CN107935055B - layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake - Google Patents
layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake Download PDFInfo
- Publication number
- CN107935055B CN107935055B CN201810024099.7A CN201810024099A CN107935055B CN 107935055 B CN107935055 B CN 107935055B CN 201810024099 A CN201810024099 A CN 201810024099A CN 107935055 B CN107935055 B CN 107935055B
- Authority
- CN
- China
- Prior art keywords
- layered
- pyridine
- visible light
- nano
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000031700 light absorption Effects 0.000 title abstract description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 54
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000004729 solvothermal method Methods 0.000 claims abstract description 12
- OENLEHTYJXMVBG-UHFFFAOYSA-N pyridine;hydrate Chemical compound [OH-].C1=CC=[NH+]C=C1 OENLEHTYJXMVBG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000012429 reaction media Substances 0.000 claims abstract description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 29
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000010521 absorption reaction Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 229960002089 ferrous chloride Drugs 0.000 abstract description 13
- 239000002107 nanodisc Substances 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 239000002086 nanomaterial Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 229910002588 FeOOH Inorganic materials 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 150000002505 iron Chemical class 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 230000032900 absorption of visible light Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- WSSMOXHYUFMBLS-UHFFFAOYSA-L iron dichloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Fe+2] WSSMOXHYUFMBLS-UHFFFAOYSA-L 0.000 description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 241000482268 Zea mays subsp. mays Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002088 nanocapsule Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
layered α -Fe with visible light absorption enhancement2O3A process for preparing laminated α -Fe by solvothermal method using pyridine-water as reaction medium and ferrous chloride as iron source2O3The method solves the problems of difficult removal of the template and the surfactant and the like, and the product obtained by the method has the advantages of controllable form, excellent performance and the like, and can produce α -Fe with high quality and high performance2O3The nanometer material provides effective ways, and the prepared product is prepared by several α -Fe with the thickness of nanometer scale2O3The disc is assembled into a layered micro-nano disc structure.
Description
Technical Field
The invention relates to the technical field of preparation of nano materials with visible light enhanced absorption characteristics, in particular to layered α -Fe with visible light enhanced absorption2O3A preparation method of nanometer round cake.
Background
Nanostructure α -Fe2O3Has wide application prospect in the fields of gas sensing, catalysis, magnetic recording, biomedicine and the like, and is well known to be α -Fe2O3The properties of the nanomaterial are directly related to their morphology, and thus, various forms of α -Fe were prepared2O3Nanomaterial is a focus of attention.
The preparation method is, for example, with span80, PVP, DMF, CTAB, (NH)4)2S2O8、NaH2PO4、NaClO3And sodium oleate and the like as morphology control agents, and series α -Fe with regular morphology, such as spindle shape, spherical shape, cube shape and the like, is synthesized by adopting a hydrothermal method2O3Nano-structureα -Fe can be obtained by adopting a precursor method2O3Synthesis of V α -Fe by sol-gel method from Kyoungja Woo et al2O3The α -Fe is obtained by adopting a thermal oxidation method2O3The α -Fe is prepared by a template method2O3Nanotubes and α -Fe2O3Porous nano structure, and solvent heating method to obtain porous popcorn α -Fe2O3From the above, it can be seen that the current pair of nano α -Fe2O3The preparation method mainly comprises a hydrothermal method, a template method and a precursor method. Most hydrothermal methods introduce various organic surfactants, which causes inconvenience in washing of the final product. The template method and the precursor method are complicated to operate.
The invention adopts a solvothermal method to successfully obtain the layered α -Fe with enhanced absorption of visible light2O3The nanometer round cake solves the problems of difficult removal of the template and the surfactant and the like.
Disclosure of Invention
The technical problem to be solved by the invention is to provide kinds of visible light enhanced absorption layered α -Fe with simple process, high product quality and excellent performance, and is suitable for industrial production2O3A preparation method of nanometer round cake.
In order to achieve the purpose, the invention adopts the technical scheme that visible light absorption-enhanced layered α -Fe2O3The preparation method of the nano round cake is characterized in that pyridine-water is used as a reaction medium, and ferrous chloride (FeCl) is used2.4H2O) is an iron source, and layered α -Fe is prepared by a solvothermal method2O3Controlling α -Fe by regulating the ratio of pyridine to water, the type of ferric salt and the reaction temperature2O3Form is shown.
Layered α -Fe as visible light enhanced absorption for the present invention2O3The preferable technical scheme of the preparation method of the nano round cake comprises the following steps:
1) FeCl was added at room temperature2.4H2Adding O solid into mixed medium of pyridine and waterStirring and mixing;
2) FeCl is added2.4H2Transferring the O-pyridine-water mixture into a reaction kettle, and obtaining layered α -Fe by a solvothermal method2O3And (4) nano round cakes.
Layered α -Fe as visible light enhanced absorption for the present invention2O3The preparation method of the nano round cake preferably comprises steps:
FeCl in step 1)2.4H2The addition ratio of O, pyridine and water is 0.2-1.2 g: 20-30 mL: 0-1.5 mL.
In the step 2), the reaction temperature of the solvothermal method is 160-180 ℃, and the reaction time is 6-24 h.
The invention uses pyridine and water as reaction media and FeCl2.4H2O is an iron source, and the lamellar α -Fe with enhanced absorption of visible light is successfully obtained by adopting a solvothermal method2O3The product obtained by the method has the advantages of controllable shape, excellent performance and the like, and is used for producing α -Fe with high quality and high performance2O3The nanometer material provides effective ways, and the prepared product is prepared by several α -Fe with the thickness of nanometer scale2O3The disc is assembled into a layered micro-nano disc structure.
Meanwhile, experiments prove that if ferrous sulfate (FeSO) is used4.7H2O) or ferric chloride (FeCl)3.6H2O) is an iron source, and random α -Fe is obtained under the same reaction conditions in a pyridine-water system2O3The results of visible light absorption test show that the layered α -Fe2O3The range of the absorption of visible light of the nano round cake is larger than that of α -Fe2O3The absorption range of the nano-particles is large, namely layered α -Fe2O3The nano-patty has enhanced visible light absorption properties.
The preparation method of the invention is compared with the existing α -Fe2O3Compared with the preparation technology of the nano material, the preparation method has the advantages of less required raw materials, simple operation and capability of obtaining α with regular form and excellent optical performance without other form control agents-Fe2O3And (3) nano materials. The beneficial effects are also shown as follows:
1) the invention is used for preparing α -Fe2O3The nano material needs less raw materials, the preparation method is simple, and the shape of the nano material is controllable α -Fe2O3The preparation of the nanometer material provides new processes.
2) Layered α -Fe obtained according to the invention2O3The nano round cake has the characteristic of enhancing the absorption of visible light, and is expected to be used in the field of removing pollutants by visible light catalysis.
Drawings
FIG. 1 is a morphological and phase analysis of the final product obtained in example 1;
FIG. 2 is a microstructure analysis of the final product obtained in example 1;
FIG. 3 is a graph showing the effect of iron salt species on the morphology of the final product in example 2;
FIG. 4 shows α -Fe in example 3 in different forms2O3The visible light absorption spectrum of the nanomaterial.
Detailed Description
The following examples and figures are combined to provide a layered α -Fe with enhanced absorption of visible light rays of the present invention2O3The preparation method of the nano-patty is further detailed in step . the morphology of the product obtained by the method of the invention is observed by using a field emission electron microscope (FE-SEM, FEI silicon 200), and the phase of the product is measured by using an X-ray diffractometer (XRD, Philips X' Pert, Cu K)αline, λ -0.15419 nm.) before observing the crystallization and intrinsic structure of the product, an appropriate amount of the product was taken and placed in an ethanol solution for ultrasonic dispersion, then the sample dispersed in the ethanol solution was transferred to a copper mesh coated with a carbon film for transmission electron microscopy characterization, and an appropriate amount of the dispersion was placed in a cuvette, and the other cuvette was filled with ethanol for UV-vis.
Example 1 visible light enhanced absorption of layered α -Fe2O3Preparation of nano round cake
Layered α -Fe with enhanced absorption of visible light2O3The preparation method of the nano round cake comprises the following steps:
1) 0.5g of FeCl was added at room temperature2.4H2O, 25mL of pyridine and 1mL of water are stirred and mixed;
2) FeCl is added2.4H2Transferring the O-pyridine-water mixture into a reaction kettle, and reacting for 16h at 170 ℃ by a solvothermal method to obtain layered α -Fe2O3And (4) nano round cakes.
α-Fe2O3Analysis of formation in pyridine-water system:
α-Fe2O3the following 3 processes can be seen, and can be represented by equations (1), (2) and (3), respectively. FeCl at room temperature2.4H2O reacts with pyridine-water system in air to generate α -FeOOH with yellow color (see reaction formulas (1) and (2)), and α -FeOOH is dehydrated to α -Fe in pyridine-water system in solvothermal reaction2O3(see reaction formula (3)).
Figures 1 and 2 are morphological and structural representations of the products obtained. As can be seen from FIGS. 1a and 1b, in FeCl2.4H2O-pyridine-H2In the O system, the obtained product is in the shape of a round cake, the round cake is composed of a plurality of round plates with the thickness of nanometer scale, and the XRD analysis on the product shows that the product in the shape of a multilayer cake is α -Fe2O3(see results in FIG. 1 c.) FIG. 2 is a single α -Fe2O3TEM and HRTEM results of the nano-wafer can obtain single α -Fe2O3The degree of crystallinity of the nano-disc is very high, and the whole disc is single crystals.
Example 2: influence of iron salt species on the final product.
Multilayer cake α -Fe2O3The formation of (b) is related to the kind of iron salt.
Under the premise of identical other experimental conditions, FeCl is adopted3.6H2O and FeSO4.7H2When two iron sources are O, α -Fe with both irregular phases is obtained2O3Nanoparticles (shown in fig. 3a and 3b, respectively). The alkaloid pyridine homoenergetic is combined with Fe2+And Fe3 +Formation of Fe (OH)2Or α -FeOOH and Fe (OH)3Precursor of hydrated iron oxide precipitate, which can obtain α -Fe through subsequent dehydration reaction2O3And (3) obtaining the product. However, only by FeCl2.4H2O in pyridine-H2α -FeOOH formed in the O system can only form α -Fe in the form of cake in the subsequent dehydration2O3. And FeSO4.7H2O in pyridine-H2α -FeOOH can be formed in the O system, but only irregular α -Fe can be obtained after dehydration2O3Nanoparticles, which illustrate a cake of α -Fe2O3The formation of (b) requires a special iron salt and a dehydration medium.
Example 3 different morphology α -Fe2O3And (3) researching the visible light absorption characteristics of the nano material.
α-Fe2O3The nano material has visible light absorption performance and α -Fe with different forms2O3The response of the nanomaterials to visible light is also different FIG. 4a is a layer α -Fe2O3The visible light absorption spectrum of the nano-disc shows that the maximum absorption wavelength is about 600nm, and the random α -Fe is shown in FIG. 4b and FIG. 4c2O3Nanoparticles (preparation of example 2, b, c correspond to FeCl as the starting material respectively3.6H2O and FeSO4.7H2O), the maximum absorption wavelength of the two is about 420nm, and a comparison shows that the layered form is α -Fe2O3Irregular nano-disc ratio α -Fe2O3The nanoparticles have a greater range of visible light absorption. Due to the fact thatThus, α -Fe was layered2O3The nanocapsules have excellent visible light absorption properties.
Example 4 ratio of pyridine to Water, reaction temperature to α -Fe2O3Influence of morphology
It was experimentally confirmed that when water was present in excess in the pyridine-water system, the product obtained was random α -Fe2O3. Due to FeCl2.4H2O itself contains partial water of crystallization, so that α -Fe with high quality and high performance can be obtained when no water is added into the system2O3And (4) nano round cakes. Control of FeCl in view of the solubility of iron salts and starting point based on low use of pyridine2.4H2The addition ratio of O, pyridine and water is 0.2-1.2 g, 20-30 mL and 0-1.5 mL, and α -Fe with the best performance can be obtained as the optimal proportion2O3And (3) obtaining the product.
In addition, when the reaction temperature of the solvothermal method is lower than 160 ℃, a relatively pure product cannot be obtained; when the temperature exceeds 180 ℃, the obtained product has larger size and is easy to generate agglomeration.
In summary, the ratio of pyridine to water, the type of iron salt and the reaction temperature were α -Fe2O3The regulation of morphology has a large degree of influence.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (1)
1, visible light enhanced absorption layered α -Fe2O3The preparation method of the nano round cake is characterized in that pyridine-water is used as a reaction medium, and FeCl is used as a material2·4H2O is an iron source, and layered α -Fe is prepared by a solvothermal method2O3Nano round cakes; by regulating the ratio of pyridine to water, the type of ferric salt and the reaction temperatureTo control α -Fe2O3Form; the method comprises the following specific steps:
1) FeCl was added at room temperature2·4H2Adding the solid O into a pyridine-water mixed medium, and stirring and mixing; FeCl2·4H2The addition ratio of O, pyridine and water is 0.2-1.2 g: 20-30 mL: 0-1.5 mL;
2) FeCl is added2·4H2Transferring the O-pyridine-water mixture into a reaction kettle, and obtaining layered α -Fe by a solvothermal method2O3And (3) carrying out solvothermal reaction on the nano round cake at the temperature of 160-180 ℃ for 6-24 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810024099.7A CN107935055B (en) | 2018-01-10 | 2018-01-10 | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810024099.7A CN107935055B (en) | 2018-01-10 | 2018-01-10 | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107935055A CN107935055A (en) | 2018-04-20 |
| CN107935055B true CN107935055B (en) | 2020-01-31 |
Family
ID=61938465
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810024099.7A Active CN107935055B (en) | 2018-01-10 | 2018-01-10 | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107935055B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293675B (en) * | 2008-06-12 | 2010-08-25 | 浙江大学 | Method for preparing hexagonal disc shaped alpha-Fe2O3 powder |
| CN103601253B (en) * | 2013-11-05 | 2014-12-24 | 陕西科技大学 | Disk type alpha-Fe2O3 photocatalyst and preparation method and application thereof |
| CN104556245B (en) * | 2014-12-31 | 2016-08-17 | 中国地质大学（武汉） | A kind of hamburger nano oxidized iron material of shape and its production and use |
| CN106082353B (en) * | 2016-06-12 | 2017-09-08 | 常州大学 | A kind of preparation method of ferric oxide nano piece |
-
2018
- 2018-01-10 CN CN201810024099.7A patent/CN107935055B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| α-Fe2O3 nanosheet-assembled hierarchical hollow mesoporous microspheres: Microwave-assisted solvothermal synthesis and application in photocatalysis;Tuan-Wei Sun et al.;《Journal of Colloid and Interface Science》;20151022;第107-117页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107935055A (en) | 2018-04-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Palanisamy et al. | Synthesis of spherical NiO nanoparticles through a novel biosurfactant mediated emulsion technique | |
| Yu et al. | Shape and Phase Control of ZnS Nanocrystals: Template Fabrication of Wurtzite ZnS Single‐Crystal Nanosheets and ZnO Flake‐like Dendrites from a Lamellar Molecular Precursor ZnS·(NH2CH2CH2NH2) 0.5 | |
| Liu et al. | Synthesis, characterization and magnetic properties of β-MnO2 nanorods | |
| Liu et al. | Hydrothermal synthesis and characterization of α-FeOOH and α-Fe2O3 uniform nanocrystallines | |
| Zhao et al. | One-step synthesis of highly water-dispersible Mn 3 O 4 nanocrystals | |
| WO2015196867A1 (en) | Method for preparing metal oxide | |
| Nyirő-Kósa et al. | Novel methods for the synthesis of magnetite nanoparticles with special morphologies and textured assemblages | |
| Sun et al. | Magnetite hollow spheres: solution synthesis, phase formation and magnetic property | |
| Wang et al. | Morphology controllable synthesis of nickel nanopowders by chemical reduction process | |
| Kashid et al. | Microwave assisted synthesis of nickel nanostructures by hydrazine reduction route: Effect of solvent and capping agent on morphology and magnetic properties | |
| Han et al. | Hierarchical flower-like Fe 3 O 4 and γ–Fe 2 O 3 nanostructures: Synthesis, growth mechanism and photocatalytic properties | |
| CN101508468A (en) | Nano-superstructure polyporous material of ferrite and method of preparing the same | |
| Cheng et al. | A facile method to fabricate porous Co3O4 hierarchical microspheres | |
| Zheng et al. | Controllable synthesis of monodispersed iron oxide nanoparticles by an oxidation-precipitation combined with solvothermal process | |
| Katsuki et al. | Controlled synthesis of hexagonal α-Fe2O3 crystals for ceramic colors by hydrothermal reaction of FeCl3 and NaOH solutions | |
| Guo et al. | Synthesis of SnO2 hollow microspheres with core-shell structures through a facile template-free hydrothermal method | |
| CN112125344A (en) | Preparation method of monodisperse nano iron oxide dispersoid | |
| Guo et al. | Synthesis, phase transition, and magnetic property of iron oxide materials: effect of sodium hydroxide concentrations | |
| CN107935055B (en) | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake | |
| KR101129559B1 (en) | Synthesis method of size and shape-controlled hematite | |
| CN104384525A (en) | Dispersing and assembling method of nickel-iron metal nano-wires | |
| Zhou et al. | Preparation of hierarchical leaf-like cobalt and enhanced magnetic properties by a new low-temperature synthesis method | |
| Shen et al. | Preparation of magnetite core–shell nanoparticles of Fe3O4 and carbon with aryl sulfonyl acetic acid | |
| CN113680291B (en) | Preparation method of paramagnetic metal oxide/spinel/carbon composite microsphere | |
| CN109338466B (en) | Preparation of single crystal Fe2O3Method for self-assembling nano-particle into elliptical micro-nano structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |