CN106914263A - A kind of preparation method of composite visible light catalyst - Google Patents

A kind of preparation method of composite visible light catalyst Download PDF

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CN106914263A
CN106914263A CN201710099279.7A CN201710099279A CN106914263A CN 106914263 A CN106914263 A CN 106914263A CN 201710099279 A CN201710099279 A CN 201710099279A CN 106914263 A CN106914263 A CN 106914263A
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tio
visible light
light catalyst
composite visible
preparation
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CN106914263B (en
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张春勇
郑纯智
文颖频
张国华
舒莉
程洁红
马迪
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Jiangsu University of Technology
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Jiangsu University of Technology
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    • 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 preparation method of composite visible light catalyst, first titanium source and nitrogen source are uniformly dispersed in ethanol, then obtain mixed material to dropwise addition water in ethanol；Mixed material is evaporated under stirring and obtains presoma；Then the presoma of preparation is transferred in Muffle furnace, in 0.5~12h is calcined at 300 DEG C~800 DEG C in Muffle furnace, obtains TiO2/g‑C3N4Composite visible light catalyst.The present invention is preparing TiO2With g C3N4While be obtained TiO2/g‑C3N4Composite visible light catalyst, by TiO2With g C3N4The synthesis of both compounds and the preparation of composite catalyst are realized in being placed on a step；Process is simple, 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

A kind of preparation method of composite visible light catalyst
The application is Application No. 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 method of visible light catalyst, and in particular to a kind of TiO2/g-C3N4Composite visible light The preparation method of catalyst.
Background technology
Semiconductor light-catalyst receives much concern always in the past few decades.Because it is widely used in direct hydrolysis obtaining Obtain the environmental protection of regenerative resource hydrogen and organic polluting water.
In numerous semiconductors, TiO2Because its nontoxic, inexpensive, high stability and excellent photo-catalysis capability turn into The semi-conducting material of most study and most application prospect.But, because its energy gap is big（Such as Detitanium-ore-type TiO2 3.2 eV）, the ultraviolet for accounting for sunshine 3%~4% can only be utilized（UV）Part, and quantum efficiency is low, so as to limit TiO2Should With.Therefore, the method such as preparation of doping, metal deposit and composite is applied to TiO2It is modified, so that expect to improve it can See light photocatalytic activity.
In recent years, a kind of new function material-graphitic carbon nitride (g-C3N4) due to nonmetal character, electronics high Mobility, low band gap（2.73eV）The characteristics of and be caused extensive concern.g-C3N4With superior reducing power, its photoresponse Wavelength is expanded to visible-range up to 450nm.But its oxidability compares TiO2It is weak, additionally, in photocatalytic process Electron-hole pair separation rate need further improve.
In order to overcome TiO2And g-C3N4Respective shortcoming, both advantages are combined, and researcher synthesizes TiO2/g-C3N4Composite.Current synthetic composite material TiO2/g-C3N4Method be mainly grinding, hydro-thermal or calcining.
Such as A of Chinese patent literature CN 103736512（Application number 201410003651.6）Disclose a kind of TiO2It is situated between Hole monocrystalline microballoon and g-C3N4The preparation method of heterojunction photocatalyst, the method is to process titanium source and g-C with the means of water-bath3N4 Mixture after obtain composite photo-catalyst.The patent document will first calcine the g-C for obtaining when preparing3N4Powder is placed in TiCl4It is brilliant In kind of 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, closed to be put into 100 DEG C of insulation 48h of air dry oven, leaches powder after reaction, washs TiO is obtained after drying2Mesoporous single crystals microballoon and g-C3N4Heterojunction photocatalyst.The preparation method is with g-C3N4It is nitrogen source, TiCl4It is titanium source, first prepares g-C3N4, and preparation process will use high-tension apparatus, and the reaction time is long.
The A of Chinese patent literature CN 103230808（Application number 201310198704.X）Disclose a kind of Pt- C3N4- TiO2The preparation method of ternary visible photochemical catalyst, melamine is first calcined obtain g-C in Muffle furnace3N4Powder；Weigh TiO2Four parts of solid powder is placed in four beakers, respectively adds absolute ethyl alcohol, then adds g-C respectively3N4Powder, ultrasonic mixing is extremely Powder is completely dispersed, and 80 DEG C dry 5h to be evaporated powder, is placed on after grinding in Muffle furnace and calcines 2h at 400 DEG C, and 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-C3N4It is nitrogen source, TiO2It is titanium Source, it is necessary to first prepare g-C respectively3N4And TiO2Can just carry out the preparation of next step, and g-C3N4And TiO2Need by cumbersome Preparation process could obtain, this can prevent TiO2/g-C3N4Large-scale production and application.
The A of Chinese patent literature CN 102962088（Application number 201210439866.3）Disclose a kind of TiO2Microballoon with g-C3N4Composite visible light catalyst and preparation method and application, the titanium sheet that will be cleaned up is placed in melamine and ammonium fluoride Hydro-thermal reaction is carried out in mixed aqueous solution, after the cooling of question response solution, the sediment in reaction solution is collected, washing and drying is simultaneously forged Burn, obtain TiO2Microballoon and g-C3N4Composite visible light catalyst.Ammonium fluoride used is in the preparation process of the preparation method There is potential safety hazard and operation are required high by extremely toxic substance in operating personnel.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of process is simple, it is easy to accomplish the TiO of industrialized production2/ g-C3N4The preparation method of composite visible light catalyst.
The technical scheme for realizing the object of the invention is a kind of TiO2/g-C3N4The preparation method of composite visible light catalyst, bag Include following steps：
1. the preparation of presoma, titanium source and nitrogen source are uniformly dispersed in ethanol, then again to containing titanium source under stirring Mixed material is obtained with water is added dropwise in the ethanol of nitrogen source；Mixed material is evaporated under stirring and obtains presoma；The titanium Source is Ti (OBu)4Or TiF4, nitrogen source is melamine or urea.
2. the presoma that 1. step prepares is transferred in Muffle furnace, in calcining at 300 DEG C~800 DEG C in Muffle furnace 0.5~12h, obtains TiO2/g-C3N4Composite visible light catalyst.
Above-mentioned steps 1. middle titanium source and nitrogen source mass ratio be 0.0001~1000.
Further, after 1. middle titanium source and nitrogen source are uniformly dispersed in ethanol, the concentration of titanium source is 0.0001g/mL to step ~1.5g/mL, the concentration of nitrogen source is 0.0001g/mL~1g/mL.
Further, step 1. reclaimed water dripping quantity for ethanol volume 10%~500%.
Above-mentioned steps 1. middle ethanol temperature be 0 DEG C~78 DEG C.
Used as preferred, the temperature of step 1. middle ethanol is 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 under stirring and obtain forerunner Body.
As preferred, 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 positive effect：（1）The present invention is preparing TiO2/g-C3N4During composite visible light catalyst, do not have First prepare TiO2Or g-C3N4, then by TiO2With melamine or g-C3N4Composite catalyst, or g-C are obtained by technique3N4 With titanium source or TiO2Composite catalyst is obtained by technique；But preparing TiO2And g-C3N4While be obtained 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；Process is simple, it is easy to accomplish industrialized production.
（2）TiO prepared by the present invention2/g-C3N4Composite visible light catalyst has obvious graphite laminated structure, product TEM collection of illustrative plates display nano-TiO2Uniform particle is distributed in graphite-like g-C3N4In；Therefore the TiO that 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.
As a example by processing 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 obtained in 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 to process oil, chemical industry, pharmacy, print The high concentration organic sewage of the industries such as dye.
Brief description of the drawings
Fig. 1 is TiO prepared by embodiment 12/g-C3N4The XRD diffracting spectrums of composite visible light catalyst；
Fig. 2 is TiO prepared by embodiment 12/g-C3N4The TEM collection of illustrative plates of composite visible light catalyst；
Fig. 3 is TiO prepared by embodiment 12/g-C3N4The UV-Vis DRS spectrum of composite visible light catalyst；
Fig. 4 is g-C prepared by comparative example 13N4XRD diffracting spectrums；
Fig. 5 is g-C prepared by comparative example 13N4TEM collection of illustrative plates；
Fig. 6 is g-C prepared by comparative example 13N4UV-Vis DRS spectrum；
Fig. 7 is TiO prepared by comparative example 22XRD diffracting spectrums；
Fig. 8 is TiO prepared by comparative example 22TEM collection of illustrative plates；
Fig. 9 is TiO prepared by comparative example 22UV-Vis DRS spectrum.
Specific embodiment
（Embodiment 1）
The present embodiment prepares TiO2/g-C3N4The method of composite visible light catalyst is comprised the following steps：
1. the preparation of presoma.By 20mL Ti (OBu)4It is uniformly dispersed in 500mL, 20 DEG C of ethanol with 20g melamines, Then again to containing Ti (OBu) under stirring4Mixed material is obtained with 50mL water is added dropwise in the ethanol of melamine；Will be mixed Compound material is at 70 DEG C~85 DEG C（It is 80 DEG C in the present embodiment）Water-bath in, be evaporated under stirring and obtain presoma.
2. the presoma that 1. step prepares is transferred in Muffle furnace, in 2h is calcined at 520 DEG C in Muffle furnace, is obtained TiO2/g-C3N4Composite visible light catalyst.
Product is obtained to the present embodiment to characterize：Characterize transmission electron microscope used（TEM）It is JEOL's strain The transmission electron microscope of the models of JEOL 2010 of formula commercial firm；X-ray diffractometer is the D/MAX- of Japanese Rigaku companies The X-ray diffractometer of 2500PC models；Ultraviolet-visible spectrometer is the spectrometer of the UV-2700 models of Shimadzu Corporation.Following reality Apply instrument used in example and comparative example ibid.
See Fig. 1, in the XRD diffracting spectrums of product, 27.29 ° belong to g-C3N4's（002）Face；25.34 °, 37.76 °, 48.14 °, 55.12 ° and 62.76 °, correspond respectively to anatase TiO2's（101）,（004）、（200）、（211) and（204） Crystal face；36.12 °, 41.22 °, 56.66 ° are belonging respectively to rutile TiO2's（101）、（111）With（220）Crystal face；Therefore produce Thing is g-C3N4, anatase titanium dioxide TiO2And rutile TiO2The mixture of crystal, shows that the present embodiment has successfully been obtained TiO2/g- C3N4Composite visible light catalyst.
See the TEM collection of illustrative plates that Fig. 2, Fig. 2 are the product obtained after 2. step calcines, 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 UV-Vis DRS spectrum of product shows, the TiO of the present embodiment synthesis2/g-C3N4It is compound visible The visible absorption region of photochemical catalyst is from 390 to 550 nm, it is seen that the scope of light absorbs is wide, intensity is high, this reality when using The composite photo-catalyst for applying example preparation can absorb substantial amounts of visible ray, it is adaptable to Photocatalytic Activity for Degradation organic pollution.
In order to check TiO manufactured in the present embodiment2/g-C3N4Photocatalysis performance, photocatalytic degradation methylene is carried out to it Blue experiment：Light-catalyzed reaction is carried 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, keep concentration and temperature uniformity, catalyst TiO2/g-C3N4Consumption is 1g/L, methylene blue initial concentration is 20mg/L, and through detection after 1h, methylene blue concentration is 1.108mg/L, the photocatalytic activity of methylene blue reaches 94.46%.
（Embodiment 2）
The present embodiment prepares TiO2/g-C3N4Remaining is same as Example 1 for the method for composite visible light catalyst, and difference exists In：Step 1. middle Ti (OBu)4Addition be 5mL, the temperature of ethanol is 25 DEG C, and bath temperature is 85 DEG C.
Detect that the product of the present embodiment is g-C through X-ray diffractometer3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal Mixture, show that the present embodiment has successfully been obtained TiO2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM collection of illustrative plates display nano-TiO of composite visible light catalyst2Uniform particle It is distributed in graphite sheet g-C3N4In.
Detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible Photo-absorption region is from 390 to 530 nm.
Method according to embodiment 1 detects TiO manufactured in the present embodiment2/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, and difference exists In：Step 1. middle Ti (OBu)4Addition be 100mL, the dripping quantity of water is 1000mL, and bath temperature is 85 DEG C.
Detect that the product of the present embodiment is g-C through X-ray diffractometer3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal Mixture, show that the present embodiment has successfully been obtained TiO2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM collection of illustrative plates display nano-TiO of composite visible light catalyst2Uniform particle It is distributed in graphite sheet g-C3N4In.
Detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible Photo-absorption region is from 390 to 530 nm.
Method according to embodiment 1 detects TiO manufactured in the present embodiment2/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, and difference exists In：Step 2. in by presoma in Muffle furnace in 2h is calcined at 600 DEG C, obtain TiO2/g-C3N4Composite visible light catalyst.
Detect that the product of the present embodiment is g-C through X-ray diffractometer3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal Mixture, show that the present embodiment has successfully been obtained TiO2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM collection of illustrative plates display nano-TiO of composite visible light catalyst2Uniform particle It is distributed in graphite sheet g-C3N4In.
Detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible Photo-absorption region is from 390 to 500 nm.
Method according to embodiment 1 detects TiO manufactured in the present embodiment2/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, and difference exists In：Step 2. in by presoma in Muffle furnace in 1h is calcined at 800 DEG C, obtain TiO2/g-C3N4Composite visible light catalyst.
Detect that the product of the present embodiment is g-C through X-ray diffractometer3N4, anatase titanium dioxide TiO2And rutile TiO2Crystal Mixture, show that the present embodiment has successfully been obtained TiO2/g-C3N4Composite visible light catalyst.
TiO manufactured in the present embodiment2/g-C3N4The TEM collection of illustrative plates display nano-TiO of composite visible light catalyst2Uniform particle It is distributed in graphite sheet g-C3N4In.
Detected through ultraviolet-visible spectrometer, the TiO of the present embodiment synthesis2/g-C3N4Composite visible light catalyst it is visible Photo-absorption region is from 390 to 480 nm.
Method according to embodiment 1 detects TiO manufactured in the present embodiment2/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, and difference exists In：Step 1. in by the TiF of 5g4It is uniformly dispersed in 500mL, 35 DEG C of ethanol with 20g melamines.
Method according to embodiment 1 detects TiO manufactured in the present embodiment2/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, and difference exists In：
Step 1. in by 20mL Ti (OBu)4It is uniformly dispersed in 500mL, 30 DEG C of ethanol with 10g urea.
Method according to embodiment 1 detects TiO manufactured in the present embodiment2/g-C3N4Photocatalysis performance, methylene blue Photocatalytic activity reaches 86.78%.
（Comparative example 1, g-C3N4）
That prepared by this comparative example is g-C3N4, remaining is same as Example 1 for preparation method, and difference is the step of this comparative example Rapid 1. presoma does not add Ti (OBu) when preparing4；Step obtains g-C after 2. calcining3N4Powder.
See Fig. 4, the XRD spectrum of product shows, the main diffraction peak of the product of this comparative example synthesis：13.32 ° and 27.29 ° and standard spectrogram（JCPDS 87-1526）Unanimously, it is belonging respectively to g-C3N4's（100）With（002）Crystal face, shows that this is right Ratio has successfully been obtained g-C3N4。
See Fig. 5, the TEM collection of illustrative plates of product shows, obtained g-C3N4Laminated structure with graphite-like.
See Fig. 6, the UV-Vis DRS spectrum of product shows, g-C obtained in this comparative example3N4Maximum absorption band exist At 394 nm, it is less than TiO to UV absorption intensity2 。
Method according to embodiment 1 detects g-C prepared by this comparative example3N4Photocatalysis performance, the photocatalysis of methylene blue Degradation rate reaches 45.21%.
（Comparative example 2, TiO2）
That prepared by this comparative example is TiO2, remaining is same as Example 1 for preparation method, the step of difference is this comparative example 1. melamine is not added when presoma prepares；Step obtains TiO after 2. calcining2。
See Fig. 7, the XRD spectrum of product shows, the TiO of this comparative example synthesis2It is Detitanium-ore-type, the data with standard （JCPDS file No.21-1272）It is consistent, does not find the crystal formation of other rutile or brookite type.25.34 °, 37.76 °, 48.14 °, 55.12 ° and 62.76 °, correspond respectively to anatase TiO2's（101）,（004）、（200）、(211) (204) crystal face.
See Fig. 8, the TEM collection of illustrative plates of product shows, the TiO of spherical shape2Certain polymerization is presented, the size of particle is 20~40 nm。
See Fig. 9, the UV-Vis DRS spectrum of product shows, the TiO of the present embodiment synthesis2Mainly in UV light area There is absorption in domain.
Method according to embodiment 1 detects TiO prepared by this comparative example2Photocatalysis performance, the photocatalysis of methylene blue Degradation rate reaches 81.81%.

Claims (1)

1. a kind of preparation method of composite visible light catalyst, the composite visible light catalyst is TiO2/g-C3N4Composite visible light Catalyst, it is characterised in that comprise the following steps：
1. the preparation of presoma, titanium source and nitrogen source are uniformly dispersed in 15 DEG C~35 DEG C ethanol, and the concentration of titanium source is 0.0001g/mL~1.5g/mL, the concentration of nitrogen source is 0.0001g/mL~1g/mL, then again to containing titanium under stirring Water is added dropwise in the ethanol of source and nitrogen source and obtains mixed material, the dripping quantity of water is the 10%~500% of ethanol volume；By mixed material In 70 DEG C~85 DEG C of water-bath, it is evaporated under stirring and obtains presoma；The titanium source is Ti (OBu)4Or TiF4, nitrogen source It is melamine or urea；
2. the presoma that 1. step prepares 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.
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