CN111514936B - TiO with hollow frame shape 2 @ MOF heterojunction photocatalyst and preparation method thereof - Google Patents
TiO with hollow frame shape 2 @ MOF heterojunction photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 10
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 9
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 9
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 9
- 229940033123 tannic acid Drugs 0.000 claims abstract description 9
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 9
- 229920002258 tannic acid Polymers 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 5
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 239000003223 protective agent Substances 0.000 abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 23
- 239000012621 metal-organic framework Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000002524 electron diffraction data Methods 0.000 description 4
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- B01J35/39—
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B01J35/23—
-
- 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
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- 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
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/40—Complexes comprising metals of Group IV (IVA or IVB) as the central metal
- B01J2531/46—Titanium
-
- 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 present invention providesTiO with hollow frame appearance 2 A preparation method of a @ MOF heterojunction photocatalyst comprises the following steps: dissolving tetraisopropyl titanate and 2-amino terephthalic acid in an organic solvent, transferring the solution to a reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain NH with a square structure 2 -MIL-125 precursor; reacting NH 2 Dissolving an MIL-125 precursor and tannic acid in an aqueous solution to obtain a mixed solution, transferring the mixed solution into a reaction kettle, heating for reacting for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain TiO with a hollow frame shape 2 @ MOF heterojunction photocatalyst. The invention selects tannic acid as a directional protective agent, and then etches NH from inside to outside by a hydrolysis method 2 MIL-125, resulting in a bare TiO with {100} planes 2 @ MOF hollow frame structure, photocatalyst TiO prepared 2 @ MOF vs. pure TiO 2 And pure MOF has higher photocatalytic activity.
Description
Technical Field
The invention relates to a nano material, and in particular relates to a TiO2@ MOF heterojunction photocatalyst with a hollow frame morphology and a preparation method thereof.
Background
The Metal Organic Framework (MOF) is a crystal material with a porous network structure formed by self-assembly of metal ions and organic ligands, and has the advantages of high specific surface area, adjustable pore diameter, high crystallinity and easy modification of the surface. NH (NH) 2 MIL-125(Ti) is an amino-functionalized Ti-based MOF, and has been used as a visible light photocatalyst in the photocatalytic fields of water purification, hydrogen production, organic synthesis and the like due to the characteristics of low price, no toxicity, stability to water/light and sensitivity to visible light. NH like other monocomponent inorganic semiconductor photocatalysts 2 MIL-125(Ti) also has a high electron-hole recombination rate under light irradiation, resulting in a decrease in photocatalytic performance. Thus, the charge separation efficiency is improved, and the recombination of photo-generated electrons and hole pairs can be inhibited, so that the photocatalytic activity is improved. The construction of semiconductor heterostructures has proven to be an effective method to improve the efficiency of separation of photogenerated electrons and hole carriers. A spatial separation of holes and electrons can be achieved. In addition, the holes in the hollow frame structure of the material can improve the diffusion efficiency of reaction molecules, expose more active sites for catalytic reaction, improve the usability of the inner surface and further have good photocatalytic property. However, the TiO with the hollow frame appearance is designed and prepared 2 The photocatalyst of the @ MOF heterostructure remains a significant challenge.
Disclosure of Invention
The invention selects tannic acid as a directional protective agent, and then etches NH from inside to outside through a hydrolysis method 2 MIL-125(Ti), resulting in a bare TiO with {100} planes 2 @ MOF hollow frame structure. The TiO with the hollow frame appearance is prepared by adopting a method of directional chemical protection and in-situ self-sacrifice hydrolytic etching 2 @ MOF heterostructure composite nanomaterials. And the prepared photocatalyst TiO 2 @ MOF vs. pure TiO 2 And pure MOF has higher photocatalytic activity.
Specifically, the invention provides TiO with a hollow frame appearance 2 A preparation method of the @ MOF heterojunction photocatalyst comprises the following steps:
s1: dissolving tetraisopropyl titanate and 2-amino terephthalic acid in an organic solvent, transferring the solution to a reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain NH with a square structure 2 -MIL-125 precursor;
s2: reacting NH 2 Dissolving an MIL-125 precursor and tannic acid in an aqueous solution to obtain a mixed solution, transferring the mixed solution into a reaction kettle, heating for reacting for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain TiO with a hollow frame shape 2 @ MOF heterojunction photocatalyst.
Further, the organic solvent is a mixture of organic solvent and water in a volume ratio of 7: 5 of N, N-dimethylformamide and a methanol solution.
Further, in the step S1, the heating temperature is 150 ℃, and the reaction time is 24 hours.
Further, in the step S2, NH 2 The mass ratio of the MIL-125 precursor to the tannic acid is 1: 2.
further, the heating temperature in the step S2 is 150 ℃, and the reaction time is 60 min.
The invention also provides TiO with the hollow frame appearance prepared by the method 2 @ MOF heterojunction photocatalyst.
Compared with the prior art, the invention has the beneficial effects that:
the invention selects tannic acid as a directional protective agent, and then etches NH from inside to outside by a hydrolysis method 2 MIL-125(Ti), resulting in a bare TiO with {100} planes 2 @ MOF hollow framework structure. The invention adopts the method of directional chemical protection and in-situ self-sacrifice hydrolytic etching to prepare TiO with hollow frame appearance 2 @ MOF heterostructure composite nanomaterial and photocatalyst TiO prepared from same 2 @ MOF vs. pure TiO 2 And pure MOF has higher photocatalytic activity.
Drawings
FIG. 1 shows NH prepared in an example of the present invention 2 X-ray powder diffraction Pattern (a) and NH of the MIL-125 precursor 2 -scanning electron microscopy of MIL-125 precursor (b);
FIG. 2 shows TiO compounds prepared in accordance with an embodiment of the present invention 2 Scanning electron micrograph (a) and elemental distribution (b-f) of @ MOF, with the inset being TiO at 500nm scale 2 @ MOF scanning Electron microscopy;
FIG. 3 illustrates TiO compounds prepared by the example of the present invention 2 X-ray powder diffraction patterns of @ MOF heterostructures;
in FIG. 4, a is TiO prepared by the example of the present invention 2 Transmission plot of the @ MOF heterostructure;
b is TiO as viewed from region 1 of the graph a 2 HRTEM image of @ MOF, where the inset is the corresponding electron diffraction pattern;
c is TiO as viewed from region 2 of the graph a 2 HRTEM image of @ MOF, where the inset is the corresponding electron diffraction pattern;
FIG. 5 shows TiO irradiated under simulated sunlight 2 @MOF，TiO 2 Photolytic hydrogen generation rate map of MOF (300W Xe lamp, AM 1.5G).
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
The first step is as follows: synthesis of NH 2 -MIL-125 precursor
Dissolving 75 mu.L of tetraisopropyl titanate (TIPT) and 70mg of 2-amino terephthalic acid in 10mL of N, N-dimethylformamide and methanol in a volume ratio of 7: 5, transferring the mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating to 150 ℃, and reacting for 24 h. After the reaction is finished, collecting the product by centrifugation, washing the product with absolute ethyl alcohol for a plurality of times, and drying the product in a drying box to obtain the NH with the square structure 2 MIL-125 precursor (FIG. 1).
The second step is that: synthesis of TiO 2 @ MOF heterojunction composite.
Taking NH 2 MIL-125 precursor (10mg) and tannic acid (20mg) were dissolved in 10mL of aqueous solution, and the above mixed solution was transferred to a Teflon autoclave and heated to the target reaction temperature (150 ℃) and the desired reaction time (60 min). After the reaction is finished, collecting a product through centrifugation, washing the product for a plurality of times by using absolute ethyl alcohol and deionized water, and drying the product in a drying box to obtain uniform TiO with the hollow frame shape 2 @ MOF heterojunction composite. FIG. 2a is a TiO prepared according to an embodiment of the present invention 2 Scanning Electron Microscopy (SEM) for @ MOF, FIG. 2(b-f) is TiO 2 @ MOF element distribution map (EDX). FIG. 3 shows TiO 2 X-ray powder diffraction pattern (XRD) of the @ MOF heterostructure. FIG. 4a is TiO 2 Transmission view of the @ MOF heterostructure (TEM). 4b is TiO as observed from region 1 of FIG. 4a 2 HRTEM image of @ MOF, inset: corresponding electron diffraction pattern (SEAD). 4c is TiO as observed from region 2 of FIG. 4a 2 HRTEM image of @ MOF, inset: corresponding electron diffraction pattern (SEAD). FIG. 5 is a graph of TiO prepared under simulated solar irradiation 2 @ MOF with TiO 2 FIG. 5 shows the comparison of hydrogen rate maps of photolyzed water from MOF (300W Xe lamp, AM 1.5G), and the photocatalyst TiO shown in FIG. 5 2 @ MOF vs. pure TiO 2 And pure MOF has higher photocatalytic activity.
Claims (6)
1. TiO with hollow frame shape 2 A preparation method of the @ MOF heterojunction photocatalyst is characterized by comprising the following steps:
s1: dissolving tetraisopropyl titanate and 2-amino terephthalic acid in an organic solvent, transferring the solution to a reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain NH with a square structure 2 -MIL-125 precursor;
s2: reacting NH 2 Dissolving an MIL-125 precursor and tannic acid in an aqueous solution to obtain a mixed solution, transferring the mixed solution into a reaction kettle, heating for reacting for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain TiO with a hollow frame shape 2 @ MOF heterojunction photocatalyst.
2. The method according to claim 1, wherein the organic solvent is a mixture of organic solvents in a volume ratio of 7: 5 of N, N-dimethylformamide and methanol.
3. The method according to claim 1, wherein in step S1, the heating temperature is 150 ℃ and the reaction time is 24 h.
4. The method according to claim 1, wherein in step S2, NH is added 2 The mass ratio of the MIL-125 precursor to the tannic acid is 1: 2.
5. the method of claim 1, wherein in step S2, the heating temperature is 150 ℃ and the reaction time is 60 min.
6. TiO with hollow frame morphology prepared by the method of any one of the preceding claims 2 @ MOF heterojunction photocatalyst.
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| CN112495444B (en) * | 2020-12-18 | 2022-12-06 | 吉林师范大学 | TiO2 2 Preparation method and application of @ HKUST-1 composite photocatalyst |
| CN114632549A (en) * | 2022-03-07 | 2022-06-17 | 河南师范大学 | alpha-TiO2@NH2Preparation method of-MIL-125 composite photocatalytic material |
| CN114632548A (en) * | 2022-03-07 | 2022-06-17 | 河南师范大学 | One-step synthesis of alpha-TiO2@NH2Method for preparing-MIL-125 composite photocatalytic material |
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