CN113398930A - Nano iron oxide photocatalyst and preparation method thereof - Google Patents
Nano iron oxide photocatalyst and preparation method thereof Download PDFInfo
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- CN113398930A CN113398930A CN202110585533.0A CN202110585533A CN113398930A CN 113398930 A CN113398930 A CN 113398930A CN 202110585533 A CN202110585533 A CN 202110585533A CN 113398930 A CN113398930 A CN 113398930A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 9
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 47
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 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 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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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
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a nano iron oxide photocatalyst and a preparation method thereof, wherein the preparation method comprises the following steps: A. putting 20-30 parts of ferric chloride and 1-2 parts of titanium dioxide into a hydrochloric acid solution, heating and stirring to prepare a precursor; B. putting the precursor into a reaction kettle, heating to 200-210 ℃, and preserving heat for 2-3 hours; C. adding pure water with the temperature of 80-90 ℃ into the product in the reaction kettle, and stirring for crystallization; D. c, carrying out suction filtration and washing on the product obtained in the step C; E. putting the product obtained in the step D into a muffle furnace, and heating to 850-950 ℃ for calcining; F. reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the temperature of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, then increasing the temperature of the muffle furnace to 500 ℃, preserving the temperature for 3 h, then taking out the product in the muffle furnace, putting in pure water and cooling to the room temperature. The invention can improve the defects of the prior art and reduce the reduction speed of the activity of the iron oxide photocatalyst.
Description
Technical Field
The invention relates to the technical field of photocatalyst preparation, in particular to a nano iron oxide photocatalyst and a preparation method thereof.
Background
The photocatalytic effect of semiconductors is widely applied to the field of sewage treatment. The band gap energy of the iron oxide is 2.2eV, the maximum absorption wavelength is 560nm, and the iron oxide shows better photoelectrochemical response to ultraviolet light and visible light. However, the photocatalytic activity of iron oxide decreases significantly with increasing use time.
Disclosure of Invention
The invention aims to solve the technical problem of providing a nano iron oxide photocatalyst and a preparation method thereof, which can solve the defects of the prior art and reduce the reduction rate of the activity of the iron oxide photocatalyst.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A preparation method of a nano iron oxide photocatalyst comprises the following steps:
the following parts are all parts by mole,
A. putting 20-30 parts of ferric chloride and 1-2 parts of titanium dioxide into a 10 wt% hydrochloric acid solution, heating to 55-60 ℃, and fully stirring to obtain a precursor;
B. putting the precursor into a reaction kettle, heating to 200-210 ℃, and preserving heat for 2-3 hours;
C. adding pure water with the temperature of 80-90 ℃ into the product in the reaction kettle, stirring and crystallizing for 30-35 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. putting the product obtained in the step D into a muffle furnace, heating to 850-950 ℃, and calcining for 6-8 hours;
F. reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the heat of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, then increasing the temperature of the muffle furnace to 500 ℃, preserving the heat for 3 h, then taking out a product in the muffle furnace, putting pure water into the product, cooling the product to room temperature, and drying the product to obtain a finished product.
Preferably, in step a, 23 parts of ferric chloride and 1 part of titanium dioxide are placed in a 10 wt% hydrochloric acid solution, heated to 60 ℃, and then sufficiently stirred to prepare a precursor.
Preferably, in the step A, ultrasonic oscillation is performed while stirring, and the power density of ultrasonic wave is 0.5 to 0.7W/cm2。
Preferably, in the step B, the precursor is put into a reaction kettle to be heated to 210 ℃, and the temperature is kept for 3 hours.
Preferably, in step C, the product in the reaction kettle is added with pure water at 85 ℃ and stirred for crystallization for 30 hours.
Preferably, in step E, the product of step D is placed in a muffle furnace and heated to 935 ℃ for calcination for 8 hours.
A nanometer ferric oxide photocatalyst is prepared by the preparation method of the nanometer ferric oxide photocatalyst.
Adopt the beneficial effect that above-mentioned technical scheme brought to lie in: the invention optimizes the doping and calcining process of the photocatalyst, so that the product has excellent spectral absorption performance and uniform mesoporous structure. Thereby effectively prolonging the service life of the product.
Drawings
FIG. 1 shows XRD patterns of the precursor (a) and the calcined nano-iron oxide powder (b) obtained in example 1.
FIG. 2 is an SEM photograph of the precursor prepared in example 1.
FIG. 3 is an SEM photograph of the nano-iron oxide powder prepared in example 1.
FIG. 4 is a Fourier infrared transform spectrum of the nano-iron oxide powder prepared in example 1.
FIG. 5 is a nitrogen adsorption-desorption isotherm of the nano-iron oxide powder prepared in example 1.
FIG. 6 is a distribution diagram of the pore diameters of the nano-sized iron oxide powder prepared in example 1.
FIG. 7 is a graph showing the degradation rate trend of methyl orange degraded by the nano-iron oxide powder prepared in example 1.
Detailed Description
Example 1
A preparation method of a nano iron oxide photocatalyst comprises the following steps:
the following parts are all parts by mole,
A. putting 23 parts of ferric chloride and 1 part of titanium dioxide into 10 wt% hydrochloric acid solution, heating to 60 ℃, and fully stirring to obtain a precursor; ultrasonic vibration while stirringThe power density of the ultrasonic wave is 0.5-0.7W/cm2；
B. Putting the precursor into a reaction kettle, heating to 210 ℃, and preserving heat for 3 hours;
C. adding pure water with the temperature of 85 ℃ into the product in the reaction kettle, stirring and crystallizing for 30 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. d, placing the product obtained in the step D into a muffle furnace, heating to 935 ℃ and calcining for 8 hours;
F. reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the heat of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, then increasing the temperature of the muffle furnace to 500 ℃, preserving the heat for 3 h, then taking out a product in the muffle furnace, putting pure water into the product, cooling the product to room temperature, and drying the product to obtain a finished product.
The XRD pattern of a in figure 1 shows that the precursor is amorphous; the precursor is calcined to obtain a final product, a corresponding XRD pattern is shown as b in figure 1, the XRD patterns of the obtained samples are identical to the standard pattern of JCPDS card (NO.33-0664), and the peaks are sharp, sharp and narrow, which indicates that the prepared product has high crystallinity and complete crystallization. Meanwhile, no other substance phase exists on the diffraction pattern, which indicates that the purity of the sample is high. Further, it can be calculated from the Scherrer formula D ═ k · λ/(β · cos θ), and the average crystal grain size is 30.8nm, indicating that the prepared sample is in the nanometer level. As can be seen from fig. 2 and 3, the prepared nano iron oxide powder is flaky and is more uniformly dispersed than the precursor. As can be seen from fig. 5, the prepared nano iron oxide powder has an IV-type isotherm of H3 hysteresis loop, indicating that the sample has a mesoporous structure. The test results also showed that the specific surface area of the sample was 19.2m2Per g, pore volume of 0.122cm3The most probable pore diameter of the sample is 3.2nm, belonging to the mesoporous range. As can be seen from fig. 7, the prepared nano iron oxide powder has a better photocatalytic degradation effect on methyl orange, and the degradation rate of methyl orange can reach 62.9% within the measured time range of 4 h.
Comparative example 1
A preparation method of a nano iron oxide photocatalyst comprises the following steps:
the following parts are all parts by mole,
A. putting 23 parts of ferric chloride into 10 wt% hydrochloric acid solution, heating to 60 ℃, and fully stirring to obtain a precursor; ultrasonic oscillation is carried out while stirring, and the power density of ultrasonic waves is 0.5-0.7W/cm2；
B. Putting the precursor into a reaction kettle, heating to 210 ℃, and preserving heat for 3 hours;
C. adding pure water with the temperature of 85 ℃ into the product in the reaction kettle, stirring and crystallizing for 30 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. d, placing the product obtained in the step D into a muffle furnace, heating to 935 ℃ and calcining for 8 hours;
F. reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the heat of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, then increasing the temperature of the muffle furnace to 500 ℃, preserving the heat for 3 h, then taking out a product in the muffle furnace, putting pure water into the product, cooling the product to room temperature, and drying the product to obtain a finished product.
Comparative example 2
A preparation method of a nano iron oxide photocatalyst comprises the following steps:
the following parts are all parts by mole,
A. putting 23 parts of ferric chloride and 1 part of titanium dioxide into 10 wt% hydrochloric acid solution, heating to 60 ℃, and fully stirring to obtain a precursor; ultrasonic oscillation is carried out while stirring, and the power density of ultrasonic waves is 0.5-0.7W/cm2；
B. Putting the precursor into a reaction kettle, heating to 210 ℃, and preserving heat for 3 hours;
C. adding pure water with the temperature of 85 ℃ into the product in the reaction kettle, stirring and crystallizing for 30 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. d, placing the product obtained in the step D into a muffle furnace, heating to 935 ℃ and calcining for 8 hours;
F. and reducing the temperature of the muffle furnace to room temperature at the speed of 150 ℃/hour to obtain a finished product.
Comparative example 3
A preparation method of a nano iron oxide photocatalyst comprises the following steps:
the following parts are all parts by mole,
A. putting 23 parts of ferric chloride and 1 part of titanium dioxide into 10 wt% hydrochloric acid solution, heating to 60 ℃, and fully stirring to obtain a precursor; ultrasonic oscillation is carried out while stirring, and the power density of ultrasonic waves is 0.5-0.7W/cm2；
B. Putting the precursor into a reaction kettle, heating to 210 ℃, and preserving heat for 3 hours;
C. adding pure water with the temperature of 85 ℃ into the product in the reaction kettle, stirring and crystallizing for 30 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. d, placing the product obtained in the step D into a muffle furnace, heating to 935 ℃ and calcining for 8 hours;
F. and reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the heat of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, taking out a product in the muffle furnace, putting pure water into the product, cooling the product to room temperature, and drying the product to obtain a finished product.
Comparative example 4
A preparation method of a nano iron oxide photocatalyst comprises the following steps:
the following parts are all parts by mole,
A. putting 23 parts of ferric chloride and 1 part of titanium dioxide into 10 wt% hydrochloric acid solution, heating to 60 ℃, and fully stirring to obtain a precursor; ultrasonic oscillation is carried out while stirring, and the power density of ultrasonic waves is 0.5-0.7W/cm2；
B. Putting the precursor into a reaction kettle, heating to 210 ℃, and preserving heat for 3 hours;
C. adding pure water with the temperature of 85 ℃ into the product in the reaction kettle, stirring and crystallizing for 30 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. d, placing the product obtained in the step D into a muffle furnace, heating to 935 ℃ and calcining for 8 hours;
F. reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the heat of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, then increasing the temperature of the muffle furnace to 500 ℃, preserving the heat for 3 h, then taking out a product in the muffle furnace, and naturally cooling to room temperature to obtain a finished product.
The products prepared in the examples 1 and 4 compared examples are subjected to cyclic multiple degradation experiments on methyl orange under the same parameter environment, and the degradation rate decline condition is shown in the following table.
| Group of | First degradation rate | Tenth degradation rate | Thirty-th degradation rate |
| Example 1 | 62.9％ | 57.2％ | 47.6％ |
| Comparative example 1 | 50.3％ | 42.1％ | 25.5％ |
| Comparative example 2 | 51.1％ | 40.6％ | 28.4％ |
| Comparative example 3 | 50.6％ | 44.1％ | 33.2％ |
| Comparative example 4 | 55.7％ | 49.2％ | 38.2％ |
Therefore, the photocatalyst prepared in the embodiment 1 of the invention has slow activity decay and longer service life.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A preparation method of a nano iron oxide photocatalyst is characterized by comprising the following steps:
the following parts are all parts by mole,
A. putting 20-30 parts of ferric chloride and 1-2 parts of titanium dioxide into a 10 wt% hydrochloric acid solution, heating to 55-60 ℃, and fully stirring to obtain a precursor;
B. putting the precursor into a reaction kettle, heating to 200-210 ℃, and preserving heat for 2-3 hours;
C. adding pure water with the temperature of 80-90 ℃ into the product in the reaction kettle, stirring and crystallizing for 30-35 hours;
D. c, carrying out suction filtration and washing on the product obtained in the step C;
E. putting the product obtained in the step D into a muffle furnace, heating to 850-950 ℃, and calcining for 6-8 hours;
F. reducing the temperature of the muffle furnace at the speed of 150 ℃/h, preserving the heat of the muffle furnace for 1 h when the temperature of the muffle furnace is reduced to 350 ℃, then increasing the temperature of the muffle furnace to 500 ℃, preserving the heat for 3 h, then taking out a product in the muffle furnace, putting pure water into the product, cooling the product to room temperature, and drying the product to obtain a finished product.
2. The method for preparing a nano iron oxide photocatalyst according to claim 1, characterized in that: in the step A, 23 parts of ferric chloride and 1 part of titanium dioxide are put into 10 wt% hydrochloric acid solution, heated to 60 ℃, and fully stirred to prepare a precursor.
3. The method for preparing a nano iron oxide photocatalyst according to claim 2, characterized in that: in the step A, ultrasonic oscillation is carried out while stirring, and the power density of ultrasonic is 0.5-0.7W/cm2。
4. The method for preparing a nano iron oxide photocatalyst according to claim 3, characterized in that: and step B, putting the precursor into a reaction kettle, heating to 210 ℃, and preserving heat for 3 hours.
5. The method for preparing a nano iron oxide photocatalyst according to claim 4, characterized in that: and step C, adding the product in the reaction kettle into pure water at 85 ℃, and stirring and crystallizing for 30 hours.
6. The method for preparing a nano iron oxide photocatalyst according to claim 5, characterized in that: and step E, putting the product obtained in the step D into a muffle furnace, heating to 935 ℃ and calcining for 8 hours.
7. A nano iron oxide photocatalyst, characterized by being prepared by the method for preparing a nano iron oxide photocatalyst according to any one of claims 1 to 6.
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Citations (6)
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|---|---|---|---|---|
| US20090318285A1 (en) * | 2006-11-08 | 2009-12-24 | Claudia Menini | Iron oxide containing precipitated crystalline titanium dioxide and process for the manufacture thereof |
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| CN111364050A (en) * | 2020-03-11 | 2020-07-03 | 华侨大学 | Preparation method of titanium-doped iron oxide photo-anode with high photoelectric water decomposition performance |
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2021
- 2021-05-27 CN CN202110585533.0A patent/CN113398930A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090318285A1 (en) * | 2006-11-08 | 2009-12-24 | Claudia Menini | Iron oxide containing precipitated crystalline titanium dioxide and process for the manufacture thereof |
| CN103537285A (en) * | 2013-08-12 | 2014-01-29 | 江苏大学 | Preparation of three-dimensional ordered macroporous iron/titanium composite oxide by template hydrothermal method and application thereof |
| CN106423169A (en) * | 2016-10-13 | 2017-02-22 | 辽宁大学 | Mesoporous Ti-Fe2O3 photocatalyst and preparation method and application thereof |
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| CN111364050A (en) * | 2020-03-11 | 2020-07-03 | 华侨大学 | Preparation method of titanium-doped iron oxide photo-anode with high photoelectric water decomposition performance |
Non-Patent Citations (1)
| Title |
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| TING WANG ET AL.: "Orthogonal synthesis, structural characteristics, and enhanced visible-light photocatalysis of mesoporous Fe2O3/TiO2 heterostructured microspheres", 《APPLIED SURFACE SCIENCE》 * |
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Application publication date: 20210917 |