CN106512977A - Preparation method and application of activated carbon doped titanium dioxide nano photocatalyst - Google Patents

Preparation method and application of activated carbon doped titanium dioxide nano photocatalyst Download PDF

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Publication number
CN106512977A
CN106512977A CN201610896156.1A CN201610896156A CN106512977A CN 106512977 A CN106512977 A CN 106512977A CN 201610896156 A CN201610896156 A CN 201610896156A CN 106512977 A CN106512977 A CN 106512977A
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activated carbon
titanium dioxide
dioxide nano
nano photocatalyst
carbon doping
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CN201610896156.1A
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Inventor
许航
吴章
高晓宏
林晨烁
丁明梅
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Hohai University HHU
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Hohai University HHU
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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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • 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
    • B01J35/002—Catalysts characterised by their physical properties
    • B01J35/004—Photocatalysts
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
    • B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
    • 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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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 relates to a preparation method and an application of an activated carbon doped titanium dioxide nano photocatalyst. The preparation method comprises the following steps of: (1) uniformly mixing absolute ethyl alcohol, glacial acetic acid and butyl titanate in a volume ratio, adding an ethyl alcohol aqueous solution into the mixed solution drop by drop, and conducting stirring for later use; (2) dissolving dried activated carbon into ultrapure water, performing centrifugal separating, taking out an upper-layer liquid and dropwise adding the upper-layer liquid into the solution prepared in the step (1) drop by drop, and performing stirring for later use; and (3) transferring the solution prepared in the step (2) into a microwave reactor to be subjected to a microwave reaction, performing centrifugal separating after the microwave reaction is ended, cleaning the obtained solid, and performing drying and grinding to obtain the activated carbon doped titanium dioxide nano photocatalyst. The activated carbon doped titanium dioxide nano photocatalyst prepared by the preparation method has the characteristic of remarkably absorbing visible light, has relatively high photocatalytic activity, and can be applied to degrading organic pollutants in water.

Description

The preparation method and application of activated carbon doping titanium dioxide nano photocatalyst
Technical field
The invention belongs to catalysis material and organic pollution light degradation field, and in particular to activated carbon is titania-doped The preparation method and application of nano-photocatalyst.
Background technology
TiO2With good biological, chemical, photochemical stability, wastewater treatment, harmful gass it have been widely used in The field such as purification, cosmetics manufacture, construction material, textile product, coating, solar energy storage and conversion, laser chemistry conversion.But It is TiO2It is broadband conductor, with wider energy gap（3.0~3.2eV）, it is only just active in black light area.Pure TiO2 It is 4% to the utilization rate of sunlight, so, in recent years in order to improve TiO2Photoelectron effect and the utilization rate to sunlight, adopt With methods such as the photosensitization of metal-doped, dyestuff, the depositions of noble metal to TiO2It is modified, but as dyestuff and metal exist Have in natural water and clearly limit, or even the heavy metal having contains overt toxicity, it is risky for photocatalysis technology.
Activated carbon is a kind of solid carbonaceous of black porous, by coal by crush, molding or with uniform coal grain Jing carbonizations, Activation production, specific surface area are larger, with stronger absorption property, are a kind of extremely wide industrial adsorbents of purposes and activated carbon With the absorbent properties stronger to light.
The content of the invention
Goal of the invention：The present invention is directed to pure TiO2A kind of low problem of energy gap width, sun light utilization efficiency, there is provided activity The preparation method and application of charcoal doping titanium dioxide nano photocatalyst, accumulates larger using activated carbon surface, notable to visible ray The characteristic of absorption is to TiO2It is modified, the catalyst for preparing has higher photocatalytic activity.
Technical scheme：
The preparation method of activated carbon doping titanium dioxide nano photocatalyst, comprises the steps：
（1）It is 3 by volume by dehydrated alcohol, glacial acetic acid and butyl titanate:0.5~1:0.5 ~ 1 mix homogeneously, then to mixed liquor In be added dropwise over ethanol water, stir 0.5 ~ 1.0 hour, it is standby；
（2）Dried activated carbon is dissolved in ultra-pure water, centrifugation, takes supernatant liquid and dropwise instill step（1）It is prepared into To solution in, stir 0.5 ~ 1.0 hour, it is standby；
（3）By step（2）The solution for preparing carries out microwave reaction in proceeding to microwave reactor, after reaction terminates, by product Centrifugation, the solid cleaning for obtaining, dry, grinding, obtains final product activated carbon doping titanium dioxide nano photocatalyst.
Further, step（1）In, in the ethanol water, ethanol is 1 with the volume ratio of water:1~2.
Further, step（2）In, the baking temperature of activated carbon is 60 ~ 80 DEG C, and drying time is 12 ~ 24 hours.
Further, step（2）In, the supernatant liquid and step（1）The liquor capacity ratio for preparing is 1:4~8.
Further, step（3）In, the condition of microwave reaction is：120 ~ 160W of microwave power, reacts 15 ~ 30 minutes.
Further, step（3）In, solid baking temperature is 60 ~ 80 DEG C, and baking temperature is 12 ~ 24 hours.
Activated carbon doping titanium dioxide nano photocatalyst organic dirt in degradation water that the preparation method is prepared The application of dye thing.
Beneficial effect：
（1）The present invention prepares the titanium dioxide nano photocatalysis agent of activated carbon doping using microwave method, and raw material is cheap and easy to get, prepares Process operation is simple, and synthesis is convenient；
（2）The activated carbon doping titanium dioxide nano photocatalyst for preparing has relative to pure titanium dioxide optical catalyst Higher visible light activity, photocatalysis efficiency are higher；
（3）The activated carbon doping titanium dioxide nano photocatalyst for preparing is relative to pure titanium dioxide optical catalyst to can See the absorption of light more preferably, advantageously more photoelectricity holes pair are produced in titanium dioxide.
Description of the drawings
Fig. 1 is the SEM photograph of the activated carbon modified titanium dioxide optical catalyst that test is obtained；
Fig. 2 is to test the activated carbon modified titanium dioxide optical catalyst UV-vis DRS spectrogram under three（DRS schemes）；
Fig. 3 is to test the activated carbon modified titanium dioxide optical catalyst fluorescence spectra under three（PL schemes）；
Fig. 4 is activated carbon modified titanium dioxide optical catalyst Photocatalytic activity curve chart in experiment four.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.This The solvent that invention is adopted is the pure level of analysis, and methods described is conventional method if no special instructions.
Embodiment 1
The preparation method of activated carbon doping titanium dioxide nano photocatalyst, comprises the steps：
（1）By 60ml dehydrated alcohol, 20ml glacial acetic acid and 20ml butyl titanate mix homogeneously, then second is added dropwise in mixed liquor Alcohol-water solution（Ethanol is 1 with the volume ratio of water:1）, persistently stir 0.5 hour, it is standby；
（2）After 10 mg activated carbons are put 60 DEG C of dryings in an oven 24 hours, it is dissolved in 50 ml ultra-pure waters, ultrasonic disperse takes Supernatant liquid dropwise instills step（1）In the solution for preparing, stir 0.5 hour, it is standby；
（3）By step（2）The solution for preparing is proceeded in microwave reactor, under the microwave power of 120w, is reacted 15 minutes, By the final product centrifugation for obtaining, it is respectively washed three times with ultra-pure water and dehydrated alcohol, puts 60 DEG C of dryings 12 in an oven Hour, grinding obtains final product the titanium dioxide nano photocatalysis agent of 1% activated carbon doping（1% AC@TiO2Photocatalyst）.
Using 1% AC@TiO of the scanning electron microscope to obtained visible-light response type2Photocatalyst carries out Electronic Speculum and sweeps Retouch and obtain SEM figures as shown in Figure 1, as can be seen from Figure 1 1% AC@TiO of obtained visible-light response type2Photocatalyst is Nanometer sheet, surface have a small amount of activated carbon to cover.
Using 1%AC@TiO of the full-automatic fluorescence spectrophotometer to obtained visible-light response type2Photocatalyst is characterized, PL figures as shown in Figure 3 are obtained, as can be seen from Figure 3 the 1%AC@TiO of visible-light response type obtained in embodiment 12Photocatalyst Relative to pure TiO2Under excitation wavelength, the excitation peak of generation is lower, therefore advantageously separates with hole in photoelectron, helps In the degraded for pollutant, this is the effect that activated carbon is effectively conducted photoelectron ability.Activated carbon modified titanium dioxide Compared with titanium dioxide optical catalyst, fluorescence intensity is substantially reduced photocatalyst, is illustrated by activated carbon modified titanium-dioxide photo Catalyst effectively increases photoelectronic separation efficiency.
Using 1%AC@TiO of the UV-vis DRS spectrogrph to obtained visible-light response type2Photocatalyst carries out electricity Scarnning mirror, obtains DRS figures as shown in Figure 2, as can be seen from Figure 2 the 1%AC@TiO of visible-light response type obtained in embodiment 12 Photocatalyst is relative to pure TiO2Absorption of the photocatalyst in visible region to light is remarkably reinforced, thus produce more photoelectrons with Hole separates, and contributes to the degraded for pollutant.
Embodiment 2
The preparation method of activated carbon doping titanium dioxide nano photocatalyst, comprises the steps：
（1）By 60ml dehydrated alcohol, 20ml glacial acetic acid and 20ml butyl titanate mix homogeneously, then second is added dropwise in mixed liquor Alcohol-water solution（Ethanol is 1 with the volume ratio of water:1）, persistently stir 0.5 hour, it is standby；
（2）After 20 mg activated carbons are put 60 DEG C of dryings in an oven 24 hours, it is dissolved in ultra-pure water, ultrasonic disperse takes upper liquid Body dropwise instills step（1）In the solution for preparing, stir 0.5 hour, it is standby；
（3）By step（2）The solution for preparing is proceeded in microwave reactor, under the microwave power of 120w, is reacted 15 minutes, By the final product centrifugation for obtaining, it is respectively washed three times with ultra-pure water and dehydrated alcohol, puts 60 DEG C of dryings 12 in an oven Hour, grinding obtains final product the titanium dioxide nano photocatalysis agent of 1% activated carbon doping（2% AC@TiO2Photocatalyst）.
Embodiment 3
The preparation method of activated carbon doping titanium dioxide nano photocatalyst, comprises the steps：
（1）By 60ml dehydrated alcohol, 20ml glacial acetic acid and 20ml butyl titanate mix homogeneously, then second is added dropwise in mixed liquor Alcohol-water solution（Ethanol is 1 with the volume ratio of water:1）, persistently stir 0.5 hour, it is standby；
（2）After 4 mg activated carbons are put 60 DEG C of dryings in an oven 24 hours, it is dissolved in ultra-pure water, ultrasonic disperse takes upper liquid Body dropwise instills step（1）In the solution for preparing, stir 0.5 hour, it is standby；
（3）By step（2）The solution for preparing is proceeded in microwave reactor, under the microwave power of 120w, is reacted 15 minutes, By the final product centrifugation for obtaining, it is respectively washed three times with ultra-pure water and dehydrated alcohol, puts 60 DEG C of dryings 12 in an oven Hour, grinding obtains final product the titanium dioxide nano photocatalysis agent of 1% activated carbon doping（0.4 % AC@TiO2Photocatalyst）.
Embodiment 4
The preparation method of activated carbon doping titanium dioxide nano photocatalyst, comprises the steps：
（1）By 60ml dehydrated alcohol, 20ml glacial acetic acid and 20ml butyl titanate mix homogeneously, then second is added dropwise in mixed liquor Alcohol-water solution（Ethanol is 1 with the volume ratio of water:1）, persistently stir 0.5 hour, it is standby；
（2）After 2 mg activated carbons are put 60 DEG C of dryings in an oven 24 hours, it is dissolved in ultra-pure water, ultrasonic disperse takes upper liquid Body dropwise instills step（1）In the solution for preparing, stir 0.5 hour, it is standby；
（3）By step（2）The solution for preparing is proceeded in microwave reactor, under the microwave power of 120w, is reacted 15 minutes, By the final product centrifugation for obtaining, it is respectively washed three times with ultra-pure water and dehydrated alcohol, puts 60 DEG C of dryings 12 in an oven Hour, grinding obtains final product the titanium dioxide nano photocatalysis agent of 1% activated carbon doping（0.2 % AC@TiO2Photocatalyst）.
Embodiment 5
The AC@TiO that embodiment 1 ~ 4 is prepared2Photocatalyst is used for oxidation processes methylene blue solution.
Degradation step is：
Step（1）：The methyl blue of 20mg is accurately weighed, is dissolved in ultra-pure water, and be settled to 1000ml, be obtained 20mg/L's Methylene blue solution；
Step（2）：50ml steps are pipetted accurately with pipet（1）The methylene blue solution for obtaining is into reactor, and adds respectively It is pure activated carbon to enter 40mg doping mass fractions（PAC）、TiO2Photocatalyst and 1% AC@TiO2Photocatalyst, reaction system control It is 0.8 g/L that system adjusts catalyst concn at 25 DEG C, respectively, the first adsorption equilibrium half an hour at half-light so as to reach absorption de- Attached balance；
Step（3）：Using 300w xenon lamps as visible light source, by step（2）It is anti-that resulting solution carries out photocatalytic degradation under light illumination Should, at interval of 5 ~ 30min time samplings, and methylene blue absorbance is measured with ultraviolet visible spectrophotometry, and calculate its turn Rate.
As a result it is as shown in Figure 4, it can be seen that when catalyst is 1% AC TiO2When, catalytic effect is best.When activated carbon contains When amount is not high, with the rising of activated carbon content, the photocatalysis effect of composite gradually strengthens, when activated carbon content 1% Effect is best；When activated carbon content is 2%, composite photocatalytic activity is substantially reduced, and is excessively to cause light due to activated carbon Active site is capped, and causes photocatalysis effect substantially to reduce, because suction of the introducing of activated carbon to material to visible ray Receive and strengthen, and activated carbon can also conduct the electronics of titanium dioxide conduction band, the light induced electron of titanium dioxide separates effect with hole Fruit strengthens.

Claims (7)

1. the preparation method of activated carbon doping titanium dioxide nano photocatalyst, it is characterised in that comprise the steps：
（1）It is 3 by volume by dehydrated alcohol, glacial acetic acid and butyl titanate:0.5~1:0.5 ~ 1 mix homogeneously, then to mixed liquor In be added dropwise over ethanol water, stir 0.5 ~ 1.0 hour, it is standby；
（2）Dried activated carbon is dissolved in ultra-pure water, centrifugation, takes supernatant liquid and dropwise instill step（1）It is prepared into To solution in, stir 0.5 ~ 1.0 hour, it is standby；
（3）By step（2）The solution for preparing carries out microwave reaction in proceeding to microwave reactor, after reaction terminates, by product Centrifugation, the solid cleaning for obtaining, dry, grinding, obtains final product activated carbon doping titanium dioxide nano photocatalyst.
2. the preparation method of activated carbon doping titanium dioxide nano photocatalyst according to claim 1, it is characterised in that step Suddenly（1）In, in the ethanol water, ethanol is 1 with the volume ratio of water:1~2.
3. the preparation method of activated carbon doping titanium dioxide nano photocatalyst according to claim 1, it is characterised in that step Suddenly（2）In, the baking temperature of activated carbon is 60 ~ 80 DEG C, and drying time is 12 ~ 24 hours.
4. the preparation method of activated carbon doping titanium dioxide nano photocatalyst according to claim 1, it is characterised in that step Suddenly（2）In, the supernatant liquid and step（1）The liquor capacity ratio for preparing is 1:4~8.
5. the preparation method of activated carbon doping titanium dioxide nano photocatalyst according to claim 1, it is characterised in that step Suddenly（3）In, the condition of microwave reaction is：120 ~ 160W of microwave power, reacts 15 ~ 30 minutes.
6. the preparation method of activated carbon doping titanium dioxide nano photocatalyst according to claim 1, it is characterised in that step Suddenly（3）In, solid baking temperature is 60 ~ 80 DEG C, and baking temperature is 12 ~ 24 hours.
7. the activated carbon doping titanium dioxide nano photocatalyst that preparation method described in any one of claim 1 ~ 6 is prepared exists The application of degraded organic pollutants.
CN201610896156.1A 2016-10-13 2016-10-13 Preparation method and application of activated carbon doped titanium dioxide nano photocatalyst Pending CN106512977A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109772328A (en) * 2019-01-29 2019-05-21 蚌埠学院 Titanium dioxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent methods for making and using same
CN111921494A (en) * 2020-06-30 2020-11-13 长江大学 Xanthoceras sorbifolia activated carbon adsorbent and preparation method and application thereof
CN113578361A (en) * 2021-07-22 2021-11-02 南京工业大学 Nano C/N/Si/TiO2Preparation method of photocatalytic composite material

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CN101318129A (en) * 2008-07-23 2008-12-10 刘守新 Supported optical catalyst and preparation method thereof
CN105797700A (en) * 2016-03-17 2016-07-27 中国计量学院 Preparation method of coconut shell activated carbon supported TiO2 photocatalyst

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CN101318129A (en) * 2008-07-23 2008-12-10 刘守新 Supported optical catalyst and preparation method thereof
CN105797700A (en) * 2016-03-17 2016-07-27 中国计量学院 Preparation method of coconut shell activated carbon supported TiO2 photocatalyst

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109772328A (en) * 2019-01-29 2019-05-21 蚌埠学院 Titanium dioxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent methods for making and using same
CN111921494A (en) * 2020-06-30 2020-11-13 长江大学 Xanthoceras sorbifolia activated carbon adsorbent and preparation method and application thereof
CN113578361A (en) * 2021-07-22 2021-11-02 南京工业大学 Nano C/N/Si/TiO2Preparation method of photocatalytic composite material

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Application publication date: 20170322