CN110694627A - Ferric oxide nano-ring photocatalyst and preparation method thereof - Google Patents
Ferric oxide nano-ring photocatalyst and preparation method thereof Download PDFInfo
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- 239000002063 nanoring Substances 0.000 title claims abstract description 37
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000002608 ionic liquid Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 11
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 9
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 239000000985 reactive dye Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 239000000975 dye Substances 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 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 3
- 229940012189 methyl orange Drugs 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 230000001699 photocatalysis Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 4
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
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- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
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- 239000000203 mixture Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000001044 red dye Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- INOIOAWTVPHTCJ-UHFFFAOYSA-N 6-acetamido-4-hydroxy-3-[[4-(2-sulfooxyethylsulfonyl)phenyl]diazenyl]naphthalene-2-sulfonic acid Chemical compound CC(=O)NC1=CC=C2C=C(C(N=NC3=CC=C(C=C3)S(=O)(=O)CCOS(O)(=O)=O)=C(O)C2=C1)S(O)(=O)=O INOIOAWTVPHTCJ-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 235000019441 ethanol Nutrition 0.000 description 1
- 238000013210 evaluation model Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/60—
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
Abstract
The application provides a ferric oxide nano-ring photocatalyst and a preparation method thereof, belonging to the technical field of nano-structure manufacturing or processing for material and surface science. Fe2O3The nano-ring photocatalyst is powder, the crystalline phase is a hexagonal structure and a rhombohedral crystal system, the appearance is a nano-ring structure, the outer diameter of the particle is 400nm, the wall thickness is 120nm, and the thickness of the ring is 150 nm. The photocatalyst is applied to dye degradation, and has the advantages of simple preparation, good dispersibility, great improvement on the degradation efficiency of industrial dye methyl orange and various reactive dyes, and the like.
Description
Technical Field
The application relates to a ferric oxide nano-ring photocatalyst and a preparation method thereof, belonging to the technical field of nano-structure manufacturing or processing for material and surface science.
Background
With the introduction of photocatalytic degradation of organic pollutants in the 70 s of the 20 th century, semiconductor photocatalysts received extensive attention of researchers in various countries. Among the numerous semiconductor photocatalysts, TiO2The nano semiconductor photocatalytic material is the most widely researched nano semiconductor photocatalytic material due to the advantages of safety, no toxicity, simple and easy synthesis method, high photocatalytic efficiency and the like. However, TiO2The photocatalytic reaction needs ultraviolet light as an excitation light source, the ultraviolet light with the wavelength of below 400nm only accounts for 3-5 percent of the total energy of sunlight, and pure TiO is used2The photoproduction electron holes generated under the excitation of light are easy to recombine, which limits TiO2The application in the field of photocatalysis.
In the solar spectrum, the visible light accounts for about 43%, so that the research and development of the high-activity and visible-light-responsive narrow-bandgap semiconductor photocatalyst has important practical significance. Fe2O3As a common n-type semiconductor material, the photocatalyst has the advantages of magnetism, proper forbidden band width (1.9eV-2.2eV), and the like, is rich in source, non-toxic, high in stability and low in cost, and therefore, the photocatalyst is used as the photocatalyst and contributes to the recovery of the catalyst and the improvement of the catalytic activity. Fe2O3The composition, morphology, size, specific surface area, and exposed crystal face activity of the nanomaterial can affect its physical and chemical properties. Therefore, to increase Fe2O3Application of nano material in photocatalysis field, and preparation of Fe with high specific surface area and high activity2O3The nano material has important application value. Zhang et al use UiO-66 with different pore sizes as template to promote alpha-Fe2O3Nano particle limited growth and synthesis of alpha-Fe2O3The results of the nano-cluster and photocatalysis experiments show that due to the confinement effect, UiO-66 and alpha-Fe2O3Promote the alpha-Fe by the synergistic effect between2O3The nanoclusters can degrade methylene blue by visible light (R.Zhang, et al. applied Surface Science,2019,466, 956-963.). Yan et al synthesized a large amount of single crystal alpha-Fe by simple and direct solvothermal method2O3The nano-rod, 1, 2-propane diamine can effectively regulate the appearance of the product, alpha-Fe2O3The nanorods have rough edges and edges, narrow forbidden bandwidth and high photocurrent response, so that the nanorods have high visible light catalytic activity and potential application value in the field of environmental management (X.Yan, et al. journal of Materials Science,2018,53(23), 15850-15858.). Y.Dong et al successfully synthesized striped alpha-Fe by solvothermal method without template agent2O3Nano-structureThe photocatalysis experiment result shows that the Congo red dye can be completely degraded by visible light irradiation for 24min, the degradation rate exceeds 99 percent, and the Congo red dye has potential application in the aspect of treating organic pollutants in sewage (Y.Dong, et al.vacuum,2018,150, 35-40.).
Disclosure of Invention
In view of the above, the present application provides an iron (Fe) oxide2O3) Nanometer ring photocatalyst, using ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM]The Cl regulates and controls the appearance of the product, and the nano annular Fe is finally synthesized in an ethanol solvent by utilizing the special high-temperature and high-pressure condition generated by a high-pressure kettle2O3The method has the characteristics of simplicity, easiness in operation, high yield, uniform appearance, porous hollow structure, good dispersibility and the like, so that the method has potential application value in the field of visible light catalysis.
The application provides a Fe2O3Nano-ring photocatalyst of said Fe2O3The nano-ring photocatalyst is powder, the crystalline phase is a hexagonal structure and a rhombohedral system, the appearance is a nano-ring structure, the outer diameter of the particle is about 400nm, the wall thickness is about 120nm, and the thickness of the ring is about 150 nm. The morphology and structure of the target product can be obtained by characterization with an X-ray diffractometer (XRD, Empyrean, Dutch Pasnake), a scanning electron microscope (SEM, JSM-6360LV, Japanese electron, acceleration voltage of 20kV) and a transmission electron microscope (TEM, JEM-1011, Japanese electron, acceleration voltage of 80 kV).
Fe having the above characteristics2O3The preparation method of the nano-ring photocatalyst comprises the following steps:
(1) dispersing ferric trichloride hexahydrate in absolute ethyl alcohol to obtain a clear solution;
(2) slowly adding ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM ] Cl into the clarified solution obtained in the step (1), violently stirring until the ionic liquid is fully dispersed, adding NaOH solid into the ionic liquid, and continuously stirring;
(3) transferring the solution in the step (2) into a stainless steel high-pressure kettle with a polytetrafluoroethylene lining, sealing the kettle, placing the kettle in an oven, and reacting at the temperature of (150-;
(4) after the reaction is finishedNaturally cooling the autoclave to room temperature, centrifugally separating the product, sequentially washing the product by deionized water and absolute ethyl alcohol, and drying the product in vacuum to obtain Fe2O3And (4) a nano ring.
Preferably, the above scheme can also be set as follows:
(1) accurately weighing (3-6) mmol ferric chloride hexahydrate to be dispersed in 20mL absolute ethyl alcohol to obtain a clear solution;
(2) slowly adding (3-6) mmol of ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM ] Cl into the clarified solution obtained in the step (1), stirring vigorously until the ionic liquid is fully dispersed, adding 6mmol of NaOH solid into the mixture, and continuing to stir magnetically;
(3) transferring the solution in the step (2) into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, sealing the autoclave with the volume filling rate of 80 percent, and placing the high-pressure autoclave in an oven (150-;
(4) after the reaction is finished, naturally cooling the autoclave to room temperature, centrifugally separating the product, sequentially washing the product for at least 5 times by deionized water and absolute ethyl alcohol, drying the product in vacuum, and drying the product for 24 hours at 70 ℃ to obtain Fe2O3And (4) a nano ring.
In the step (1), ferric chloride hexahydrate is dispersed in absolute ethyl alcohol by an ultrasonic method.
(3-6) mmol of ferric chloride hexahydrate corresponding to the ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM ] Cl, (3-6) mmol.
In the step (3), the volume filling rate in the autoclave was 80%.
Nanoring Fe prepared herein2O3The characteristics of the photocatalyst can be summarized as follows:
(1) and heat treatment is not needed in the reaction process, so that the production cost of the material is reduced.
(2) The synthesis method is simple, easy to operate, good in repeatability and easy to obtain raw materials.
(3) The photocatalyst has a hollow porous structure, provides a channel for the transmission of reaction substances, increases the specific surface area and reaction sites, and is beneficial to the absorption of light in the process of photocatalytic reaction.
(4) And purchased nanoFe2O3By contrast, we have found that nano-ring Fe prepared using the scheme of the present application2O3The degradation efficiency of industrial dye methyl orange and various reactive dyes is greatly improved.
The present application is further described with reference to the following drawings and detailed description.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of the product of example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the product of example 1;
FIG. 3 is a Transmission Electron Microscope (TEM) photograph of the product of example 1;
FIG. 4 shows Fe of the present application2O3Nanorings and nano-Fe purchased2O3Under the irradiation of visible light, the concentration of the methyl orange solution changes along with time;
FIG. 5 shows Fe of the present application2O3Nanorings and nano-Fe purchased2O3And (3) irradiating for 120min by using visible light to realize the degradation effect of various reactive dyes.
Detailed Description
Example 1
Accurately weighing 4mmol ferric chloride hexahydrate, dispersing in 20mL absolute ethyl alcohol, and obtaining a clear solution under the action of ultrasonic waves. To the clear solution was slowly added 4mmol of ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM]And Cl, stirring vigorously for 30min, adding 6mmol of NaOH solid after the solution is fully dispersed, and continuing to stir magnetically for 1 h. The solution was transferred to a stainless steel autoclave lined with polytetrafluoroethylene (80% volume fill) and the autoclave was sealed. And (3) placing the autoclave in an oven for reaction at 160 ℃ for 24h, and naturally cooling the autoclave to room temperature after the reaction is finished. Centrifugally separating the product, sequentially washing with deionized water and absolute ethyl alcohol for at least 5 times, and vacuum drying the product in a vacuum drying oven at 70 ℃ for 24h to obtain Fe2O3And (4) a nano ring.
All diffraction peaks in the XRD pattern (FIG. 1) can be assigned to the hexagonal rhombohedral structure Fe2O3Standard card (JCPDSNo.33-0664) indicates that the product is hexagonalThe structure belongs to a rhombohedral system; no other diffraction peaks were observed, indicating a higher purity of the product; the SEM result (figure 2) visually shows that the product is in a circular plate-shaped structure, and has good dispersity and uniform size; further, when the TEM image (FIG. 3) is observed, the center of the circular plate-like structure is a hollow structure and the surface is porous, the circular outer diameter is about 400nm, the wall thickness is about 120nm, and the ring thickness is about 150 nm.
To study the photocatalytic activity of the prepared products, solutions of degraded methyl orange and various reactive dyes, such as reactive bright yellow R-4RLN, reactive orange KN-3G, reactive red R-4BD, reactive dark blue R-2GLN and reactive black R-2BG (purchased from Tantuki, Inc., Zhejiang province) were used as evaluation models. For comparison, an equal mass (50mg as an example) of Fe prepared in this example2O3Nanorings and nano-Fe purchased directly2O3Adding 10 mg.L into 100mL-1Performing ultrasonic dispersion in a dye solution to obtain a suspension, and stirring the suspension in a dark place for 60min to achieve absorption and desorption balance; to the above solution was added 5mL of H2O2Solution (30 wt.%), stirring well; irradiating with 300W xenon lamp as light source (with filter to make incident wavelength more than 420nm), sampling at intervals, centrifuging, testing the clear solution with ultraviolet-visible spectrophotometer (UV-vis, UV-2550, Shimadzu corporation), and observing concentration change of dye.
The concentration change curve of the methyl orange solution is shown in fig. 4, and the comparison of the curves shows that: fe prepared in this example under the same experimental conditions2O3The nano-ring is a photocatalyst, visible light irradiates for 60min to ensure that the degradation rate of the methyl orange solution exceeds 90 percent, and the irradiation for 100min almost completely degrades the methyl orange solution; and nano Fe directly purchased2O3Powder, light irradiation 100min, degradation rate of methyl orange solution 55%, and Fe prepared in this example2O3The degradation rate of the nano-ring is obviously higher than that of nano Fe directly purchased2O3。
Under the action of the catalyst, after various reactive dyes are irradiated by visible light for 100min, the degradation effect of various reactive dyes is shown in fig. 5, and Fe prepared in the embodiment2O3The degradation rate of the nano-ring to various reactive dyes exceeds 95 percent, and the purchased nano-Fe2O3Has not exceeded 50%. The comparison of the photocatalysis experimental data shows that Fe2O3The nano-ring has high activity and high speed for degrading dye, and shows excellent visible light catalytic activity.
Examples 2 to 27:
the ionic liquid [ BMIM ] in Table 1 is adopted]The amount of Cl and other experimental conditions were varied to obtain the desired Fe content by varying the reaction temperature and reaction time, ferric chloride hexahydrate and ionic liquid according to the procedure described in example 12O3A nanoring photocatalyst.
TABLE 1 Fe under different conditions2O3Nanoring preparation
The synthesis method for carrying out structure on the finished product nano-ring prepared in the embodiment has the advantages of simple operation, good repeatability, easy reaction control, high yield, product verification and catalytic performance experiments, can determine that the product nano-ring has the same hexagonal structure, is a hollow nano-ring structure, has uniform size, good dispersibility, porous surface and better crystallinity, and can obtain the same effect as the embodiment 1 when used as a photocatalyst for degrading methyl orange solution and various reactive dye solutions.
Claims (7)
1. A ferric oxide nanometer ring photocatalyst is characterized in that: said Fe2O3The nano-ring photocatalyst is powder, the crystalline phase is a hexagonal structure and a rhombohedral crystal system, the appearance is a nano-ring structure, the outer diameter of the particle is 400nm, the wall thickness is 120nm, and the thickness of the ring is 150 nm.
2. A preparation method of a ferric oxide nano-ring photocatalyst is characterized by comprising the following steps:
(1) dispersing ferric trichloride hexahydrate in absolute ethyl alcohol to obtain a clear solution;
(2) adding ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM ] Cl into the clarified solution obtained in the step (1), stirring until the ionic liquid is fully dispersed, adding solid NaOH into the solution, and continuing stirring;
(3) transferring the solution in the step (2) into a stainless steel high-pressure kettle with a polytetrafluoroethylene lining, sealing the kettle, and reacting at the temperature of (150-;
(4) after the reaction is finished, naturally cooling the autoclave to room temperature, centrifugally separating the product, sequentially washing the product by deionized water and absolute ethyl alcohol, and drying the product in vacuum to obtain Fe2O3And (4) a nano ring.
3. The method for preparing the ferric oxide nano-ring photocatalyst according to claim 2, wherein the method comprises the following steps: in the step (1), ferric chloride hexahydrate is dispersed in absolute ethyl alcohol by an ultrasonic method.
4. The method for preparing the ferric oxide nano-ring photocatalyst according to claim 2, wherein the method comprises the following steps: (3-6) mmol of ferric chloride hexahydrate corresponding to the ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM ] Cl, (3-6) mmol.
5. The method for preparing the ferric oxide nano-ring photocatalyst according to claim 2, wherein the method comprises the following steps: in the step (3), the volume filling rate in the autoclave was 80%.
6. A preparation method of a ferric oxide nano-ring photocatalyst is characterized by comprising the following steps:
(1) weighing (3-6) mmol ferric chloride hexahydrate to be dispersed in absolute ethyl alcohol to obtain a clear solution;
(2) adding (3-6) mmol of ionic liquid 1-butyl-3-methylimidazolium chloride [ BMIM ] Cl into the clarified solution obtained in the step (1), stirring until the ionic liquid is fully dispersed, adding 6mmol of solid NaOH, and continuing to stir by magnetic force;
(3) transferring the solution in the step (2) into a stainless steel autoclave lined with polytetrafluoroethylene, sealing the autoclave with a volume filling rate of 80 percent, and reacting at (150-;
(4) after the reaction is finished, naturally cooling the autoclave to room temperature, centrifugally separating the product, sequentially washing the product for at least 5 times by deionized water and absolute ethyl alcohol, and drying the product for 24 hours in vacuum at 70 ℃ to obtain Fe2O3A nanoring photocatalyst.
7. The method for preparing ferric oxide nano-ring photocatalyst according to claim 6, wherein the method comprises the following steps: in the step (1), ferric chloride hexahydrate is dispersed in absolute ethyl alcohol by an ultrasonic method.
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| CN201911023410.7A Withdrawn CN110694627A (en) | 2019-10-25 | 2019-10-25 | Ferric oxide nano-ring photocatalyst and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112340779A (en) * | 2020-09-28 | 2021-02-09 | 燕山大学 | Doughnut-shaped Fe2O3Preparation method of/C lithium ion battery cathode material |
| CN113522247A (en) * | 2021-07-29 | 2021-10-22 | 北京科技大学 | Enzyme-driven alpha-Fe2O3UiO porous micromotor and preparation method and application thereof |
| CN114471615A (en) * | 2022-02-24 | 2022-05-13 | 河南科技大学 | Preparation method and application of Pd-Cu alloy nano sea urchin |
| CN115055185A (en) * | 2022-06-14 | 2022-09-16 | 新余学院 | Preparation method and application of iron oxide nanofiber |
-
2019
- 2019-10-25 CN CN201911023410.7A patent/CN110694627A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112340779A (en) * | 2020-09-28 | 2021-02-09 | 燕山大学 | Doughnut-shaped Fe2O3Preparation method of/C lithium ion battery cathode material |
| CN113522247A (en) * | 2021-07-29 | 2021-10-22 | 北京科技大学 | Enzyme-driven alpha-Fe2O3UiO porous micromotor and preparation method and application thereof |
| CN114471615A (en) * | 2022-02-24 | 2022-05-13 | 河南科技大学 | Preparation method and application of Pd-Cu alloy nano sea urchin |
| CN114471615B (en) * | 2022-02-24 | 2023-07-21 | 河南科技大学 | Preparation method and application of Pd-Cu alloy nano sea urchin |
| CN115055185A (en) * | 2022-06-14 | 2022-09-16 | 新余学院 | Preparation method and application of iron oxide nanofiber |
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