CN105148983B - Photochemical catalyst of dyestuff and preparation method thereof in a kind of degrading waste water - Google Patents
Photochemical catalyst of dyestuff and preparation method thereof in a kind of degrading waste water Download PDFInfo
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- CN105148983B CN105148983B CN201510630598.7A CN201510630598A CN105148983B CN 105148983 B CN105148983 B CN 105148983B CN 201510630598 A CN201510630598 A CN 201510630598A CN 105148983 B CN105148983 B CN 105148983B
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- 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
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Abstract
The invention discloses photochemical catalyst of dyestuff in a kind of degrading waste water and preparation method thereof, belong to photocatalysis field.The photochemical catalyst of dyestuff is using mesoporous silicon oxide as carrier in degrading waste water of the present invention, and the mesoporous silicon oxide supported on carriers has the nano zine oxide of doping copper；The mass fraction of Zn-ef ficiency is 5 40%, and the mass fraction of copper is 0.1 5%.The photochemical catalyst catalytic degradation methylene blue of dyestuff or rhodamine B are visible light-responded, cost is low, degradation efficiency is high, stability good in degrading waste water of the present invention.
Description
Technical field
The present invention relates to photocatalysis field, the photochemical catalyst of dyestuff and its preparation side in more particularly to a kind of degrading waste water
Method.
Background technology
With industrial expansion, the water resource of many countries and regions all receives different degrees of pollution, and increasingly tight
Weight, seriously threatens natural environment and human health, therefore Industrial Waste Water Treatments are increasingly paid close attention to accordingly.In these works
In industry sewage, the features such as dyeing waste water is due to colourity depth, strong toxicity, difficult degradation, big pH value fluctuation takes conventional method difficult
To carry out effective processing to it.
Recently as going deep into for research, it has been found that photocatalysis has in terms of waste water control, solar energy conversion to lure
The application prospect of people.Wherein photocatalytic oxidation is as a kind of deep oxidation method method, so that its energy consumption is low, reaction condition is gentle, behaviour
Make simple, the low feature of cost, be acknowledged as most promising pollutant removal technology.
Zinc oxide is a kind of semi-conducting material of broad stopband, and band gap is 3.3 ev at room temperature, due to nonhazardous, ring
Border is friendly, it is easy to the advantages of preparing, and as a kind of new catalysis material.Under the irradiation of light, zinc oxide is produced after exciting
Raw light induced electron-photohole has the ability of oxidationreduction, can make organic matter after redox reaction by progressively
Degraded, is finally fully oxidized as environment amenable carbon dioxide, water and inorganic molecules.
In the technology that zinc oxide photocatalysis degrades dyeing waste water, it is important to which being to develop has high catalysis degradation modulus, height
The photochemical catalyst of stability, low production cost.
In order to improve the photocatalytic activity of zinc oxide, some metals or nonmetallic are generally added in zinc oxide, from
And suppress the compound of light induced electron electronics and photohole, so as to improve catalysis degradation modulus.
Chinese invention patent such as Publication No. " A of CN 102626625 " is disclosed to adulterate in Zinc oxide nanoparticle
Precious metals ag or Pd.Although having preferable degradation effect to wastewater degradation under visible light, the expensive price of noble metal
The practical application of catalyst can be govern to a certain extent.
" CN103977806 A " Chinese invention patent reports the doping metals Co in zinc oxide and is applied to Publication No.
The photocatalytic degradation of dyeing waste water.Although the catalyst has higher photocatalytic degradation effect, the catalyst can only be in ripple
Reacted under the long ultraviolet light less than 400nm.Generally, it is considered that the 5% of ultraviolet portion deficiency sunshine gross energy, and wavelength
The 43% of sunshine gross energy is accounted in 400 ~ 700 nm visible ray.Therefore it is to improve too to develop visible light-responded catalyst
Positive energy utilization rate, realizes an important directions of zinc oxide photocatalysis technology.
In addition, by semi-conducting material load on a inert carrier, can significantly improve the reaction stability of photochemical catalyst.It is public
The number of opening is " CN 1772375A " Chinese invention patent is rare-earth metal doped in nano zine oxide, then enters with porous material
Row mechanical mixture.Although the reaction stability of catalyst obtains the raising of part, the inhomogeneities of physical mixed still exists
The raising of catalyst performance is govern to a certain extent.
The content of the invention
Not enough in order to make up the above, the invention provides a kind of visible light-responded, cost is low, degradation efficiency is high, stability
Photochemical catalyst of dyestuff and preparation method thereof in good degrading waste water.
The technical scheme is that：
The photochemical catalyst of dyestuff in a kind of degrading waste water, using mesoporous silicon oxide as carrier, the mesoporous silicon oxide is carried
The nano zine oxide of doping copper is loaded with body.Wherein, nano zine oxide is major catalyst, and copper is co-catalyst.
Meso-porous titanium dioxide silicon carrier is preferably MCM types series, most preferably MCM-48 types mesoporous silicon oxide.The type mesoporous silicon oxide
It is used as carrier, catalytic efficiency highest.
Preferably, the mass fraction of Zn-ef ficiency is 5-40%, and the mass fraction of copper is 0.1-5%
Preferably, the mass fraction of Zn-ef ficiency is 20-25%, and the mass fraction of copper is 0.8-2%.Remaining is equal
For meso-porous titanium dioxide silicon carrier.
Application of the photochemical catalyst of dyestuff in degrading waste water Methylene Blue and rhodamine B in the degrading waste water.
Using the method for the photocatalyst for degrading methylene blue in waste and rhodamine B of dyestuff in the degrading waste water, to
The photochemical catalyst of dyestuff in the degrading waste water is added in waste water containing methylene blue and/or rhodamine B, is 420- in wavelength
Under 800nm light source irradiation, stirring reaction 0.2-6h filters out catalyst.Wherein, Wastewater Dyes content is 5-50mg/
L, the addition of catalyst is met：0.6-1.5mg catalyst/1mL waste water, preferably 0.8-1.2mg catalyst/1mL waste water；Should
Degradation reaction is carried out at room temperature, and the photocatalytic degradation time is preferably 2-3h.
The preparation method of the photochemical catalyst of dyestuff in the degrading waste water, including step：
1）Ground after the corresponding zinc salt of volatile acid and mantoquita are mixed, in air atmosphere, 1- is calcined in 300-600 DEG C
5 hours；
2）Room temperature is cooled to, then deionized water washing dries 1-10h, the nano-zinc oxide powder for the copper that must adulterate；
3）The nano-zinc oxide powder for the copper that adulterates is dispersed in the aqueous solution of cetyl trimethylammonium bromide
In, stir 1-6h at 20-50 DEG C；
4）PH to 9-13 is adjusted using concentrated ammonia liquor, the silicon source of mesoporous silicon oxide, aging 6-30h is added；
5）2-15h is dried in suction filtration, washing at 40-200 DEG C；
6）In being calcined 3-15h at 300-600 DEG C, room temperature is cooled to, the photochemical catalyst of dyestuff in degrading waste water is obtained.
Preferably, step 1）In, the corresponding zinc salt of volatile acid be zinc acetate, the crystalline hydrate of zinc acetate,
Zinc nitrate, the crystalline hydrate of zinc nitrate, zinc carbonate；The corresponding mantoquita of volatile acid is copper acetate, the crystalline hydrate of copper acetate
Thing, copper nitrate, the crystalline hydrate of copper nitrate, basic copper carbonate.
Preferably, step 1）In, the mol ratio of zinc salt and mantoquita is 1:1-400:1.
Preferably, the molal quantity of cetyl trimethylammonium bromide is Zn-ef ficiency, copper and element silicon mole
The 5%-20% of number summation.
Preferably, step 3）Cetyl trimethylammonium bromide in the aqueous solution of cetyl trimethylammonium bromide
Mass fraction be 1%-90%.
Preferably, step 4）The silicon source of intermediary hole silica is in tetraethyl orthosilicate, Ludox, white carbon
It is one or more of.It is furthermore preferred that the silicon source of mesoporous silicon oxide is tetraethyl orthosilicate.Meso-porous titanium dioxide is used as using tetraethyl orthosilicate
Preferably, degradation speed is fast for catalyst effect obtained by the silicon source of silicon, and degradation rate is high.
Beneficial effects of the present invention are：
1）Using Metaporous silicon dioxide material as carrier, the photochemical catalyst of the nano zine oxide of carried with doped copper.Jie
Hole earth silicon material has big aperture, than surface and pore volume, in addition, its surface has abundant silicone hydroxyl, with it
As carrier, be conducive to methylene blue molecule and rhodamine B molecule etc. in a large amount of absorption and enrichment on mesoporous material surface, this is
The nano zine oxide of doping Cu elements carries out rapid light degradation and provides abundant raw material preparation；Furthermore, Cu elements are in nanometer
The doping of zinc oxide, can cause zinc oxide absorption spectrum to be moved to high wavelength direction, and can make the catalyst under visible light
Photocatalysis is carried out, so as to reduce the operating cost of zinc oxide photocatalysis degraded.
2）Common synthetic method is taken in the preparation of catalyst, that is, by the nano zine oxide of the doping Cu elements prepared
Powder, is added in meso-porous titanium dioxide silicon precursor, aging is then hydrolyzed.This preparation method can not only keep the Cu that adulterates
Pattern, the crystal formation of the nano zine oxide of element, and light induced electron can be suppressed using carrier and carried metal strong effect power
With being combined for hole, promote hole and surface hydroxyl free radical more effectively degradation of methylene blue and rhodamine B, so as to improve
Photocatalytic activity；In addition, this preparation method can be such that carrier is uniformly mixed with carried metal, so as to improve photochemical catalyst
Reaction stability.
3）Methylene blue and/or rhodamine B in the photochemical catalyst catalytic degradation waste water of the present invention, can be in radiation of visible light
Under, room temperature condition is degraded, and reaction condition is gentle, and cost is low, it is easy to accomplish.
4）The photochemical catalyst of the present invention is easy to regeneration and used, and still has extraordinary photocatalysis performance after regeneration repeatedly.
Embodiment
Embodiment 1
After anhydrous nitric acid zinc and anhydrous nitric acid copper mechanical mixture, grind 20 minutes, the mol ratio of zinc salt and mantoquita is 1:1.
In air atmosphere, at 300 DEG C, it is calcined 3 hours.It is cooled to after room temperature, is washed with deionized 3 times, and in 80 DEG C of dry 2h,
The nano-zinc oxide powder of doping Cu elements is made.
Above-mentioned gained powder is added in the aqueous solution of cetyl trimethylammonium bromide, 4 is stirred at 20 DEG C small
When；With the pH of concentrated ammonia liquor regulation system（11-12）, then add tetraethyl orthosilicate, aging 8h；Wherein, the atom of different material
Number ratio is（Zn, Cu and Si sum）：Cetyl trimethylammonium bromide：Ammonia：Water=1: 0.05: 20：50, water therein is
Water in the cetyl trimethylammonium bromide aqueous solution；Aging is finished, filtering and washing, in 80 DEG C of dry 6 h, 300 DEG C of roasting 5h,
It is cooled to room temperature, obtains the photochemical catalyst of mesoporous silicon oxide MCM-48 loaded Cu nanometer doped zinc oxides.
Appreciation condition：In the 40 mg/L waste water from dyestuff containing methylene blue, the addition quality of catalyst is useless with dyestuff
The volume of water is calculated as 1.0 mg/mL, under the light source irradiation in the range of 420 ~ 600nm of wavelength, reaction is stirred at room temperature, photocatalysis is anti-
It is 2 hours between seasonable, Filtration of catalyst obtains degraded and removes the water body after methylene blue.
As a result show：The present embodiment mesoporous silicon oxide MCM-48 is the photocatalysis of carrier loaded Cu nanometer doped zinc oxides
Agent is 99.2% to the degradation rate of methylene blue.
Embodiment 2
After zinc carbonate and basic copper carbonate mechanical mixture, grind 60 minutes, the mol ratio of zinc salt and mantoquita is 400:1.
In air atmosphere, at 500 DEG C, it is calcined 1 hour.It is cooled to after room temperature, is washed with deionized 3 times, and 5 is dried at 150 DEG C
H, is made the nano-zinc oxide powder of doping Cu elements.
Above-mentioned gained powder is added in the aqueous solution of cetyl trimethylammonium bromide, 2 is stirred at 50 DEG C small
When；With the pH of concentrated ammonia liquor regulation system（12-13）, then add tetraethyl orthosilicate, aging 8h；Wherein, the atom of different material
Number ratio is（Zn, Cu and Si sum）：Cetyl trimethylammonium bromide：Ammonia：Water=1: 0.20: 40：100, water therein
For the water in the cetyl trimethylammonium bromide aqueous solution；Aging is finished, filtering and washing, in 150 DEG C of dry 12 h, 550 DEG C of roastings
10h is burnt, is cooled to after room temperature, obtains the photochemical catalyst of mesoporous silicon oxide MCM-48 loaded Cu nanometer doped zinc oxides.
Appreciation condition：In the 40 mg/L waste water from dyestuff containing methylene blue, the addition quality of catalyst is useless with dyestuff
The volume of water is calculated as 1.0 mg/mL, under the light source irradiation in the range of 500 ~ 700nm of wavelength, reaction is stirred at room temperature, photocatalysis is anti-
3 hours between seasonable, Filtration of catalyst obtains degraded and removes the water body after methylene blue.
As a result show：The mesoporous MCM-48 earth silicon materials of the present embodiment are the light of carrier loaded Cu nanometer doped zinc oxides
Catalyst is 99.4% to the degradation rate of methylene blue.
Embodiment 3
After acetic anhydride zinc and Salicylaldoxime mechanical mixture, grind 40 minutes, the mol ratio of zinc salt and mantoquita is 20:
1.In air atmosphere, at 400 DEG C, it is calcined 2 hours.It is cooled to after room temperature, is washed with deionized 3 times, and it is dry at 110 DEG C
Dry 3 h, is made the nano-zinc oxide powder of doping Cu elements.
Above-mentioned gained powder is added in the aqueous solution of cetyl trimethylammonium bromide, 3 is stirred at 30 DEG C small
When；With the pH of concentrated ammonia liquor regulation system（11-12）, then add tetraethyl orthosilicate, aging 8h；Wherein, the atom of different material
Number ratio is（Zn, Cu and Si sum）：Cetyl trimethylammonium bromide：Ammonia：Water=1: 0.15: 30：70, water therein is
Water in the cetyl trimethylammonium bromide aqueous solution；Aging is finished, filtering and washing, in 110 DEG C of dry 8 h, 500 DEG C of roastings
6h, is cooled to after room temperature, obtains the photochemical catalyst of mesoporous silicon oxide MCM-48 loaded Cu nanometer doped zinc oxides.
Appreciation condition：In the 40 mg/L waste water from dyestuff containing methylene blue, the addition quality of catalyst is useless with dyestuff
The volume of water is calculated as 1.0 mg/mL, under the light source irradiation in the range of 420 ~ 550nm of wavelength, reaction is stirred at room temperature, photocatalysis is anti-
3 hours between seasonable, Filtration of catalyst obtains degraded and removes the water body after methylene blue.
As a result show：The mesoporous MCM-48 earth silicon materials of the present embodiment are carrier, loaded Cu nanometer doped zinc oxide
Photochemical catalyst is 99.6% to the degradation rate of methylene blue.
Embodiment 4
After Zinc diacetate dihydrate and copper acetate monohydrate mechanical mixture, grind 40 minutes, the mol ratio of zinc salt and mantoquita
For 20: 1.In air atmosphere, at 400 DEG C, it is calcined 2 hours.It is cooled to after room temperature, is washed with deionized 3 times, and 110
DEG C dry 3 h, be made doping Cu elements nano-zinc oxide powder.
Above-mentioned gained powder is added in the aqueous solution of cetyl trimethylammonium bromide, 3 is stirred at 30 DEG C small
When, then with the pH of concentrated ammonia liquor regulation system（11-12）, then add tetraethyl orthosilicate, aging 8h；Wherein, different material
Atom number ratio is（Zn, Cu and Si sum）：Cetyl trimethylammonium bromide：Ammonia：Water=1: 0.15: 30：70, it is therein
Water is the water in the cetyl trimethylammonium bromide aqueous solution；Aging is finished, filtering and washing, in 110 DEG C of dry 8 h, 500 DEG C
6h is calcined, is cooled to after room temperature, obtains a kind of photochemical catalyst of mesoporous silicon oxide MCM-48 loaded Cu nanometer doped zinc oxides.
Appreciation condition：In the 40 mg/L waste water from dyestuff containing methylene blue, the addition quality of catalyst is useless with dyestuff
The volume of water is calculated as 1.0 mg/mL, under the light source irradiation in the range of 450 ~ 600nm of wavelength, reaction is stirred at room temperature, photocatalysis is anti-
3 hours between seasonable, Filtration of catalyst obtains degraded and removes the water body after methylene blue.
Regeneration condition：After light-catalyzed reaction terminates, with deionized water and ethanol, washing catalyst precipitation several times, will successively
Gained is deposited in 120 DEG C of dryings 2 hours.
As a result show：Using mesoporous MCM-48 earth silicon materials as the photochemical catalyst of carrier loaded Cu nanometer doped zinc oxides
Still there is extraordinary catalytic performance after reusing four times.Result of the test is：The catalyst is used for the first time, methylene blue
Degradation rate is 99.5%, the catalyst is reused for the first time, the degradation rate of methylene blue is 99.3%, and second of recycling should
Catalyst, the degradation rate of methylene blue is 99.2%, the catalyst is reused for the third time, the degradation rate of methylene blue is
99.0%, reuse the catalyst for the 4th time, the degradation rate of methylene blue is 98.8%.
Embodiment 5
After zinc carbonate and basic copper carbonate mechanical mixture, grind 60 minutes, the mol ratio of zinc salt and mantoquita is 400:1.
In air atmosphere, at 500 DEG C, it is calcined 1 hour.It is cooled to after room temperature, is washed with deionized 3 times, and 5 is dried at 150 DEG C
h.The nano-zinc oxide powder of doping Cu elements is made.By above-mentioned gained powder, cetyl trimethylammonium bromide is added to
In the aqueous solution, stirred 2 hours at 50 DEG C；With the pH of concentrated ammonia liquor regulation system（12-13）, tetraethyl orthosilicate is then added, always
Change 8h；The atom number ratio of wherein different material is（Zn, Cu and Si sum）：Cetyl trimethylammonium bromide：Ammonia：Water=1:
0.20: 40：100, water therein is the water in the cetyl trimethylammonium bromide aqueous solution；Aging is finished, filtering and washing,
150 DEG C of dryings 12 h, 550 DEG C of roasting 10h, are cooled to after room temperature, obtain mesoporous silicon oxide MCM-48 loaded Cu dopen Nanos
The photochemical catalyst of zinc oxide.
Appreciation condition：In the 40 mg/L waste water from dyestuff containing rhodamine B, the addition quality of catalyst is with waste water from dyestuff
Volume be calculated as 1.0 mg/mL, under the irradiation of light source in the range of 420 ~ 600nm of wavelength, reaction, light-catalyzed reaction is stirred at room temperature
3 hours time, Filtration of catalyst obtains degraded and removes the water body after rhodamine B.
As a result show：Using the mesoporous MCM-48 earth silicon materials of the present embodiment as carrier, loaded Cu nanometer doped zinc oxide
Photochemical catalyst be 80.6% to the degradation rate of rhodamine B.
Claims (8)
1. the photochemical catalyst of dyestuff in a kind of degrading waste water, it is characterised in that：Using mesoporous silicon oxide as carrier, described mesoporous two
The nano zine oxide of doping copper is loaded with silica support；The preparation side of the photochemical catalyst of dyestuff in the degrading waste water
Method, including step：
1）Ground after the corresponding zinc salt of volatile acid and mantoquita are mixed, in air atmosphere, be calcined 1-5 in 300-600 DEG C small
When；
2）Room temperature is cooled to, then deionized water washing dries 1-10h, the nano-zinc oxide powder for the copper that must adulterate；
3）The nano-zinc oxide powder for the copper that adulterates is dispersed in the aqueous solution of cetyl trimethylammonium bromide,
1-6h is stirred at 20-50 DEG C；
4）PH to 9-13 is adjusted using concentrated ammonia liquor, the silicon source of mesoporous silicon oxide, aging 6-30h is added；
5）2-15h is dried in suction filtration, washing at 40-200 DEG C；
6）In being calcined 3-15h at 300-600 DEG C, room temperature is cooled to, the photochemical catalyst of dyestuff in degrading waste water is obtained；
Step 1）In, the corresponding zinc salt of volatile acid is zinc acetate, the crystalline hydrate of zinc acetate, zinc nitrate, the knot of zinc nitrate
Brilliant hydrate, zinc carbonate；The corresponding mantoquita of volatile acid is copper acetate, the crystalline hydrate of copper acetate, copper nitrate, copper nitrate
Crystalline hydrate.
2. the photochemical catalyst of dyestuff in degrading waste water as claimed in claim 1, it is characterised in that：The mass fraction of Zn-ef ficiency is 5-
40%, the mass fraction of copper is 0.1-5%.
3. the photochemical catalyst of dyestuff in degrading waste water as claimed in claim 1, it is characterised in that：Step 1）In, zinc salt and mantoquita
Mol ratio be 1:1-400:1.
4. the photochemical catalyst of dyestuff in degrading waste water as claimed in claim 3, it is characterised in that：Cetyl trimethylammonium bromide
Molal quantity be Zn-ef ficiency, copper and element silicon molal quantity summation 5%-20%.
5. the photochemical catalyst of dyestuff in degrading waste water as claimed in claim 1, it is characterised in that：Step 3）Cetyl trimethyl
The mass fraction of cetyl trimethylammonium bromide is 1%-90% in the aqueous solution of ammonium bromide.
6. the photochemical catalyst of dyestuff in degrading waste water as claimed in claim 1, it is characterised in that：Step 4）Intermediary hole silica
Silicon source be tetraethyl orthosilicate, Ludox, white carbon in one or more.
7. the photochemical catalyst of dyestuff is in degrading waste water Methylene Blue and rhodamine B in degrading waste water as claimed in claim 1
Application.
8. photocatalyst for degrading methylene blue in waste and rhodamine B using dyestuff in degrading waste water described in claim 1
Method, it is characterised in that：The light of dyestuff in the degrading waste water is added into the waste water containing methylene blue and/or rhodamine B
Catalyst, in wavelength under 420-800nm light source irradiation, stirring reaction 0.2-6h filters out catalyst.
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| CN106477706A (en) * | 2016-12-14 | 2017-03-08 | 盐城工学院 | Method and the processing method of waste water from dyestuff that a kind of methylenum careuleum is faded |
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| CN110404521B (en) * | 2019-07-31 | 2022-01-28 | 西北大学 | Adsorbent for selectively adsorbing methylene blue and preparation method and application thereof |
| CN111420652B (en) * | 2020-04-22 | 2023-07-18 | 安徽锦华氧化锌有限公司 | Application of active zinc oxide in promotion of azo dye wastewater degradation |
| CN111871417B (en) * | 2020-08-24 | 2022-11-01 | 广州大学 | Mesoporous nanorod catalyst and preparation method and application thereof |
| CN113101965A (en) * | 2021-04-16 | 2021-07-13 | 滨州学院 | Light alkane isomerization catalyst loaded with molybdenum nitride, preparation method and application |
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