CN111036190A - Preparation method of carbon-doped modified zinc oxide visible-light-driven photocatalyst - Google Patents
Preparation method of carbon-doped modified zinc oxide visible-light-driven photocatalyst Download PDFInfo
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- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000725 suspension Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 27
- 239000004065 semiconductor Substances 0.000 abstract description 16
- 239000011787 zinc oxide Substances 0.000 abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 6
- 229940012189 methyl orange Drugs 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000000975 dye Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
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- 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
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- 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
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- 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
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Abstract
The invention discloses a preparation method of a carbon-doped modified zinc oxide visible-light-driven photocatalyst, belonging to the technical field of preparation and application of nano materials. The method can realize artificial introduction of surface defects by doping the non-metallic element carbon into the zinc oxide semiconductor. The band gap of the zinc oxide semiconductor is narrowed due to the introduction of carbon doping and surface defects, so that the light absorption range of the zinc oxide is expanded to a visible light region, and the utilization rate of the zinc oxide semiconductor to the visible light is further improved. The carbon source used in the method is polyvinylpyrrolidone, and the method is simple, environment-friendly and high in catalytic efficiency. The performance of the catalyst for photocatalytic degradation of the dye is evaluated by adopting the ratio of the methyl orange concentration reduction value to the initial concentration in unit time, and the carbon-doped modified zinc oxide visible-light-driven photocatalyst has potential application value in the aspect of degrading the dye under the visible light condition.
Description
Technical Field
The invention belongs to the field of preparation and application of nano materials, and particularly relates to a preparation method of a carbon-doped modified zinc oxide visible-light-driven photocatalyst (C-ZnO).
Background
Among various metal oxide semiconductors used in photocatalysis, zinc oxide (ZnO), an n-type semiconductor, has been drawing attention from many researchers because of its advantages such as non-toxicity, high chemical stability, low cost, and no secondary pollution to the environment. However, ZnO semiconductor materials also have some disadvantages, such as: the preparation process is relatively complex, the yield is not high, required instruments and equipment are expensive, the ZnO semiconductor material is easy to generate rapid recombination of photo-generated electron-hole pairs, and the ZnO semiconductor only has light absorption in an ultraviolet region but hardly has light absorption in a visible region, so the adverse factors limit the application and industrialization of the pure ZnO semiconductor material in the field of photocatalysis. Researchers have tried many methods to overcome these disadvantages, such as doping metals or non-metallic elements to create surface defects, coupling with other semiconductors or metals, etc.
The defects in the semiconductor photocatalytic material can be realized by some experimental methods, such as doping, pressurizing, constructing a Z-type photocatalytic system and the like. According to investigation, the non-metal such as carbon, boron, sulfur and nitrogen is doped into the semiconductor to reduce the electron-hole recombination rate, so as to improve the photocatalytic activity, and especially carbon doping has received great attention to improve the photocatalytic activity of the semiconductor and enhance the stability of the semiconductor catalyst under the irradiation of visible light.
The invention develops a simple and convenient route to prepare the carbon-doped modified ZnO visible-light-driven photocatalyst, takes methyl orange as a target degradation product of the dye, and researches the performance of the carbon-doped modified ZnO visible-light-driven degradation dye.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a novel preparation method of a carbon-doped modified zinc oxide visible-light-driven photocatalyst, which is simple and feasible, high in yield and high in visible-light-driven catalysis efficiency.
The purpose of the invention is realized as follows: a preparation method of a carbon-doped modified zinc oxide visible-light-driven photocatalyst comprises the following steps:
(1) 17.56g of zinc acetate dihydrate (Zn (CH) was weighed out3COO)2·2H2O) solid, adding Zn (CH)3COO)2·2H2Adding O into 80mL of deionized water, stirring for 30min at room temperature at the rotating speed of 600rpm, and completely dissolving to form a solution A;
(2) weighing 0.2g of polyvinylpyrrolidone (PVP for short, M.W.1300000) solid, adding PVP into the solution A, stirring for 1h at 65 ℃ and the rotating speed of 600rpm, and dispersing to form suspension B;
(3) weighing 1.0g of sodium hydroxide (NaOH) solid, adding NaOH into 25mL of deionized water, stirring at room temperature at the rotating speed of 500rpm, and completely dissolving to form a colorless transparent solution D;
(4) dropwise adding the solution D into the suspension B at a speed of 30D/min to form a suspension E, then moving the suspension E into a high-pressure reaction kettle, then placing the high-pressure reaction kettle into an oven to react for 7 hours at 100 ℃, naturally cooling to room temperature and then carrying out centrifugal treatment, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, removing supernatant, cleaning precipitates with deionized water, then carrying out two-time centrifugal and water washing treatment processes again, the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, then cleaning the precipitates with absolute ethyl alcohol and carrying out centrifugal treatment for three times, the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, drying the centrifuged precipitates in the oven at 60 ℃ for 12 hours to obtain the carbon-doped modified zinc oxide precursor.
(5) And (3) putting the precursor of the carbon-doped modified zinc oxide obtained in the step (4) into a muffle furnace for high-temperature calcination treatment, heating to 400 ℃ at the speed of 5 ℃/min, preserving the temperature for 4 hours, and naturally cooling to room temperature to obtain the carbon-doped modified zinc oxide visible-light-driven photocatalyst (C-ZnO).
The invention has the following advantages and positive effects:
1. the photocatalyst synthesized by the method has high purity and good chemical stability, enhances the absorption of the C-ZnO to visible light, and has higher photocatalytic activity under the irradiation of the visible light.
2. The process method is environment-friendly, low in cost, wide in raw material source, simple in method and easy to operate; the catalyst has very wide application prospect in degrading dyes under visible light conditions.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a carbon-doped modified zinc oxide visible light catalyst (C-ZnO) according to the present invention;
FIG. 2 is a graph of solid ultraviolet-visible diffuse reflectance (UV-vis DRS) of C-ZnO of the present invention;
FIG. 3 is a graphical representation of the photocatalytic degradation of methyl orange by C-ZnO in accordance with the present invention.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
A preparation method of a carbon-doped modified zinc oxide visible-light-driven photocatalyst comprises the following steps:
(1) 17.56g of zinc acetate dihydrate (Zn (CH) was weighed out3COO)2·2H2O) solid, adding Zn (CH)3COO)2·2H2Adding O into 80mL of deionized water, stirring for 30min at room temperature at the rotating speed of 600rpm, and completely dissolving to form a solution A;
(2) weighing 0.2g of polyvinylpyrrolidone (PVP for short, M.W.1300000) solid, adding PVP into the solution A, stirring for 1h at 65 ℃ and the rotating speed of 600rpm, and dispersing to form suspension B;
(3) weighing 1.0g of sodium hydroxide (NaOH) solid, adding NaOH into 25mL of deionized water, stirring at room temperature at the rotating speed of 500rpm, and completely dissolving to form a colorless transparent solution D;
(4) dropwise adding the solution D into the suspension B at a speed of 30D/min to form a suspension E, then moving the suspension E into a high-pressure reaction kettle, then placing the high-pressure reaction kettle into an oven to react for 7 hours at 100 ℃, naturally cooling to room temperature and then carrying out centrifugal treatment, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, removing supernatant, cleaning precipitates with deionized water, then carrying out two-time centrifugal and water washing treatment processes again, the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, then cleaning the precipitates with absolute ethyl alcohol and carrying out centrifugal treatment for three times, the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, drying the centrifuged precipitates in the oven at 60 ℃ for 12 hours to obtain the carbon-doped modified zinc oxide precursor.
(5) And (3) putting the precursor of the carbon-doped modified zinc oxide obtained in the step (4) into a muffle furnace for high-temperature calcination treatment, heating to 400 ℃ at the speed of 5 ℃/min, preserving the temperature for 4 hours, and naturally cooling to room temperature to obtain the carbon-doped modified zinc oxide visible-light-driven photocatalyst (C-ZnO).
The reagent dosage in the above steps can be scaled up proportionally.
The reagents in the above steps are all analytically pure and are not further processed.
The carbon-doped modified zinc oxide visible-light-induced photocatalyst prepared by the method is characterized by X-ray diffraction (XRD) and solid ultraviolet-visible diffuse reflection (UV-vis DRS):
from the XRD diffraction image of FIG. 1, it can be seen that all diffraction peaks of C-ZnO correspond to ZnO semiconductor standard card (JCPDS card No.36-1451), no diffraction peak of carbon is observed, and the diffraction peak of the carbon-doped modified zinc oxide visible light photocatalyst is found to shift towards a small angle, which indicates that the nonmetal carbon is successfully doped into the ZnO semiconductor and no other impurity peak appears, which indicates that the C-ZnO photocatalyst prepared by the method of the present invention has very high purity;
as can be seen from the UV-vis DRS plot of FIG. 2, C-ZnO has significant absorption in the visible region compared to pure ZnO.
FIG. 3 is a graphical representation of the photocatalytic degradation of methyl orange by C-ZnO, and it can be seen from the graph that ZnO has almost no activity to methyl orange after 75min of visible light irradiation, while methyl orange is almost completely degraded in a reaction system with C-ZnO as a catalyst, which indicates that the C-ZnO catalyst has potential application value in the field of dye degradation under the condition of visible light irradiation.
Claims (1)
1. A preparation method of a carbon-doped modified zinc oxide visible-light-driven photocatalyst comprises the following steps:
(1) 17.56g of zinc acetate dihydrate (Zn (CH) was weighed out3COO)2·2H2O) solid, adding Zn (CH)3COO)2·2H2Adding O into 80mL of deionized water, stirring for 30min at room temperature at the rotating speed of 600rpm, and completely dissolving to form a solution A;
(2) weighing 0.2g of polyvinylpyrrolidone (PVP for short, M.W.1300000) solid, adding PVP into the solution A, stirring for 1h at 65 ℃ and the rotating speed of 600rpm, and dispersing to form suspension B;
(3) weighing 1.0g of sodium hydroxide (NaOH) solid, adding NaOH into 25mL of deionized water, stirring at room temperature at the rotating speed of 500rpm, and completely dissolving to form a colorless transparent solution D;
(4) dropwise adding the solution D into the suspension B at a speed of 30D/min to form a suspension E, then moving the suspension E into a high-pressure reaction kettle, then placing the high-pressure reaction kettle into an oven to react for 7 hours at 100 ℃, naturally cooling to room temperature and then carrying out centrifugal treatment, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, discarding supernatant, cleaning precipitates with deionized water and then carrying out two-time centrifugal and water washing treatment processes again, the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, then cleaning the precipitates with absolute ethyl alcohol and carrying out centrifugal treatment for three times, the centrifugal rotation speed is 5000rpm, the centrifugal time is 6 minutes, drying the centrifuged precipitates in the oven at 60 ℃ for 12 hours to obtain a carbon-doped modified zinc oxide precursor;
(5) and (3) putting the precursor of the carbon-doped modified zinc oxide obtained in the step (4) into a muffle furnace for high-temperature calcination treatment, heating to 400 ℃ at the speed of 5 ℃/min, preserving the temperature for 4 hours, and naturally cooling to room temperature to obtain the carbon-doped modified zinc oxide visible-light-driven photocatalyst (C-ZnO).
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2019
- 2019-12-18 CN CN201911308993.8A patent/CN111036190A/en active Pending
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Application publication date: 20200421 |