CN114260027B - Method for preparing metal oxide@metal organic framework core-shell material - Google Patents
Method for preparing metal oxide@metal organic framework core-shell material Download PDFInfo
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910044991 metal oxide Inorganic materials 0.000 title abstract description 10
- 150000004706 metal oxides Chemical class 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims abstract description 14
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 13
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 10
- 239000002105 nanoparticle Substances 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000010335 hydrothermal treatment Methods 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 2
- 238000007605 air drying Methods 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000011257 shell material Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 239000013110 organic ligand Substances 0.000 abstract description 8
- 230000035484 reaction time Effects 0.000 abstract description 8
- 238000001308 synthesis method Methods 0.000 abstract description 5
- 230000006911 nucleation Effects 0.000 abstract description 4
- 238000010899 nucleation Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000011162 core material Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000012621 metal-organic framework Substances 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 238000003917 TEM image Methods 0.000 description 6
- SLCITEBLLYNBTQ-UHFFFAOYSA-N CO.CC=1NC=CN1 Chemical compound CO.CC=1NC=CN1 SLCITEBLLYNBTQ-UHFFFAOYSA-N 0.000 description 3
- ZJLKZLGZJOXUSX-UHFFFAOYSA-N CO.O.O.O.O.O.O.[N+](=O)([O-])[O-].[Zn+2].[N+](=O)([O-])[O-] Chemical compound CO.O.O.O.O.O.O.[N+](=O)([O-])[O-].[Zn+2].[N+](=O)([O-])[O-] ZJLKZLGZJOXUSX-UHFFFAOYSA-N 0.000 description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000011824 nuclear material Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of nano materials, and relates to a preparation method of a metal oxide@metal organic framework core-shell structure material, which has the following structural formula: ceO (CeO) 2 ZIF-8, wherein the core-shell material is prepared from CeO 2 Is core and ZIF-8 is shell. According to the invention, by increasing the concentration of the organic ligand, the ZIF-8 shell layer is coated on the surface of the cerium oxide under the regulation of nucleation kinetics. Meanwhile, the method of the invention has universality and can realize the preparation of different metal oxide particles @ ZIF-8 core-shell structure materials. The synthesis method has the characteristics of simple process, good repeatability, short reaction time, mild reaction conditions, large specific surface area, high porosity, excellent catalytic performance and the like, and has great application prospect.
Description
Technical Field
The invention belongs to the technical field of material preparation, and in particular relates to CeO 2 New synthesis method of ZIF-8 core-shell structure material.
Background
Composite materials have very important significance for basic research and industrial applications, and therefore, the structural design of composite materials has attracted attention from a large number of scientific researchers. Core-shell structure, nano-scale ordered assembly formed by coating one nano-material with another nano-material through chemical bond or other acting forceThe structure is a novel composite material design concept. The core-shell material integrates the properties of a single material, can realize a synergistic effect, and has been widely applied in the fields of energy storage and conversion, catalysis, electrochemistry and the like. Metal Organic Frameworks (MOFs) are porous materials formed by orderly assembling metal nodes and organic ligands, and have the advantages of high specific surface area, large porosity, good designability and the like. Thus, MOFs are ideal for encapsulating nanoparticle shell materials. Generally, in core-shell structures, the inner nanoparticle core is responsible for the main physicochemical properties such as catalytic, magnetic and luminescent properties, while the outer MOF shell layer serves as an adjunct for pre-enrichment, selectivity improvement and prevention of coagulation. Currently, significant progress has been made by researchers in the field of coating inorganic nanoparticles, such as noble metal nanoparticles and up-conversion nanoparticles, with MOFs as shell materials. However, the lack of synthetic methods remains a significant bottleneck limiting core-shell structural design. Furthermore, few reports have been made on metal oxide @ MOF core-shell materials, because MOFs shells have difficulty nucleating and growing directly on the surface of the metal oxide. The synthesis of metal oxide @ MOF core-shell materials is generally based on a self-templating or surface modification process. The self-templating method is simple and easy to implement, but it requires the core and shell materials to have the same metal center, which greatly limits the choice of materials. Surface modification methods often require further surface modification or time-consuming layer-by-layer modification of the shell material, and also complicate the shell-core interface. Therefore, it is of great importance to develop a simple and rapid synthetic strategy that can directly nucleate and grow MOF shells on the surface of metal oxides without the need for templates and further surface modifications. Increasing the concentration of the organic ligand can promote nucleation kinetics, reduce critical crystal nucleus size, and enable a large number of amorphous small crystal nuclei to be easily adsorbed on the surface of the nanoparticle cores, so that a continuous shell is grown. Based on the regulation of nucleation kinetics, we successfully prepared CeO under the condition of no template and no surface modification 2 The @ ZIF-8 core-shell structure material has important significance for synthesis and further application of the core-shell functional material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a simple and rapid preparation method without a template and further surface modification aiming at the defects of the existing metal oxide@metal organic framework core-shell structure material preparation technology. The invention uses CeO 2 The synthesis of @ ZIF-8 is illustrated by way of example as shown in FIG. 1 in which the process comprises the steps of: (a) CeO (CeO) 2 Preparation of nanoparticles: cerium nitrate hexahydrate is used as a raw material, polyvinylpyrrolidone is used as a stabilizer, the two substances are added into ethylene glycol, the mixture is stirred and dispersed to obtain a clear mixed solution, the clear mixed solution is transferred into a polytetrafluoroethylene autoclave for hydrothermal treatment, and then the mixture is cooled, centrifuged, washed and dried and then placed into a muffle furnace for calcination; (b) CeO (CeO) 2 Preparation of @ ZIF-8 core-shell structural material: dissolving a certain amount of 2-methylimidazole in methanol, adding cerium dioxide, performing ultrasonic dispersion, then adding a proper amount of a methanol solution of zinc nitrate hexahydrate into the mixed system, centrifuging, washing and drying;
the method has the main advantages that:
1) The reaction temperature is low and the reaction time is short. The cladding process related by the synthesis method is carried out at room temperature, and CeO can be obtained after 1 minute of reaction 2 The ZIF-8 core-shell structure material avoids the problems of overlong reaction time and the like when the core-shell structure material is synthesized in the past;
2) The preparation process is simple. The cladding process related by the synthesis method does not need a template or further surface modification of the nuclear material, and ZIF-8 can be used for preparing CeO by simply increasing the concentration of the organic ligand 2 Surface nucleation and growth of (a) to finally form a uniform and complete shell layer;
3) Universality. The synthesis method can be expanded to wrap different metal oxides such as Fe by ZIF-8 3 O 4 And ZnCo 2 O 4 ；
4) Practicality of materials. CeO prepared by the method 2 The specific surface area of the @ ZIF-8 is as high as 337.8 m 2 g -1 . CeO due to the synergistic effect of the core and the shell 2 ZIF-8 has excellent catalytic properties. At the position ofCeO under certain experimental conditions 2 The @ ZIF-8 core-shell material can efficiently catalyze the oxidation reaction of VOCs and can greatly promote the diffusion of gas.
Drawings
FIG. 1 CeO prepared according to the present invention 2 Schematic synthesis of ZIF-8 core-shell structure material.
FIG. 2 CeO prepared according to the present invention 2 And CeO 2 Characterization diagram (A) CeO of @ ZIF-8 core-shell structure material 2 Nanoparticle TEM image (B) CeO 2 CeO amplified by @ ZIF-8 TEM image (C) 2 A @ ZIF-8 TEM image; wherein: the concentration of zinc nitrate hexahydrate is 24mmol/L, the concentration of organic ligand is 2.436 mol/L, and the reaction time is 1 minute.
FIG. 3 CeO prepared according to the present invention at various reaction times 2 TEM image of ZIF-8 core-shell material (A) 1 min (B) 3 min (C) 30 min (D) 2 hours (E) 12 hours and (F) 24 hours. Wherein: the concentration of the zinc nitrate hexahydrate is 24mmol/L, and the concentration of the organic ligand is 2.436 mol/L.
FIG. 4 CeO prepared according to the invention at different organic ligand concentrations 2 TEM image of ZIF-8 core-shell structure material (A) 0.091 mol/L, (B) 0.305 mol/L, (C) 0.609 mol/L, (D) 1.218 mol/L, (E) 2.436 mol/L and (F) 4.872 mol/L. Wherein: the concentration of zinc nitrate hexahydrate was 24mmol/L and the reaction time was 1 minute.
FIG. 5 Fe prepared on the basis of the scheme of the present invention 3 O 4 ZIF-8 and ZnCo 2 O 4 SEM image of ZIF-8 core-shell structure material. (A) Fe (Fe) 3 O 4 , （B）Fe 3 O 4 @ZIF-8, （C）ZnCo 2 O 4 ，（D）ZnCo 2 O 4 @ ZIF-8. Wherein: the concentration of zinc nitrate hexahydrate is 24mmol/L, the concentration of organic ligand is 2.436 mol/L, and the reaction time is 1 minute.
Description of the embodiments
The example is implemented on the premise of the scheme of the invention and gives CeO 2 The preparation process of the @ ZIF-8 core-shell structure material is specifically.
Example 1
(1) 50 mg cerium oxide as a core material is placed into 10 mL of 2-methylimidazole methanol solution (2.436 mol/L) for ultrasonic dispersion for 30 minutes, then 10 mL zinc nitrate hexahydrate methanol solution (24 mmol/L) is added for reaction at room temperature for 1 minute;
(2) Centrifuging to collect a product, and washing the product with absolute ethanol for 3 times;
(3) The product was placed in a vacuum oven and dried for 12 hours, and the product synthesis scheme and TEM images are shown in figures 1 and 2.
Example 2
(1) 50 mg ceria as a core material was put into 10 mL of a methanol solution of 2-methylimidazole (2.436 mol/L), ultrasonic dispersion was performed for 30 minutes, and then 10 mL of a methanol solution of zinc nitrate hexahydrate (24 mmol/L) was added, and the reaction times at room temperature were 1 minute, 3 minutes, 30 minutes, 2 hours, 12 hours and 24 hours, respectively;
(2) Centrifuging to collect a product, and washing the product with absolute ethanol for 3 times;
(3) The product was placed in a vacuum oven and dried for 12 hours, and the product was synthesized as shown in FIG. 3.
Example 3
(1) 50 mg ceria as a core material was put into 10 mL of a methanol solution of 2-methylimidazole (the concentrations thereof are 0.091 mol/L, 0.305 mol/L, 0.609 mol/L, 1.218 mol/L, 2.436 mol/L and 4.872 mol/L, respectively), and subjected to ultrasonic dispersion for 30 minutes, followed by addition of a methanol solution of 10 mL zinc nitrate hexahydrate (24 mmol/L), and reaction at room temperature for 1 minute;
(2) Centrifuging to collect a product, and washing the product with absolute ethanol for 3 times;
(3) The product was placed in a vacuum oven and dried for 12 hours, and the product was synthesized as shown in FIG. 4.
Example 4
(1) 50 mg ferroferric oxide serving as a nuclear material is placed into 10 mL of 2-methylimidazole methanol solution (2.436 mol/L) for ultrasonic dispersion for 30 minutes, then 10 mL zinc nitrate hexahydrate methanol solution (24 mmol/L) is added for reaction at room temperature for 1 minute;
(2) Centrifuging to collect a product, and washing the product with absolute ethanol for 3 times;
(3) The product was placed in a vacuum oven and dried for 12 hours, and the SEM images of the product synthesis are shown in fig. 5A and 5B.
Example 5
(1) Putting 50 mg zinc oxide and cobalt oxide compound serving as a nuclear material into 10 mL of 2-methylimidazole methanol solution (2.436 mol/L), performing ultrasonic dispersion for 30 minutes, then adding 10 mL zinc nitrate hexahydrate methanol solution (24 mmol/L), and reacting for 1 minute at room temperature;
(2) Centrifuging to collect a product, and washing the product with absolute ethanol for 3 times;
(3) The product was placed in a vacuum oven and dried for 12 hours and the SEM images of the product synthesis are shown in fig. 5C and 5D.
Claims (8)
1. A preparation method of a core-shell structure material is characterized by comprising the following steps: synthesizing a core-shell structure material by a two-step method; the core-shell structure material is CeO 2 The steps of @ ZIF-8 are as follows: (a) CeO (CeO) 2 Preparation of nanoparticles: cerium nitrate hexahydrate is used as a raw material, polyvinylpyrrolidone is used as a stabilizer, the two substances are completely placed in ethylene glycol, a clear mixed solution is obtained by stirring and dispersing, and the clear mixed solution is transferred into a polytetrafluoroethylene autoclave for hydrothermal treatment, cooled, centrifuged, washed and dried and then placed in a muffle furnace for calcination; (b) CeO (CeO) 2 Preparation of @ ZIF-8 core-shell structural material: adding cerium oxide into a methanol solution of 2-methylimidazole, performing ultrasonic dispersion, adding a methanol solution of zinc nitrate hexahydrate into the mixed system, wherein the molar concentration ratio of the 2-methylimidazole to the zinc nitrate hexahydrate is 100:1, reacting for 1 min at room temperature, centrifuging, washing and drying to obtain CeO 2 ZIF-8 core-shell structural material.
2. The method for preparing a core-shell structure material according to claim 1, wherein the mass ratio of cerium nitrate hexahydrate to polyvinylpyrrolidone is 5:2.
3. The method of claim 1, wherein the hydrothermal temperature is 160 ℃ and the hydrothermal time is 8 h.
4. The method for preparing a core-shell structure material according to claim 1, wherein the product obtained after hydrothermal reaction is collected by centrifugation, washed with deionized water and absolute ethyl alcohol for 3 times, and dried in an air drying oven at 80 ℃ for 3 h.
5. The method for preparing a core-shell structure material according to claim 1, wherein the calcination temperature is 300 ℃ and the calcination time is 1 h.
6. The method for preparing a core-shell structured material according to claim 1, wherein the molar concentration ratio of 2-methylimidazole to zinc nitrate hexahydrate is 100:1.
7. The method for preparing a core-shell structure material according to claim 1, wherein the ultrasonic dispersion time is 30 min.
8. The method for preparing a core-shell structure material according to claim 1, wherein the reaction product is collected by centrifugation, washed 3 times with absolute ethyl alcohol, and the washed material is placed in a vacuum drying oven for overnight drying.
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