CN102580742A - Activated carbon-loaded cuprous oxide photocatalyst and preparation method thereof - Google Patents
Activated carbon-loaded cuprous oxide photocatalyst and preparation method thereof Download PDFInfo
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- CN102580742A CN102580742A CN2012100242834A CN201210024283A CN102580742A CN 102580742 A CN102580742 A CN 102580742A CN 2012100242834 A CN2012100242834 A CN 2012100242834A CN 201210024283 A CN201210024283 A CN 201210024283A CN 102580742 A CN102580742 A CN 102580742A
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
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Abstract
The invention provides an activated carbon-loaded cuprous oxide photocatalyst which can be used as a photocatalyst for degrading the organic pollutant such as phenols and purifying the air, wherein a preparation method of the activated carbon-loaded cuprous oxide photocatalyst comprises the following steps of: dipping the treated activated carbon in copper sulfate solution, and reducing by C6O12O6 or Na2SO3. The invention has the beneficial effects that the preparation of the activated carbon-loaded cuprous oxide photocatalyst takes copper sulfate as raw material, takes the activated carbon as a carrier, and loads the cuprous oxide on the activated carbon, so that the photocatalyst is simple in preparation method, low in cost, good in stability, and high in photocatalytic activity. The photocatalyst can be directly used for catalytically oxidizing the waste water such as the phenols and purifying the indoor air under an ultraviolet-visible light condition, so that the method is easy to operate, mild in reaction condition, and high in pollutant removing ratio.
Description
Technical field
The present invention relates to a kind of activated carbon supported type photochemical catalyst and preparation method thereof, this catalyst is applicable to the purification method of wastewater treatments such as dyestuff and indoor pollution air.
Background technology
China is first big country of DYE PRODUCTION and consumption, and dye well dyeing waste water contaminant capacity is big and wide.The dye well dyeing waste water has characteristics such as the water yield is big, colourity is high, complex chemical composition, bio-refractory, is one of bigger industrial wastewater of difficulty of governance.BOD, COD, organic toxic substance and colourity etc. are the major pollutants in this type waste water, if these pollutants are unprocessed or deal with improperly with discharge of wastewater, will produce severe contamination to water body.Usually; The dye well dyeing waste water generally adopts filtration, coagulation, is precipitated as main physico-chemical process; Because this type waste water contains a large amount of biodegradable aromatic series organic matter, heterocycle and polycyclic compounds of being difficult to; And content is higher, and the domestic and international at present processing to this type of waste water does not all have desirable processing method.The photocatalytic oxidation degradation of dye waste water is the hot technology that latest developments are got up.Photocatalysis oxidation technique utilizes ultraviolet light or visible light irradiation to have the semiconductor light-catalyst of photocatalytic activity, belongs to metal oxide semiconductor, sulfide or composite oxides etc. more.Like titanium dioxide (TiO
2), zinc oxide (ZnO), zinc sulphide (ZnS), tungstic acid (WO
3), cadmium sulfide (CdS), bismuth oxide (Bi
2O
3) etc., semi-conductive intragranular contains band structure, and it can be with usually by a low energy valence band (Valent band who is full of electronics; VB) and high energy conduction band (the Conduct band of a sky; CV) constitute, separated by the forbidden band between valence band and the conduction band, the size in this zone is called energy gap; It can differ from and be that band-gap energy, semi-conductive band-gap energy are generally 0. 2~3. 0 eV.When catalyst was penetrated in the illumination that is equal to or greater than band-gap energy with energy, the electronics on the valence band was excited, and crossed the forbidden band and got into conduction band, on valence band, produced corresponding hole simultaneously, and promptly light induced electron/hole is to (e
-/ h
+).Light induced electron on conduction band has stronger reducing power, and the photohole on valence band has very strong oxidisability.Because the discontinuity of semiconductor energy gap, the life-span in electronics and hole is longer, under electric field action or through the mode that spreads, moves, and is adsorbed on the lip-deep material generation of catalyst particle redox reaction, is perhaps captured by the lattice surface defective.Hole and electronics in catalyst inside or the surface also maybe be directly compound.Under illumination condition, the photocatalytic process on the semiconductor can be divided into the completion of four steps: the absorption electrons/ through light is separated; The absorption of reactant; Redox reaction; The product desorption.In this process, because the photohole that the ultraviolet excitation semiconductor produces and move to semiconductor surface and captured the back by water or hydroxyl and form hydroxyl radical free radical and have very strong oxidability, can the most organic pollutions of oxidation and to make it permineralization be CO
2, like all kinds of organic pollutions such as dyestuff, aldehydes matter, alkene, aldehydes, Polychlorinated biphenyls, surfactants.
At present, adopting maximum semiconductor light-catalysts is TiO
2Titanium dioxide has physical characteristics such as high specific area, high density, blemish and high surface ability and nontoxic, stable, chemical property such as catalytic activity is high, reaction speed is fast; Simultaneously low and can make the thorough mineralizing and degrading of organic matter to the selectivity of organic pollutant degradation again; Do not cause advantages such as secondary pollution, in the actual production life is used, be widely used.But because TiO
2Greater band gap (Eg=3.2 eV), can only be by ultraviolet excitation (λ<387 nm), and sunshine medium ultraviolet light only accounts for 3~4 % of sunshine gross energy, has greatly limited its research and application.If adopt artificial ultraviolet source, then need expensive equipment, thereby improve TiO
2Photochemical catalyst visible light-responded or develop meaning and the broad prospect of application that all kinds of visible light responsive photocatalysts have particular importance, and can derive many new industries simultaneously.Main method has: 1) adopt doped transition metal ions TiO
2The preparation visible light catalyst; 2) through transition metal and nonmetalloid codope; 3) through nonmetalloid calking and displacement doped Ti O
2Realize that the visible light catalytic effect is considered to a key progress.Yet with l) method is the same, the activity of the photochemical catalyst of acquisition under visible light be well below the activity of business-like Degussa P25 under ultraviolet light, and its used light source still has tangible ultraviolet light, and the activity under ultraviolet light the two is approaching; 4) utilize dye sensitization TiO
2Realize the visible light catalytic effect.This respect scientist has made a large amount of elaborations, has obtained the impressive progress of dyestuff contaminant degraded under excited by visible light.
Catalytic wet air oxidation is a kind of treatment technology of handling organic wastewater that last century, the eighties grew up in the world, but costs an arm and a leg, and makes its application receive great restriction.Photocatalysis oxidation technique is that the organic wastewater and the indoor air purification that grow up over past ten years are handled one of important method.Cuprous oxide (Cu
2O) be the p type, semiconductor material of direct band gap, of many uses.At the bactericide of coatings industry as marine antifouling priming paint; Be used for red glass and red enamel colouring agent in glass industry; Be used as catalyst in organic industry.Existing bibliographical information (the Li-Li Ma et al of cuprous oxide that utilize as the photocatalyst for degrading organic dye waste water; Materials Research Bulletin 45 (2010) 961 – 968); Invention (the Fukumoto that copper compound matrix activated carbon deodorant is also arranged; Kazuhiro et al, JP 2004166920) and activated charcoal carried copper oxide (CuO) be used for the invention (CN 1876232A) of coking chemical waste water.Although photocatalysis oxidation technique has treatment effect preferably, this technology will realize that industrialization also need be in selection visible light response catalyst active component, the separation that solves catalyst, aspect the making a breakthrough property achievements such as selection of carrier to waste water from dyestuff, indoor pollution air etc.
Summary of the invention
Technical problem to be solved by this invention is: propose a kind of dye wastewater treatment using and indoor pollution air with visible light response catalyst and preparation method thereof, and carry out the processing that Treatment by Photocatalysis Oxidation has waste water from dyestuff and indoor air pollutants with shaped activated carbon loaded catalysts such as this powdery and particles.
Technical scheme of the present invention:
A kind of powder or granular active carbon load cuprous oxide photochemical catalyst, its component and content are:
The cuprous oxide weight percent content is 1.0-5.0%, and the active carbon weight percent content is 95.0-99.0%.
A kind of preparation method of activated carbon supported cuprous oxide photochemical catalyst, this method may further comprise the steps:
(1) filters after active carbon is stirred 24h with 3mol/L ammonia spirit dipping, be washed till neutrality with distilled water;
(2) step (1) active carbon processed is used 5mol/L HNO
3Solution impregnation is filtered after stirring 24h, is washed till neutrality with distilled water, puts into baking oven, and is in 110 ℃ of oven dry, subsequent use;
(3) take by weighing the CuSO that a certain amount of pretreated active carbon impregnated in 0.04mol/L ~ 0.2 mol/L respectively
4In the solution, be 90rpm at rotating speed, temperature is in 25 ℃ the constant temperature culture oscillator behind the dipping 24h, filters.
(4) active carbon that step (3) is obtained is transferred to proper C
6H
12O
6In NaOH solution, place the constant temperature culture oscillator again, temperature is 30 ℃, rotating speed is rotational oscillation 24h under the 90rpm condition, takes out washing to neutral.
(5) loaded Cu that step (4) is obtained
2The active carbon of O changes dry 3h in 80 ℃ the vacuum drying chamber over to, makes activated carbon supported cuprous oxide photochemical catalyst.
The present invention compares the beneficial effect that is had with prior art:
The preparation of activated carbon supported cuprous oxide photochemical catalyst is to be raw material with copper sulphate, is carrier with the active carbon, and cuprous oxide is downloaded on the active carbon, and method for preparing catalyst is easy, cheap, good stability, photocatalytic activity are high.With waste water and indoor air purifications such as this catalyst oxidation phenols, can under the ultraviolet-visible optical condition, directly carry out, easy operating, reaction condition is gentle, and the clearance of pollutant is high.
Description of drawings
Fig. 1 is a column-shaped active carbon SEM pattern.
Fig. 2 is a column-shaped active carbon surface scan electron microscope pattern.
Fig. 3 a is Cu
2The bar-shaped Cu of O carried-type active carbon surface
2O SEM pattern
Fig. 3 b is the ability spectrogram of Fig. 3 a.
Fig. 4 is Cu
2The starlike Cu of O carried-type active carbon surface
2O SEM pattern.
Fig. 5 is Cu
2The relevant x-ray diffraction pattern of O carried active carbon.
Fig. 6 is Cu
2The absorption spectrum of O carried active carbon degraded catechol.
The specific embodiment
Following embodiment further specifies activated carbon supported cuprous oxide photochemical catalyst provided by the invention, preparation method and application.
Activated carbon supported cuprous oxide photochemical catalyst and preparation method
(1) filters after active carbon is stirred 24h with 3mol/L ammonia spirit dipping, be washed till neutrality with distilled water;
(2) step (1) active carbon processed is used 5mol/L HNO
3Solution impregnation is filtered after stirring 24h, is washed till neutrality with distilled water, puts into baking oven, and is in 110 ℃ of oven dry, subsequent use;
(3) take by weighing the CuSO that the pretreated active carbon of 5g impregnated in 50mL 0.04mol/L
4In the solution, be 90rpm at rotating speed, temperature is in 25 ℃ the constant temperature culture oscillator behind the dipping 24h, filters.
(4) active carbon that step (3) is obtained is transferred to and contains 0.2g C
6H
12O
650mLNaOH (0.05mol/L) solution in, place the constant temperature culture oscillator again, temperature is 30 ℃, rotating speed is rotational oscillation 24h under the 90rpm condition, crosses to filter product, washing is to neutral.
(5) loaded Cu that step (4) is obtained
2The active carbon of O changes dry 3h in 80 ℃ the vacuum drying chamber over to, makes activated carbon supported 1% cuprous oxide photochemical catalyst.
Step (1), (2) are identical with implementation method one;
(3) take by weighing the CuSO that the pretreated active carbon of 5g impregnated in 0.2mol/L
4In the solution, be 90rpm at rotating speed, temperature is in 25 ℃ the constant temperature culture oscillator behind the dipping 24h, filters.
(4) active carbon that step (3) is obtained is transferred to and contains 0.6g C
6H
12O
650mLNaOH (0.2mol/L) NaOH solution in, place the constant temperature culture oscillator again, temperature is 30 ℃, rotating speed is rotational oscillation 24h under the 90rpm condition, crosses to filter product, washing is to neutral.
(5) loaded Cu that step (4) is obtained
2The active carbon of O changes dry 3h in 80 ℃ the vacuum drying chamber over to, makes activated carbon supported 5% cuprous oxide photochemical catalyst.
Embodiment 3
Step (1), (2) are identical with implementation method one;
(3) get 5g step (2) active carbon processed, 50mL 0.2mol/L CuSO
4With 50mL 0.05 mol/L Na
2SO
3Be positioned in the beaker of 500 mL and react, to cushioning liquid that wherein adds 300 mL pH=5 HAc-NaAc and 0.1g glucose, reaction 3h or microwave 30min under 70 ℃ of conditions cross and filter product, and washing is to neutral.
(4) loaded Cu that step (3) is obtained
2The active carbon of O changes dry 3h in 80 ℃ the vacuum drying chamber over to, makes activated carbon supported 1% cuprous oxide photochemical catalyst.
Instance with waste water such as activated carbon supported cuprous oxide photocatalyst treatment phenols.
Instance 4
Take by weighing an amount of catechol solid and be configured to the catechol solution of 100mg/L, with the Cu of instance 1 preparation
2O/AC is a photochemical catalyst, utilizes the incandescent lamp of 200W to be light source, is the maximum absorption wavelength of the catechol aqueous solution with 275 nm, surveys its absorbance.The photocatalytic degradation rate K of sample is with computes:
K=[(A
0-A
t)/A
0]×100%
In the formula: A
O, the absorbance of initial sample; A
t, the absorbance of sample when the reaction time is t.Absorption spectrum after the degraded such as Fig. 6.Behind the degraded 2.5h, degradation rate reaches more than 80%.Use more than 4 times after the catalyst recovery after the recovery, degradation efficiency is constant basically.
Take by weighing the methyl orange solution of certain density autogamy, with the Cu of instance 3 preparations
2O/AC is a photochemical catalyst, the photochemical reactor that utilizes Kaifeng Red Star scientific instrument factory to produce, and employing dominant wavelength is that the 300W mercury lamp of 365 nm is done radiation source, is the maximum absorption wavelength of methyl orange solution with 463nm, surveys its absorbance.The photocatalytic degradation rate K of sample presses instance 4 methods and calculates.Behind the degraded 2h, degradation rate reaches more than 98%.Use more than 4 times after the catalyst recovery after the recovery, degradation efficiency is constant basically.
Can know that by the instance 4 and the degradation rate of instance 5 degradeds the effect of activated carbon supported cuprous oxide catalysis degradable organic pollutant is remarkable.The activated carbon supported cuprous oxide photochemical catalyst its preparation method that the present invention makes is simple, cheap, good stability, high, reusable to the clearance of organic pollution, has good economic competitiveness.
Claims (8)
1. activated carbon supported cuprous oxide photochemical catalyst, it is characterized in that: cuprous oxide is deposited on the acid-treated active carbon, and the cuprous oxide weight percent content is 1.0-5.0%, and the active carbon weight percent content is 95.0-99.0%.
2. photochemical catalyst according to claim 1 is characterized in that: said photochemical catalyst impregnated in CuSO through active carbon
4And C
6H
12O
6Alkaline solution in, make through redox reaction.
3. photochemical catalyst according to claim 1 is characterized in that: said photochemical catalyst impregnated in CuSO through active carbon
4And Na
2SO
3In the solution, in HAc-NaAc cushioning liquid, heat, make through redox reaction.
4. photochemical catalyst according to claim 1 is characterized in that: described active carbon is column, cylindric, amorphous granular shape or Powdered.
5. the preparation method of the described photochemical catalyst of claim 1, its step is following:
Pretreated active carbon impregnated in the CuSO of 0.04mol/L ~ 0.2 mol/L
4In the solution, be 90rpm at rotating speed, temperature is in 25 ℃ the constant temperature culture oscillator behind the dipping 24h, filters;
The active carbon that obtains is transferred to C
6H
12O
6In NaOH solution, place the constant temperature culture oscillator again, be 30 ℃ in temperature, rotating speed is rotational oscillation 24h under the 90rpm condition, takes out washing to neutral;
The product that obtains changed over to dry 3h in 80 ℃ the vacuum drying chamber, make activated carbon supported cuprous oxide photochemical catalyst.
6. the preparation method of the described photochemical catalyst of claim 1, its step is following:
With pretreated active carbon, 50mL 0.04mol/L CuSO
4With 50mL 0.05 mol/L Na
2SO
3Be positioned in the beaker of 500 mL and react, to cushioning liquid that wherein adds 300 mL pH=5 HAc-NaAc and 0.1g glucose, under 70 ℃ of conditions, react 3h, filter, washing is to neutral;
With the loaded Cu that obtains
2The active carbon of O changes dry 3h in 80 ℃ the vacuum drying chamber over to, makes activated carbon supported 1% cuprous oxide photochemical catalyst.
7. according to claim 5 or 6 described preparation methods, it is characterized in that described preliminary treatment comprises:
Filter after active carbon stirred 24h with 3mol/L ammonia spirit dipping, be washed till neutrality with distilled water;
Then active carbon processed is used 5mol/L HNO
3Solution impregnation is filtered after stirring 24h, is washed till neutrality with distilled water, in 110 ℃ of oven dry.
8. the purposes of the described photochemical catalyst of claim 1 is as the photocatalytic degradation of phenols such as catechol, aldehydes organic pollution.
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