CN107983353B - TiO 22-Fe2O3Preparation method and application of composite powder - Google Patents
TiO 22-Fe2O3Preparation method and application of composite powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 99
- 239000002131 composite material Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 142
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 129
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 75
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000005286 illumination Methods 0.000 claims abstract description 12
- 239000011941 photocatalyst Substances 0.000 claims abstract description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 48
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000002244 precipitate Substances 0.000 claims description 26
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 24
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000003786 synthesis reaction Methods 0.000 claims description 18
- 230000015572 biosynthetic process Effects 0.000 claims description 16
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- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 13
- 239000001257 hydrogen Substances 0.000 abstract description 13
- 239000002096 quantum dot Substances 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
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- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 8
- 229910052595 hematite Inorganic materials 0.000 description 7
- 239000011019 hematite Substances 0.000 description 7
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 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 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 230000033558 biomineral tissue development Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
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- 150000001875 compounds Chemical class 0.000 description 4
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- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
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- 239000007789 gas Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
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- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
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- 238000010672 photosynthesis Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 208000002430 Multiple chemical sensitivity Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 238000000231 atomic layer deposition Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
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- 238000000338 in vitro Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
- 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 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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- 102000004169 proteins and genes Human genes 0.000 description 1
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- 230000004044 response Effects 0.000 description 1
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- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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- 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
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/39—
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
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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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/38—Organic compounds containing nitrogen
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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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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a TiO 22/Fe2O3The preparation method of the composite powder adopts green leaves of plants as a biological template and a photocatalytic reaction carrier to adjust TiO2/Fe2O3The catalytic reaction is carried out under the illumination, and TiO is prepared at low temperature2Nanoparticle (quantum dot)/Fe2O3Composite powder with a laminated rod-shaped structure; also discloses the TiO2/Fe2O3The composite powder is used as a photocatalyst or a new energy material; the preparation method has the advantages of low temperature, low cost and simple operation, and the prepared TiO2/Fe2O3The composite powder has a novel nano particle (quantum dot)/laminated nanorod microstructure, a large specific surface area and good photocatalytic performance (photocatalytic degradation and photo-hydrolysis hydrogen production).
Description
Technical Field
The invention belongs to the technical field of photocatalysis and new energy, and relates toTitanium dioxide (TiO)2) Iron oxide (Fe)2O3) The technical field of photocatalysis and new energy, in particular to TiO2Nanoparticle (quantum dot)/Fe2O3Preparation method of laminated nanorod composite powder and TiO prepared by same2/Fe2O3Use of the composite powder.
Background
In recent years, researchers have begun to pay attention to a large number of photocatalysts for photoresponse in order to more effectively utilize inexhaustible clean energy, namely solar energy, and to continuously solve the energy crisis at present. Wherein, TiO2As a semiconductor photocatalyst, the photocatalyst has low cost, no toxicity and high chemical and physical stability, and is widely applied to solar water decomposition hydrogen production, carbon dioxide conversion, solar energy conversion and storage, organic matter degradation, sewage treatment and other aspects. Unfortunately, TiO2The band gap of (Eg =3.2 eV) is wide, inhibiting its ability to absorb visible light, only ultraviolet light. The visible light occupies most of the solar spectrum, and the utilization rate of solar energy is greatly limited. Therefore, current research is focused on how to focus on TiO2The absorption spectrum of the catalyst is expanded to a visible light region, so that better visible light catalysis performance is obtained.
In recent years, researchers have succeeded in doping TiO with metals (silver, gold, platinum, etc.) or non-metals (carbon, sulfur, fluorine, nitrogen, etc.)2To obtain TiO with visible light catalytic activity2The powder is applied to visible light hydrolysis hydrogen production and water pollution treatment.
For example, as early as 1986, Sato et al discovered that nitrogen incorporation can render TiO2Has visible light Activity (Sato S. Photocatalytic Activity of NO)x-doped TiO2in the Visible Light region chem. Phys. Lett., 1986, 123: 126-. At present, the preparation of metal or inorganic non-metal doped TiO2Various methods are available, such as: magnetron sputtering, ion implantation, chemical vapor deposition, firing, sol-gel, and the like. However, these conventional methods usually require a high degree of workBy thermal processes or by the use of expensive additives to achieve TiO2And (3) effectively doping the powder. High cost, low efficiency and the obtained doped TiO2The photocatalytic activity efficiency of the powder needs to be improved.
Therefore, researchers have attempted to improve TiO via another effective approach2With visible light catalytic activity, i.e. with a narrower band gap material and TiO2In combination, a semiconductor junction is created. The currently commonly selected material with a narrow band gap is Fe2O3、CuO、Cu2O, CdSe, CdTe, etc. These materials with TiO2The composite material is compounded to obtain a novel ultraviolet-visible light absorption composite structure with a wide wavelength range, and the novel ultraviolet-visible light absorption composite structure has more excellent performances in photolysis of water to produce hydrogen and treatment of environmental pollutants. Of particular interest is that hematite, as one of the iron oxides, is an active nanocatalysis material. Due to the narrow band gap width (Eg =2.2 eV), low cost and high stability, the method is taken as the most potential candidate material for preparing TiO with more excellent structure and photoelectric property2A composite material.
Recent studies have shown that TiO2/Fe2O3Multilayer films and other composite structures (e.g. Fe)2O3Nano particle coated TiO2Nanosheets, TiO2/Fe2O3Core-shell structure, etc.) has excellent ultraviolet-visible response (y, Zhong et. al, Controllable Synthesis of TiO2@Fe2O3Core-Shell Nanotube Arrays with Double-Wall Coating as Superb Lithium-Ion Battery Anodes. Sci. Rep., 2017, 7: 4092；K. Yao et. al, Fe2O3-TiO2core-shell nanorod arrays for visible lightphotocatalytic applications. Catalysis Today, 2016, 270: 51；K. E. deKrafftet. al, Metal-Organic Framework Templated Synthesis of Fe2O3/TiO2Nanocomposite for Hydrogen production. adv. mater. 2012, 24: 2014). Compared with single TiO2The material has higher efficiency in the aspects of organic matter degradation and hydrogen energy preparation. On the other hand, recent research tables of Sun et alAmorphous TiO with core-shell structure2/α-Fe2O3Nano composite material, compared with anatase type TiO obtained after calcination2/α-Fe2O3Shows more excellent visible light catalytic performance, research shows α -Fe2O3And amorphous TiO2Can separate photo-generated electrons and holes more effectively under visible light, thereby improving the visible light catalytic activity (D.D. Sun, et. al, Tunable Synthesis of Core-shell α -Fe)2O3/TiO2Composite Nanoparticles and the TheirVisible-light Photocalalytic Activity, chem. Res. Chin. Univ., 2016, 32, 882). Thus, amorphous TiO2/α-Fe2O3The preparation of nanocomposites is also of great significance.
At present, TiO is prepared2/Fe2O3The method of the composite material comprises a sol-gel method, an ultrasonic chemical method, an electrochemical method, an evaporation-induced self-assembly method, an atomic layer deposition method, a mechanochemical synthesis method, a hydrothermal preparation technology and the like. In general, these techniques are complex and versatile in nature. Often, special chemical aids, precision equipment or sensitive procedures are required to achieve the desired structure and performance.
On the other hand, TiO obtained in the prior art2/Fe2O3The composite material is generally rough in morphology structure, not perfect and fine enough, and the photoelectric property of the material is also inhibited to a certain extent. Therefore, cheap, simple and efficient TiO is sought2/Fe2O3New synthetic methods for composite materials are constantly sought by researchers.
Disclosure of Invention
The invention aims to solve the technical problem of providing a TiO with a quantum dot-laminated nanorod structure aiming at the defects in the prior art2/Fe2O3A preparation method of composite powder.
The technical scheme adopted by the invention for solving the technical problems is as follows: TiO 22/Fe2O3The preparation method of the composite powder comprises the following steps:
(1) extracting green plant leaf juice: selecting fresh green leaves, and repeatedly washing the leaves clean by water and ethanol; cutting green leaves into fine pieces, grinding into green leaf juice, storing the green leaf juice in a sterilized centrifuge tube, and storing at 4 deg.C;
（2）TiO2/Fe2O3preparing a mixed solution: weighing 1-3 g of ferric trichloride powder, dissolving the ferric trichloride powder in 15-20 ml of green leaf juice, and stirring for 1-2 hours to fully mix the ferric trichloride powder with the green leaf juice; according to the volume ratio of green leaf juice to tetrabutyl titanate of 5-20: measuring tetrabutyl titanate by 1 weight, dropwise adding the tetrabutyl titanate into the ferric trichloride solution, and fully stirring to obtain TiO2/Fe2O3Precipitating the mixed solution;
（3）TiO2/Fe2O3and (3) performing light reaction on the precipitation mixed solution: the TiO prepared in the step (2)2/Fe2O3Placing the precipitate mixed solution under ultraviolet-visible light for illumination reaction, wherein the illumination time is 2-4 h;
（4）TiO2/Fe2O3low-temperature synthesis of composite powder: the TiO prepared in the step (3)2/Fe2O3The precipitation mixed solution is quickly transferred to a polytetrafluoroethylene reaction kettle for low-temperature synthesis reaction; placing the reaction kettle in a muffle furnace, heating to 120-220 ℃ at a heating rate of 5-10 ℃/min, and keeping the temperature at the highest temperature for 20-36 h;
（5）TiO2/Fe2O3purifying the composite powder: centrifuging the product obtained in the step (4) to obtain a reddish brown precipitate; fully cleaning, centrifuging and freeze-drying the reddish brown precipitate to obtain TiO2Nanoparticle (quantum dot)/Fe2O3A composite powder having a laminated rod-like structure.
The TiO2/Fe2O3The preparation method of the composite powder has the advantages that the green leaf juice in the step (1) needs to be taken at present, and the preservation time at 4 ℃ is not more than 3 days.
The TiO2/Fe2O3Method for preparing composite powderThe dropping mode of the tetrabutyl titanate in the step (2) is that a liquid-transferring gun is used for dropping the tetrabutyl titanate into the ferric trichloride solution; the sufficient stirring condition is that tetrabutyl titanate and ferric trichloride solution are stirred for 1.5-2.5 h at room temperature, and the rotating speed is 800-.
The TiO2/Fe2O3The preparation method of the composite powder comprises the step (3) of irradiating with ultraviolet visible full spectrum light of 200-800 nm.
The TiO2/Fe2O3The preparation method of the composite powder comprises the step (4) of quickly transferring the precipitation mixed solution into a polytetrafluoroethylene reaction kettle under the condition of prepared TiO2/Fe2O3The precipitate mixed liquor needs to be transferred to a reaction kettle within 2h for next hydrothermal reaction, so that excessive hydrolysis is avoided.
The TiO2/Fe2O3The preparation method of the composite powder comprises the following steps of (4) enabling the total volume of a reaction kettle to be 50-100 ml; the highest temperature in the muffle furnace is 180-220 ℃, and the heat preservation time is 20-24 h.
The TiO2/Fe2O3The preparation method of the composite powder comprises the following steps of (5) centrifuging at a rotating speed of 8000-10000 r/min; the full cleaning condition is that deionized water is used for centrifugal cleaning for 2-3 times, then ethanol is used for centrifugal cleaning for 1-2 times, and finally clear water is used for centrifugal cleaning for 1-2 times.
The invention also provides TiO obtained by the preparation method2Nanoparticle (quantum dot)/Fe2O3The laminated nano-rod composite powder is used as a photocatalyst or a new energy material.
The invention has the beneficial effects that: TiO prepared according to the above method2/Fe2O3The powder has a perfect composite structure: TiO 22Quantum dots or nano particles are uniformly covered on Fe2O3Laminating the nanorods; wherein the TiO is2Is amorphous or crystalline TiO2And has a perfect quantum dot or nanoparticle structure; fe2O3Is a singleThe hematite phase is of a laminated nanorod structure; TiO 22/Fe2O3The specific surface area of the composite powder is 85-122 m2g-1。
The invention selects a special and cheap biological raw material to prepare TiO with novel structure at low temperature2/Fe2O3A composite material; in the technology of the invention, the green leaves of the plants play the role of regulating and controlling the biological template and the synthetic process at the same time, and not only can be used as the template to regulate TiO2/Fe2O3The microstructure and the crystal form of the compound can be used as a photocatalytic reaction carrier to adjust the reaction process under the illumination of light; the preparation method has the advantages of low temperature, low cost and simple operation, and the prepared TiO is2/Fe2O3The composite powder has a novel microstructure: TiO 22The nano particles or quantum dots are uniformly covered on the Fe2O3Is laminated on the nano rod, and the obtained powder has large specific surface area. Reference, the TiO2/Fe2O3The composite material has good performances of photocatalytic degradation of dye and photolysis of water to produce hydrogen.
Drawings
FIG. 1 shows TiO compounds prepared in accordance with one to four examples of the present invention2/Fe2O3XRD spectrogram of the composite powder;
FIG. 2 shows TiO prepared according to example one of the present invention2/Fe2O3SEM photograph of the composite powder;
FIG. 3 shows TiO prepared according to example two of the present invention2/Fe2O3SEM photograph of the composite powder;
FIG. 4 shows TiO prepared in example III of the present invention2/Fe2O3SEM photograph of the composite powder;
FIG. 5 is a graph showing TiO compounds prepared in comparative example (example four) of the present invention2/Fe2O3SEM photograph of the composite powder.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example one
TiO 22/Fe2O3The preparation method of the composite powder comprises the following steps:
(1) extracting green plant leaf juice: selecting fresh green leaves, and repeatedly cleaning with water and ethanol. Cutting green leaves into fine pieces, and grinding into green leaf juice. Storing the extracted green leaf juice in a sterilized centrifugal tube, storing at 4 ℃, and using as an organic template and a photoreaction carrier in subsequent experiments; in order to maintain the biological activity of the green leaf juice, the extracted green leaf juice needs to be used at present.
（2）TiO2/Fe2O3Preparing a mixed solution: weighing 1 g of ferric chloride powder, dissolving in 20 ml of green leaf juice, and stirring for 2h to fully mix ferric chloride and the green leaf juice; according to the volume ratio of the green leaf juice to the tetrabutyl titanate of 20: measuring tetrabutyl titanate (the volume of the green leaf juice is 20 times of that of tetrabutyl titanate) by 1 weight, dropwise adding into the ferric trichloride solution by using a liquid-transferring gun, and fully stirring for 2h at the rotating speed of 800r/min to obtain TiO2/Fe2O3Precipitating the mixed solution.
（3）TiO2/Fe2O3And (3) performing light reaction on the precipitation mixed solution: the TiO prepared in the step (2)2/Fe2O3And placing the precipitate mixed solution in ultraviolet-visible light (with the wavelength of 200-800 nm) for illumination reaction for 2 hours.
（4）TiO2/Fe2O3Low-temperature synthesis of composite powder: the TiO prepared in the step (3)2/Fe2O3The precipitate mixed solution is quickly transferred to a sealed and corrosion-resistant polytetrafluoroethylene reaction kettle of 100ml for hydrothermal reaction; the reaction kettle is placed in a muffle furnace, the temperature is raised to 120 ℃ at the heating rate of 5 ℃/min, and the temperature is kept at the highest temperature for 24 hours.
（5）TiO2/Fe2O3Purifying the composite powder: centrifuging the product obtained in the step (4) to obtain a reddish brown precipitate (the rotating speed is 8000 r/min); the reddish brown precipitate is successively removedWashing with water for 2 times, washing with ethanol for 1 time, washing with deionized water for 1 time, and freeze drying to obtain TiO2/Fe2O3The composite powder of (1).
The TiO obtained in the example is detected by XRD method2/Fe2O3The composition of the matter phase of the composite powder is amorphous TiO2And Fe2O3(hematite phase) (see line a in FIG. 1); scanning Electron Microscope (SEM) analysis shows that the powder has a quantum dot-laminated nanorod structure (shown in figure 2), and the specific surface area of the powder is 108 m2g-1。
The TiO prepared in this example was taken2/Fe2O3Adding the composite powder into organic dye methylene blue solution (TiO)2/Fe2O3The concentration of the composite powder is 1 g/L, and the concentration of methylene blue is 1 multiplied by 10-5mol/L). Irradiating with visible light with wavelength greater than 420nm for 3 hr. The experimental results show that the obtained TiO2/Fe2O3The composite powder has good visible light catalytic activity and can degrade 75% of methylene blue within 3 hours of visible light irradiation.
The TiO prepared in this example was taken2/Fe2O3The composite powder is subjected to a photolysis water hydrogen production experiment.
The method comprises the following specific steps: the experiment used a 350W xenon lamp (shanghai blue stripe electronics ltd) as the light source and filtered the ultraviolet light with a 420nm filter to provide a visible light source. The distance between the light source and the front of the three-neck flask is set as 20 cm.
In this experiment, 50mg of TiO was weighed2/Fe2O3Powdered and uniformly dispersed into 80mL of aqueous methanol. To ensure TiO2Mixing the nanometer powder with methanol solution, and stirring and ultrasonic treating the water solution. Method for reducing chloroplatinic acid by light on TiO2/Fe2O3The powder surface was plated with 0.6wt% of noble metal Pt. Before the light irradiation, nitrogen gas was introduced into the three-necked flask for 40 minutes to remove dissolved oxygen from the solution. After each 3 hours of light irradiation, 0.4mL of gas was extracted from the system by a trace gas injector and immediately injected into the systemThe amount of hydrogen gas generated was measured on a gas chromatograph (GC-14C, Shimadzu Japan).
The experimental result shows that the hydrogen content of the photolysis water is 4 mol/g when the visible light with the wavelength of more than 420nm is used for irradiation for 3 h.
Another object of the present invention is to use as a photocatalyst or a new energy material. The prepared TiO is mixed2Nanoparticle (quantum dot)/Fe2O3The laminated nanorod composite powder is used for photocatalytic treatment of an organic dye aqueous solution, and can adsorb and degrade macromolecular dye in a very short time. And the photolytic water reaction can be carried out under visible light to prepare a clean and pollution-free hydrogen source.
Example two
TiO 22/Fe2O3The preparation method of the composite powder comprises the following steps:
(1) extracting green plant leaf juice: selecting fresh green leaves, and repeatedly cleaning with water and ethanol. Cutting green leaves into fine pieces, and grinding into green leaf juice. Storing the extracted green leaf juice in a sterilized centrifugal tube, storing at 4 ℃, and using as an organic template and a photoreaction carrier in subsequent experiments; in order to maintain the biological activity of the green leaf juice, the extracted green leaf juice needs to be used at present.
（2）TiO2/Fe2O3Preparing a mixed solution: weighing 1.4 g of ferric chloride powder, dissolving in 20 ml of green leaf juice, and stirring for 1h to fully mix ferric chloride and the green leaf juice; according to the volume ratio of the green leaf juice to the tetrabutyl titanate of 10: measuring tetrabutyl titanate (volume of green leaf juice is 10 times of tetrabutyl titanate) 1, adding dropwise into the ferric trichloride solution with liquid-transferring gun, stirring for 2.5 hr at rotation speed of 1200r/min to obtain TiO2/Fe2O3Precipitating the mixed solution.
（3）TiO2/Fe2O3And (3) performing light reaction on the precipitation mixed solution: the TiO prepared in the step (2)2/Fe2O3And placing the precipitate mixed solution in ultraviolet-visible light (with the wavelength of 200-800 nm) for illumination reaction for 3 hours.
（4）TiO2/Fe2O3Low-temperature synthesis of composite powder: the TiO prepared in the step (3)2/Fe2O3The precipitate mixed solution is quickly transferred to a sealed and corrosion-resistant 50ml polytetrafluoroethylene reaction kettle for hydrothermal reaction; and (3) placing the reaction kettle in a muffle furnace, raising the temperature to the maximum temperature of 180 ℃ at the temperature raising rate of 8 ℃/min, and preserving the temperature for 20 hours at the maximum temperature.
（5）TiO2/Fe2O3Purifying the composite powder: centrifuging the product obtained in the step (4) to obtain a reddish brown precipitate (the rotating speed is 10000 r/min); washing the reddish brown precipitate with deionized water for 3 times, washing with ethanol for 2 times, washing with deionized water for 1 time, and freeze drying to obtain TiO2/Fe2O3The composite powder of (1).
The TiO obtained in this example was tested by the same test method as in example one2/Fe2O3The composition of the matter phase of the composite powder is amorphous TiO2And Fe2O3(hematite phase) (see the line b in figure 1), the powder has a nanoparticle-laminated nanorod composite structure with a specific surface area of 122m2g-1. The resulting TiO2/Fe2O3The powder has higher visible light catalytic activity and can degrade 63 percent of methylene blue within 3 hours of visible light irradiation with the wavelength of more than 420 nm; the hydrogen content of photolyzed water was 2.8 mol/g.
EXAMPLE III
TiO 22/Fe2O3The preparation method of the composite powder comprises the following steps:
(1) extracting green plant leaf juice: selecting fresh green leaves, and repeatedly cleaning with water and ethanol. Cutting green leaves into fine pieces, and grinding into green leaf juice. Storing the extracted green leaf juice in a sterilized centrifugal tube, storing at 4 ℃, and using as an organic template and a photoreaction carrier in subsequent experiments; in order to maintain the biological activity of the green leaf juice, the extracted green leaf juice needs to be used at present.
（2）TiO2/Fe2O3Preparing a mixed solution: weighing 3g of ferric chloride powder, dissolving in 15 ml of green leaf juice, and stirring for 2h to fully mix ferric chloride and the green leaf juice; according to the volume ratio of green leaf juice to tetrabutyl titanate of 5: measuring tetrabutyl titanate (volume of green leaf juice is 5 times of tetrabutyl titanate) 1, adding dropwise into the ferric trichloride solution with liquid-transferring gun, stirring for 2.5 hr at rotation speed of 1200r/min to obtain TiO2/Fe2O3Precipitating the mixed solution.
（3）TiO2/Fe2O3And (3) performing light reaction on the precipitation mixed solution: the TiO prepared in the step (2)2/Fe2O3And placing the precipitate mixed solution under ultraviolet-visible light (with the wavelength of 200-800 nm) for illumination reaction for 3 hours.
（4）TiO2/Fe2O3Low-temperature synthesis of composite powder: the TiO prepared in the step (3)2/Fe2O3The precipitate mixed solution is quickly transferred to a sealed and corrosion-resistant polytetrafluoroethylene reaction kettle of 100ml for hydrothermal reaction; placing the reaction kettle in a muffle furnace, heating to the maximum temperature of 220 ℃ at the heating rate of 10 ℃/min, and keeping the temperature at the maximum temperature for 36 hours;
（5）TiO2/Fe2O3purifying the composite powder: centrifuging the product obtained in the step (4) to obtain a reddish brown precipitate (the rotating speed is 10000 r/min); washing the reddish brown precipitate with deionized water for 2 times, washing with ethanol for 1 time, washing with deionized water for 2 times, and freeze drying to obtain TiO2/Fe2O3The composite powder of (1).
The TiO obtained in this example was tested by the same test method as in example one2/Fe2O3The phase composition of the composite powder of (2) is TiO2(anatase phase and rutile phase) and Fe2O3(hematite phase) (see the line c in figure 1), the powder has a perfect composite structure, and TiO increases with the temperature2The nano particles grow up and uniformly cover the Fe2O3On the nano-rod. The specific surface area is 85 m2g-1. Obtained TiO2/Fe2O3The powder has higher visible light catalytic activity and can degrade 45 percent of methylene blue within 3 hours of visible light irradiation with the wavelength of more than 420 nm; the hydrogen content of photolyzed water is 2 mol/g.
COMPARATIVE EXAMPLE 1 (EXAMPLE IV)
To verify TiO2/Fe2O3The precipitation mixed liquor needs to be transferred into a reaction kettle for low-temperature synthesis reaction within 2h, the damage effect of excessive hydrolysis on the appearance of the product is the same as the third experimental scheme of the embodiment, and only TiO is added2/Fe2O3And standing the precipitate mixed solution at room temperature for 24 h, and transferring the precipitate mixed solution to a reaction kettle for low-temperature synthesis reaction.
Dissolving 1 g of ferric chloride powder in 20 ml of green leaf juice, and stirring for 2 hours to fully mix ferric chloride and the green leaf juice; according to the volume ratio of the green leaf juice to the tetrabutyl titanate of 20: measuring tetrabutyl titanate by 1 weight, dropwise adding the tetrabutyl titanate into the ferric trichloride solution by using a liquid transfer gun, fully stirring for 1h at the rotating speed of 800r/min to obtain TiO2/Fe2O3Precipitating the mixed solution;
the prepared TiO is mixed2/Fe2O3Placing the precipitate mixed solution under ultraviolet-visible light (with the wavelength of 200-800 nm) for illumination reaction for 2 h; the illuminated TiO is treated2/Fe2O3The precipitate mixed solution is quickly transferred to a sealed and corrosion-resistant polytetrafluoroethylene reaction kettle of 100ml for hydrothermal reaction; placing the reaction kettle in a muffle furnace, heating to 120 ℃ at the heating rate of 5 ℃/min, and keeping the temperature at the highest temperature for 24 hours; centrifuging the product obtained by the muffle furnace to obtain a reddish brown precipitate (the rotating speed is 8000 r/min); washing the reddish brown precipitate with deionized water for 2 times, washing with ethanol for 1 time, washing with deionized water for 1 time, and freeze drying to obtain TiO2/Fe2O3The composite powder of (1).
The TiO obtained in this example was tested by the same test method as in example one2/Fe2O3The phase of the composite powder of (2) is made of amorphous TiO2And Fe2O3(hematite phase) composition (seeFIG. 1 line d). As can be seen from the scanned pictures, the morphology of the powder is a spherical assembly (see FIG. 5). As can be seen from the comparative example, excessive hydrolysis breaks down the nanoparticle (quantum dot)/stacked rod composite structure obtained by green leaf juice conditioning.
From the above detailed description of the embodiments of the present invention, it can be understood that the present invention solves the problem of preparing TiO with a perfect composite structure and a large specific surface area by the conventional method2/Fe2O3The difficult conditions of high cost and complex process of the composite powder, and the prepared TiO with novel structure2/Fe2O3The powder has excellent performance, and is suitable for the photocatalyst and can effectively improve the catalytic activity under visible light.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
The upper and lower limits and interval values of the raw materials and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can realize the method, and the examples are not listed.
The invention also includes TiO prepared according to the above method2/Fe2O3The powder has a perfect composite structure: TiO 22The nano particles or quantum dots are uniformly covered on the Fe2O3And laminating the nanorods. TiO 22/Fe2O3The specific surface area of the composite powder is 85-122 m2g-1. In addition, the nitrogen-doped TiO prepared by the invention2The powder material can be used as a photocatalyst and can successfully degrade macromolecular dye methyl orange blue. And the method can be used for new energy materials to successfully prepare clean hydrogen through photolysis of water.
Detecting the obtained TiO by XRD2/Fe2O3Composite powder of TiO2The composition of the object phase is amorphous or other crystal phases; fe2O3Is a single hematite phase. The microstructure of the obtained powder is observed by adopting a scanning electron microscope, and the powder is found to have a perfect composite structure: TiO 22The nano particles or quantum dots are uniformly covered on the Fe2O3And laminating the nanorods.
The invention adopts leaves of green plants to replace other organic templates to prepare TiO with novel structure at low temperature2/Fe2O3And (3) composite powder. It is well known that in the delicate nature, some biological systems synthesize inorganic minerals with perfect structure and excellent properties at room temperature through biomineralization processes. In the formation of these minerals, some organic matter (proteins, polysaccharides, polymers) that is involved in the mineralization process plays a crucial role. The formation of these mineral materials first self-assembles orderly to form certain organic structures, and then on the basis of the organic structures, the inorganic materials are guided to further assemble and form. Therefore, a large number of researchers learn the biomineralization process in the nature, extract or synthesize organic matters with mineralization and guide the synthesis of inorganic materials in vitro. On the other hand, in nature, a large number of green plants synthesize substances necessary for their lives at room temperature through photosynthesis. This process is mainly achieved by the transfer of electrons. Therefore, the invention selects the green leaves capable of photosynthesis as the organic template for the first time, so that the green leaves can be expected to be on TiO2/Fe2O3In the preparation process of the composite powder, the special biological template function is realized to guide and regulate TiO2/Fe2O3And (3) a composite structure of powder. Meanwhile, the process of material synthesis is hoped to be influenced by the electron transfer process under illumination, and the appearance and performance which cannot be obtained by simple biomineralization are obtained.
The green plant widely exists in nature and is used as a biological template and a photoreaction carrier to prepare TiO2/Fe2O3The composite powder has low cost and simple operation, and is suitable for industrial large-scale production. The fresh green leaf juice has special biological activity and function compared with a single organic template. In the preparation method, the green leaf juice is selected as the biological raw material and plays a role of biological modelPlate and regulator effects of the synthesis process. Not only can be used as a template to adjust TiO2/Fe2O3The microstructure and the crystal form of the compound can adjust the reaction process under the illumination, thereby realizing the synthesis of TiO at low temperature2/Fe2O3The aim of the composite powder is to solve the problem that the composite powder with excellent performances in multiple aspects is difficult to obtain simultaneously in a single synthesis process, and obtain TiO with peculiar appearance, large specific surface area and strong visible light catalytic activity2/Fe2O3And (3) composite powder.
The invention effectively solves the problem that some special chemical auxiliary substances, precise equipment or sensitive programs are often needed to obtain the expected structure and performance in the prior art. And a single low-temperature synthesis process is difficult to simultaneously obtain the problems of excellent structure and performance in various aspects. The preparation method has the advantages of low temperature, low cost and simple operation, and the prepared TiO is2/Fe2O3The composite powder has a novel microstructure: TiO 22The nano particles or quantum dots are uniformly covered on the Fe2O3The powder obtained by the method is laminated on the nano rod, has large specific surface area and good photocatalytic performance.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (7)
1. TiO 22/Fe2O3The preparation method of the composite powder is characterized by comprising the following steps:
(1) extracting green plant leaf juice:
selecting fresh green leaves, and repeatedly washing the leaves clean by water and ethanol; cutting green leaves into fine pieces, grinding into green leaf juice, storing the green leaf juice in a sterilized centrifuge tube, and storing at 4 deg.C;
（2）TiO2/Fe2O3preparing a mixed solution:
weighing 1-3 g of ferric trichloride powder, dissolving the ferric trichloride powder in 15-20 ml of green leaf juice, and stirring for 1-2 hours to fully mix the ferric trichloride powder with the green leaf juice; according to the volume ratio of green leaf juice to tetrabutyl titanate of 5-20: measuring tetrabutyl titanate by 1 weight, dropwise adding the tetrabutyl titanate into the ferric trichloride solution, and fully stirring to obtain TiO2/Fe2O3Precipitating the mixed solution;
（3）TiO2/Fe2O3and (3) performing light reaction on the precipitation mixed solution:
adding TiO into the mixture2/Fe2O3Placing the precipitate mixed solution under ultraviolet-visible light for illumination reaction, wherein the illumination time is 2-4 h;
（4）TiO2/Fe2O3low-temperature synthesis of composite powder:
adding TiO into the mixture2/Fe2O3The precipitation mixed solution is quickly transferred to a polytetrafluoroethylene reaction kettle for low-temperature synthesis reaction; placing the reaction kettle in a muffle furnace, heating to 120-220 ℃ at a heating rate of 5-10 ℃/min, and keeping the temperature at the highest temperature for 20-36 h;
（5）TiO2/Fe2O3purifying the composite powder:
centrifuging the product obtained in the step (4) to obtain a reddish brown precipitate; fully cleaning, centrifuging and freeze-drying the reddish brown precipitate to obtain TiO2/Fe2O3The composite powder of (1).
2. A TiO according to claim 12/Fe2O3The preparation method of the composite powder is characterized in that the green leaf juice in the step (1) is used as it is, and the green leaf juice is preserved for no more than 3 days at 4 ℃.
3. A TiO according to claim 12/Fe2O3The preparation method of the composite powder is characterized in that the tetrabutyl titanate in the step (2) is dropwise added into the ferric trichloride solution by using a liquid-transferring gun; the full stirring condition is room temperatureStirring tetrabutyl titanate and ferric trichloride solution for 1.5-2.5 h at the rotation speed of 800-.
4. A TiO according to claim 12/Fe2O3The preparation method of the composite powder is characterized in that the condition that the precipitation mixed solution is quickly transferred into a polytetrafluoroethylene reaction kettle in the step (4) is prepared TiO2/Fe2O3The precipitate mixed liquor is transferred to a reaction kettle for next hydrothermal reaction within 2h, so that excessive hydrolysis is avoided.
5. A TiO according to claim 12/Fe2O3The preparation method of the composite powder is characterized in that the total volume of the reaction kettle in the step (4) is 50-100 ml; the highest temperature in the muffle furnace is 180-220 ℃, and the heat preservation time is 20-24 h.
6. A TiO according to claim 12/Fe2O3The preparation method of the composite powder is characterized in that the centrifugal rotating speed in the step (5) is 8000-10000 r/min; the full cleaning condition is that deionized water is used for centrifugal cleaning for 2-3 times, then ethanol is used for centrifugal cleaning for 1-2 times, and finally clear water is used for centrifugal cleaning for 1-2 times.
7. TiO obtainable by a process according to any one of claims 1 to 62/Fe2O3The composite powder is characterized by being used as a photocatalyst or a new energy material.
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| CN109589959B (en) * | 2019-01-23 | 2021-09-28 | 西北师范大学 | Preparation of alpha-ferric oxide/titanium dioxide nano composite material and application thereof in photocatalytic reduction of carbon dioxide |
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