniform particle is distributed in graphite-like g-C3N4In；Therefore TiO prepared by the present invention2/g-C3N4It is multiple
Conjunction visible light catalyst photocatalytic activity center is more, and absorptivity and photocatalytic activity are higher, the photocatalytic degradation of organic matter
Rate is higher.
For handling organic matter methylene blue, TiO prepared by the present invention2/g-C3N4The light of composite visible light catalyst is urged
Change degradation rate and reach 94.46%, than using TiO made from equal conditions2And g-C3N4Photocatalytic activity be higher by respectively
12.65% and 49.25%.
(3) TiO prepared by the present invention2/g-C3N4Composite visible light catalyst can be used for handling petroleum, chemical industry, pharmacy, print
The high concentration organic sewage of the industries such as dye.
Detailed description of the invention
Fig. 1 is TiO prepared by embodiment 12/g-C3N4The XRD diffracting spectrum of composite visible light catalyst；
Fig. 2 is TiO prepared by embodiment 12/g-C3N4The TEM map of composite visible light catalyst；
Fig. 3 is TiO prepared by embodiment 12/g-C3N4The ultraviolet-visible diffuse reflectance spectrum of composite visible light catalyst；
Fig. 4 is g-C prepared by comparative example 13N4XRD diffracting spectrum；
Fig. 5 is g-C prepared by comparative example 13N4TEM map；
Fig. 6 is g-C prepared by comparative example 13N4Ultraviolet-visible diffuse reflectance spectrum；
Fig. 7 is TiO prepared by comparative example 22XRD diffracting spectrum；
Fig. 8 is TiO prepared by comparative example 22TEM map；
Fig. 9 is TiO prepared by comparative example 22Ultraviolet-visible diffuse reflectance spectrum.
Specific embodiment
(embodiment 1)
The present embodiment prepares TiO2/g-C3N4The method of composite visible light catalyst the following steps are included:
1. the preparation of presoma.By 20mL Ti (OBu)4Disperse in 500mL, 20 DEG C of ethyl alcohol with 20g melamine
It is even, then under stirring again to contain Ti (OBu)4Mixed material is obtained with 50mL water is added dropwise in the ethyl alcohol of melamine；
By mixed material in 70 DEG C~85 DEG C (in the present embodiment be 80 DEG C) of water-bath, be evaporated to obtain presoma under stirring.
2. 1. presoma that step is prepared is transferred in Muffle furnace, 2h is calcined at 520 DEG C in Muffle furnace, is obtained
TiO2/g-C3N4Composite visible light catalyst.
Product is made to the present embodiment to characterize: characterizing transmission electron microscope (TEM) used is Japan Electronics strain
The transmission electron microscope of 2010 model of JEOL of formula commercial firm；X-ray diffractometer is the D/MAX- of Rigaku company, Japan
The X-ray diffractometer of 2500PC model；Ultraviolet-visible spectrometer is the spectrometer of the UV-2700 model of Shimadzu Corporation.Following reality
Instrument used in example and comparative example is applied to be same as above.
See Fig. 1, in the XRD diffracting spectrum of product, 27.29 ° belong to g-C3N4(002) face；25.34 °, 37.76 °,
48.14 °, 55.12 ° and 62.76 °, correspond respectively to anatase TiO2(101), (004), (200), (211) and (204) is brilliant
Face；36.12 °, 41.22 °, 56.66 ° are belonging respectively to rutile TiO2(101), (111) and (220) crystal face；Therefore product
It is g-C3N4, anatase titanium dioxide TiO2And rutile TiO2The mixture of crystal shows that TiO has successfully been made in the present embodiment2/g-C3N4
Composite visible light catalyst.
See that Fig. 2, Fig. 2 are the TEM map of the product obtained 2. step is calcined after, stain is nano-TiO in figure2Particle, by
Fig. 1 can be clearly seen that nano-TiO in the product of the present embodiment2Uniform particle is distributed in graphite sheet g-C3N4In.
See Fig. 3, the ultraviolet-visible diffuse reflectance spectrum of product is shown, the TiO of the present embodiment synthesis2/g-C3N4It is compound visible
From 390 to 550 nm of visible absorption region of photochemical catalyst, it is seen that the range of light absorption is wide, intensity is high, uses Shi Benshi
A large amount of visible light can be absorbed in the composite photo-catalyst for applying example preparation, is suitable for Photocatalytic Activity for Degradation organic pollutant.
In order to examine TiO manufactured in the present embodiment2/g-C3N4Photocatalysis performance, photocatalytic degradation methylene is carried out to it
Blue test: light-catalyzed reaction carries out in cylindrical glass reactor, and using 300 W xenon lamps as light source, light source is away from liquid level
20cm；Add magnetic agitation below reaction vessel, be sufficiently mixed solution, keeps concentration and temperature uniformity, catalyst
TiO2/g-C3N4Dosage is 1g/L, methylene blue initial concentration is 20mg/L, and through detecting after 1h, methylene blue concentration is
The photocatalytic activity of 1.108mg/L, methylene blue reach 94.46%.
(embodiment 2)
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, difference
Be in: step 1. in Ti (OBu)4Additional amount be 5mL, the temperature of ethyl alcohol is 25 DEG C, and bath temperature is 85 DEG C.
It is detected through X-ray diffractometer, the product of the present embodiment is g-C3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal
Mixture, show that TiO has successfully been made in the present embodiment2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM map of composite visible light catalyst shows nano-TiO2Uniform particle
It is distributed in graphite sheet g-C3N4In.
It is detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible
From 390 to 530 nm of photo-absorption region.
TiO manufactured in the present embodiment is detected according to the method for embodiment 12/g-C3N4Photocatalysis performance, methylene blue
Photocatalytic activity reaches 96.32%.
(embodiment 3)
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, difference
Be in: step 1. in Ti (OBu)4Additional amount be 100mL, the dripping quantity of water is 1000mL, and bath temperature is 85 DEG C.
It is detected through X-ray diffractometer, the product of the present embodiment is g-C3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal
Mixture, show that TiO has successfully been made in the present embodiment2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM map of composite visible light catalyst shows nano-TiO2Uniform particle
It is distributed in graphite sheet g-C3N4In.
It is detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible
From 390 to 530 nm of photo-absorption region.
TiO manufactured in the present embodiment is detected according to the method for embodiment 12/g-C3N4Photocatalysis performance, methylene blue
Photocatalytic activity reaches 91.45%.
(embodiment 4)
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, difference
Be in: step 2. in presoma calcined into 2h at 600 DEG C in Muffle furnace, obtain TiO2/g-C3N4Composite visible light catalysis
Agent.
It is detected through X-ray diffractometer, the product of the present embodiment is g-C3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal
Mixture, show that TiO has successfully been made in the present embodiment2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM map of composite visible light catalyst shows nano-TiO2Uniform particle
It is distributed in graphite sheet g-C3N4In.
It is detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible
From 390 to 500 nm of photo-absorption region.
TiO manufactured in the present embodiment is detected according to the method for embodiment 12/g-C3N4Photocatalysis performance, methylene blue
Photocatalytic activity reaches 89.35%.
(embodiment 5)
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, difference
Be in: step 2. in presoma calcined into 1h at 800 DEG C in Muffle furnace, obtain TiO2/g-C3N4Composite visible light catalysis
Agent.
It is detected through X-ray diffractometer, the product of the present embodiment is g-C3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal
Mixture, show that TiO has successfully been made in the present embodiment2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM map of composite visible light catalyst shows nano-TiO2Uniform particle
It is distributed in graphite sheet g-C3N4In.
It is detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible
From 390 to 480 nm of photo-absorption region.
TiO manufactured in the present embodiment is detected according to the method for embodiment 12/g-C3N4Photocatalysis performance, methylene blue
Photocatalytic activity reaches 75.76%.
(embodiment 6)
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, difference
Be in: step 1. in by the TiF of 5g4It is uniformly dispersed in 500mL, 35 DEG C of ethyl alcohol with 20g melamine.
TiO manufactured in the present embodiment is detected according to the method for embodiment 12/g-C3N4Photocatalysis performance, methylene blue
Photocatalytic activity reaches 85.56%.
(embodiment 7)
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, difference
Be in:
Step 1. in by 20mL Ti (OBu)4It is uniformly dispersed in 500mL, 30 DEG C of ethyl alcohol with 10g urea.
TiO manufactured in the present embodiment is detected according to the method for embodiment 12/g-C3N4Photocatalysis performance, methylene blue
Photocatalytic activity reaches 86.78%.
(comparative example 1, g-C3N4)
The preparation of this comparative example is g-C3N4, remaining is same as Example 1 for preparation method, the difference is that this comparative example
The step of 1. presoma prepare when Ti (OBu) is not added4；Step obtains g-C after 2. calcining3N4Powder.
See Fig. 4, the XRD spectrum of product is shown, this comparative example synthesis product main diffraction peak: 13.32 ° and
27.29 ° with standard spectrogram (JCPDS 87-1526) unanimously, be belonging respectively to g-C3N4(100) and (002) crystal face, show that this is right
G-C has successfully been made in ratio3N4。
See that Fig. 5, the TEM map of product are shown, g-C obtained3N4Laminated structure with graphite-like.
See Fig. 6, the ultraviolet-visible diffuse reflectance spectrum of product is shown, g-C made from this comparative example3N4Maximum absorption band exist
At 394 nm, TiO is lower than to UV absorption intensity2 。
The g-C of this comparative example preparation is detected according to the method for embodiment 13N4Photocatalysis performance, the photocatalysis of methylene blue
Degradation rate reaches 45.21%.
(comparative example 2, TiO2)
The preparation of this comparative example is TiO2, remaining is same as Example 1 for preparation method, the difference is that this comparative example
Melamine is not added when 1. presoma prepares in step；Step obtains TiO after 2. calcining2。
See Fig. 7, the XRD spectrum of product is shown, the TiO of this comparative example synthesis2It is Detitanium-ore-type, the data with standard
(JCPDS file No.21-1272) is consistent, and does not find the crystal form of other rutile or brookite type.25.34 °,
37.76 °, 48.14 °, 55.12 ° and 62.76 °, correspond respectively to anatase TiO2(101), (004), (200), (211) and
(204) crystal face.
See that Fig. 8, the TEM map of product are shown, the TiO of ball shape2Certain polymerization is presented, the size of particle is 20~40
nm。
See Fig. 9, the ultraviolet-visible diffuse reflectance spectrum of product is shown, the TiO of the present embodiment synthesis2Mainly in UV light area
There is absorption in domain.
The TiO of this comparative example preparation is detected according to the method for embodiment 12Photocatalysis performance, the photocatalysis of methylene blue
Degradation rate reaches 81.81%.
Claims (4)
1. a kind of TiO2/g-C3N4The preparation method of composite visible light catalyst, it is characterised in that the following steps are included:
1. titanium source and nitrogen source are uniformly dispersed by the preparation of presoma in ethanol, the concentration of titanium source is 0.0001g/mL~1.5g/
ML, the concentration of nitrogen source are 0.0001g/mL~1g/mL；Then it is dripped again into the ethyl alcohol containing titanium source and nitrogen source under stirring
Water is added to obtain mixed material；By mixed material in 70 DEG C~85 DEG C of water-bath, be evaporated to obtain presoma under stirring；Institute
Stating titanium source is Ti (OBu)4Or TiF4, nitrogen source is melamine or urea；
2. 1. presoma that step is prepared is transferred in Muffle furnace, in Muffle furnace at 300 DEG C~800 DEG C calcining 0.5~
12h obtains TiO2/g-C3N4Composite visible light catalyst.
2. TiO according to claim 12/g-C3N4The preparation method of composite visible light catalyst, it is characterised in that: step
1. the dripping quantity of middle water is the 10%~500% of ethyl alcohol volume.
3. TiO according to claim 12/g-C3N4The preparation method of composite visible light catalyst, it is characterised in that: step
1. the temperature of middle ethyl alcohol is 0 DEG C~78 DEG C.
4. TiO according to claim 32/g-C3N4The preparation method of composite visible light catalyst, it is characterised in that: step
1. the temperature of middle ethyl alcohol is 15 DEG C~35 DEG C.
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