CN115028847B - CoNi alloy MOF porous material and preparation and application thereof - Google Patents
CoNi alloy MOF porous material and preparation and application thereof Download PDFInfo
- Publication number
- CN115028847B CN115028847B CN202210532317.4A CN202210532317A CN115028847B CN 115028847 B CN115028847 B CN 115028847B CN 202210532317 A CN202210532317 A CN 202210532317A CN 115028847 B CN115028847 B CN 115028847B
- Authority
- CN
- China
- Prior art keywords
- porous material
- mof
- coni alloy
- acetate tetrahydrate
- mixed solution
- 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
- 239000000956 alloy Substances 0.000 title claims abstract description 48
- 229910002441 CoNi Inorganic materials 0.000 title claims abstract description 44
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 44
- 239000011148 porous material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 claims abstract description 12
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 10
- 230000009467 reduction Effects 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 12
- 238000005054 agglomeration Methods 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 3
- 239000012621 metal-organic framework Substances 0.000 description 44
- 238000001000 micrograph Methods 0.000 description 7
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 6
- 229920003081 Povidone K 30 Polymers 0.000 description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000004627 transmission electron microscopy Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- UNIBAJHMJGXVHL-UHFFFAOYSA-N 3-phenylbenzene-1,2,4,5-tetracarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C(C=2C=CC=CC=2)=C1C(O)=O UNIBAJHMJGXVHL-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012216 imaging agent Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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
- Y02E60/50—Fuel cells
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a CoNi alloy MOF porous material and preparation and application thereof, wherein the porous material is prepared by the following steps: (1) Adding cobalt acetate tetrahydrate, nickel acetate tetrahydrate and an organic connecting agent into absolute ethyl alcohol, stirring and dissolving to obtain a transparent mixed solution; (2) Transferring the mixed solution into a reaction kettle, performing hydrothermal reaction, washing and drying the obtained reaction product to obtain precursor powder; (3) And (3) placing the precursor powder in an inert atmosphere for high-temperature reduction, and then cooling to room temperature to obtain a target product. The invention can obtain product particles with good dispersibility and uniform morphology and particle size, can still keep the original morphology completely after high-temperature reduction in nitrogen atmosphere, and has no obvious agglomeration phenomenon. Meanwhile, the CoNi alloy MOF porous material has excellent performances in the fields of microwave absorption, catalysis, sensors and the like.
Description
Technical Field
The invention belongs to the technical field of functional materials, and relates to a CoNi alloy MOF porous material, and preparation and application thereof.
Background
Metal-organic framework (MOF) materials are self-assembled by Metal ions and organic ligands through coordination bonds, and are exciting crystalline porous materials in novel materials. The MOF material has a highly regular topological structure and periodic network channels, and is widely applied to the fields of gas storage, catalysis, electronic conduction materials, sensors, electromagnetic interference resistance and the like. However, the pure MOF has lower conductivity and dielectric properties, and cannot meet the requirement of electromagnetic impedance matching; and MOF materials are often susceptible to agglomeration and cannot fully expose their reactive sites, resulting in limited applications. In order to improve the conductivity of the MOF and solve the agglomeration phenomenon, thermal annealing of the precursor of the MOF is one of the strategies for obtaining porous metal carbon-based nanostructure materials, and by selecting different metal sources and organic linkers, the final composition of the MOF derivative can be effectively controlled, and many efforts have been made to prove that the MOF is an ideal template for manufacturing multifunctional inorganic functional materials thanks to the diversified composition and good chemical uniformity of the MOF.
The CoNi alloy is widely studied due to the special physical and chemical properties, and is suitable for different fields such as microwave absorption, catalysis, hydrogen storage, biomedical micro devices, magnetic resonance imaging agents and the like. The application of the CoNi alloy is affected by both compositional and morphological factors, as differences in composition and morphology will result in changes in the inherent magnetic moment, permeability, and magnetism of the alloy material. The CoNi alloy with a single component has the phenomena of high density, easy oxidation, easy agglomeration and the like. Therefore, the electromagnetic wave absorber has the defect of single electromagnetic loss mechanism when the electromagnetic wave absorber interacts with electromagnetic waves, and the problems of attenuation and impedance matching are difficult to simultaneously meet, so that the wave absorbing performance is not ideal. When used as a catalyst, agglomeration of the CoNi alloy results in a substantial reduction of the catalyst active sites, thereby reducing its catalytic activity. Therefore, if the special-performance material is used for modifying the morphology or the character, the specific surface area, the chemical stability, the electron conduction rate and the like of the alloy material can be improved, and the application performance of the alloy material can be further effectively enhanced.
Disclosure of Invention
The invention aims to provide a CoNi alloy MOF porous material, and preparation and application thereof.
The aim of the invention can be achieved by the following technical scheme:
one of the technical schemes of the invention provides a preparation method of a CoNi alloy MOF porous material, which comprises the following steps:
(1) Adding cobalt acetate tetrahydrate, nickel acetate tetrahydrate and an organic connecting agent into absolute ethyl alcohol, stirring and dissolving to obtain a transparent mixed solution;
(2) Transferring the mixed solution into a reaction kettle, performing hydrothermal reaction, washing and drying the obtained reaction product to obtain precursor powder;
(3) And (3) placing the precursor powder in an inert atmosphere for high-temperature reduction, and then cooling to room temperature to obtain a target product.
Further, in the step (1), the organic linking agent is any one of polyvinylpyrrolidone (PVP-K30), 2-methylimidazole, terephthalic acid, 3', 5' -biphenyltetracarboxylic acid.
In the step (1), the mass ratio of the cobalt acetate tetrahydrate, the nickel acetate tetrahydrate and the organic connecting agent is (1-6): (1-3): (3-23).
Further, in the step (1), the addition amount of the absolute ethyl alcohol satisfies the following conditions: ni in the mixed solution 2+ The concentration is 1-4 g/L.
In the step (2), the temperature of the hydrothermal reaction is 60-130 ℃ and the time is 5-12 h.
Further, in the step (2), the washing process is as follows: and adopting deionized water and ethanol to centrifugally wash for a plurality of times at 8000-10000 rpm.
Further, in the step (2), the drying process specifically includes: vacuum drying at 60-80 deg.c.
Further, in the step (3), the high-temperature reduction temperature is 400-600 ℃ and the time is 1-3h.
Further, the inert atmosphere is a nitrogen atmosphere.
The second technical scheme of the invention provides a CoNi alloy MOF porous material which is prepared by adopting the preparation method, and is characterized in that the CoNi alloy MOF porous material is in a cube fluffy shape, the size is 0.4-0.6 mu m, and the surface of the CoNi alloy MOF porous material is distributed with a regular and ordered pore structure.
The third technical scheme of the invention provides application of the CoNi alloy MOF porous material, and the CoNi alloy MOF porous material is used in the fields of microwave absorption, catalysis or sensors.
The method synthesizes the CoNi-MOF precursor by adopting a high-efficiency and simple solvothermal reaction method, and can obtain product particles with good dispersibility and uniform morphology particle size by simply adjusting the types of the organic connecting agents, and the product particles can still maintain the original morphology completely after being reduced at high temperature in nitrogen atmosphere without obvious agglomeration phenomenon. Meanwhile, the CoNi alloy MOF porous material has excellent performances in the fields of microwave absorption, catalysis, sensors and the like.
Compared with the prior art, the preparation method of the CoNi alloy MOF porous material is simple and convenient, easy to operate, and relatively mild and easy to control the preparation conditions. The obtained CoNi alloy MOF is cubic and is distributed with regular pore channels, so that the CoNi alloy MOF has larger specific surface area and high porosity, and has attractive application prospects in the aspects of gas adsorption, biosensing, catalysis, electromagnetic interference and the like. The method can effectively solve the surface agglomeration phenomenon by adjusting the organic connecting agent for forming MOF, thereby fully exposing the reactive sites and enhancing the application capability of the reactive sites.
Drawings
Fig. 1 is a scanning electron microscope image and a transmission electron microscope image of example 1: (a1) Example 1-scanning electron microscopy of a CoNi alloy MOF precursor; (a2) Example 1-high power scanning electron microscope image and schematic outline of CoNi alloy MOF precursor; (b1) Example 1-scanning electron microscopy of a CoNi alloy MOF porous material; (b2) Example 1-high power scanning electron microscope image of CoNi alloy MOF porous material; (c1) Example 1-transmission electron microscopy of a CoNi alloy MOF porous material; (c2) Example 1-high power transmission electron microscopy of CoNi alloy MOF porous materials.
FIG. 2 is a transmission electron microscope image of examples 2-4: (a) Example 2-transmission electron microscopy of a CoNi alloy MOF precursor; (b) Example 3-transmission electron microscopy of a CoNi alloy MOF precursor; (c) Example 4-transmission electron microscopy of a CoNi alloy MOF precursor.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
Raw materials sold or conventional treatment techniques.
Example 1:
preparation of a CoNi alloy MOF porous material:
firstly, 0.84g of cobalt acetate tetrahydrate, 0.42g of nickel acetate tetrahydrate and 3g of PVP-K30 are respectively weighed and added into 160mL of absolute ethyl alcohol, and the mixture is fully stirred and dissolved to obtain a transparent mixed solution.
Next, the transparent solution was transferred to a Teflon lined stainless steel hot-reactor and heated at 90℃for 6 hours. After cooling to room temperature, centrifugal washing is carried out for a plurality of times by deionized water, vacuum drying is carried out at 70 ℃, and the CoNi alloy MOF precursor powder is obtained after collection.
Finally, the precursor powder is placed in a porcelain boat and is placed in a tube furnace, and under the protection of inert gas nitrogen, the temperature is 2 ℃/min -1 The temperature is increased to 500 ℃, the reaction is carried out for 2 hours at high temperature, and after the reaction is naturally cooled to room temperature, the CoNi alloy MOF porous material is in a cube fluffy shape, the size is 0.4-0.6 mu m, and the surface of the porous material is distributed with a regular and ordered pore structure.
Example 2:
compared to example 1, the vast majority are identical, except in this example: the organic linking agent used is terephthalic acid.
Example 3:
compared to example 1, the vast majority are identical, except in this example: the organic linking agent used was 2-methylimidazole.
Example 4:
compared to example 1, the vast majority are identical, except in this example: the organic linking agent used is 3, 5' -biphenyltetracarboxylic acid.
The microscopic morphology of the morphology-controllable CoNi alloy MOF porous material in the above example was characterized by using a scanning electron microscope (SEM, hitachi FE-SEM S-4800), and a powder sample was coated on the surface of the conductive paste for testing. The microstructure information of a series of alloy materials is characterized by a transmission electron microscope (TEM, JEOL JEM-2100F), and powder samples are subjected to ultrasonic dispersion in ethanol and then are dripped on a carbon-supported copper mesh for drying and testing.
FIG. 1 is a scanning electron microscope image and a transmission electron microscope image of example 1, wherein the CoNi alloy MOF precursor synthesized in example 1 is a cube with pyramid-shaped ends, the length is about 1.5-3 μm, the side length is 0.4-0.6 μm, and the surface is smooth. The particle size distribution of the sample is uniform and the dispersibility is good. The morphology and the size of the CoNi alloy MOF after high-temperature reduction are not changed greatly, but the surface is rough, a large number of ordered pore channels are distributed inside, the particle size distribution of the whole sample is uniform, and the dispersibility is good. When the composite material is used as a microwave absorber, the effective wave absorption frequency band is within the range of 10-14GHz, and the thickness is 2.6mm, the reflection loss is minimized to be-53 dB.
Compared with example 1, the morphology of the CoNi alloy MOF precursor changed greatly due to the changed kind of the organic linking agent. As shown in FIG. 2, when the organic binder was terephthalic acid, the CoNi alloy MOF precursor was square, with a side length of about 0.5 μm, smooth surface, and a relatively uniform sample particle size, but a relatively severe agglomeration. When the organic connecting agent is 2-methylimidazole, the CoNi alloy MOF precursor is spherical, the particle size is about 0.2-0.3 mu m, and the sample particle size is good in uniformity and dispersibility, but still has agglomeration. When the organic connecting agent is 3, 5' -biphenyl tetracarboxylic acid, the CoNi alloy MOF precursor is in a cube shape, the particle size distribution and the dispersibility of the sample are poor, and the agglomeration phenomenon is serious. Thus, the choice of the organic linker species has a significant impact on the morphology, particle size and dispersibility of the sample.
Example 5:
compared to example 1, the vast majority are identical, except in this example: the mass ratio of the added amounts of cobalt acetate tetrahydrate, nickel acetate tetrahydrate and PVP-K30 is 1.26g:0.42g:4.2g, ni 2+ The concentration was 1.0g/L.
Example 6:
compared to example 1, the vast majority are identical, except in this example: the mass ratio of the added amounts of cobalt acetate tetrahydrate, nickel acetate tetrahydrate and PVP-K30 is 2.1g:0.84g:6.3g, ni 2+ The concentration was 2.6g/L.
Example 7:
compared to example 1, the vast majority are identical, except in this example: the mass ratio of the added amounts of cobalt acetate tetrahydrate, nickel acetate tetrahydrate and PVP-K30 is 2.52g:1.26g:7.56g, ni 2+ The concentration was 3.0g/L.
Example 8:
and implementationIn comparison to example 1, the vast majority are identical, except in this example: the mass ratio of the added amounts of cobalt acetate tetrahydrate, nickel acetate tetrahydrate and PVP-K30 is 1.68g:1.26g:9.66g, ni 2+ The concentration was 4.0g/L.
Example 9:
the reaction time was 12 hours except that the temperature of the hydrothermal reaction was adjusted to 60℃in this example.
Example 10:
the reaction time was 9 hours except that the temperature of the hydrothermal reaction was adjusted to 80℃in this example.
Example 11:
compared to example 1, the vast majority are identical, except in this example: the temperature of the hydrothermal reaction was adjusted to 100℃and the reaction time was 6 hours.
Example 12:
compared to example 1, the vast majority are identical, except in this example: the temperature of the hydrothermal reaction was adjusted to 130℃and the reaction time was 5 hours.
Example 13:
most of the same as in example 1 except that in this example, the temperature of the high temperature reduction was adjusted to calcine at 400℃for 3 hours.
Example 14:
most of the same as in example 1 except that in this example, the temperature of the high temperature reduction was adjusted to calcine at 600℃for 1h.
Example 15:
compared to example 1, the vast majority are identical, except in this example: the mass of the cobalt acetate tetrahydrate and the mass of the organic connecting agent are adjusted so that the mass ratio of the cobalt acetate tetrahydrate to the nickel acetate tetrahydrate to the organic connecting agent is 1:1:3.
example 16:
compared to example 1, the vast majority are identical, except in this example: the mass of the cobalt acetate tetrahydrate and the mass of the organic connecting agent are adjusted so that the mass ratio of the cobalt acetate tetrahydrate to the nickel acetate tetrahydrate to the organic connecting agent is 6:3:23.
the previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (3)
1. The preparation method of the CoNi alloy MOF porous material is characterized by comprising the following steps of:
(1) Adding cobalt acetate tetrahydrate, nickel acetate tetrahydrate and an organic connecting agent into absolute ethyl alcohol, stirring and dissolving to obtain a transparent mixed solution;
(2) Transferring the mixed solution into a reaction kettle, performing hydrothermal reaction, washing and drying the obtained reaction product to obtain precursor powder;
(3) Placing the precursor powder in an inert atmosphere for high-temperature reduction, and then cooling to room temperature to obtain a target product;
in the step (1), the organic connecting agent is polyvinylpyrrolidone;
in the step (1), the mass ratio of the cobalt acetate tetrahydrate, the nickel acetate tetrahydrate and the organic connecting agent is (1-6): (1-3): (3-23);
in the step (1), the addition amount of the absolute ethyl alcohol satisfies the following conditions: ni in the mixed solution 2+ The concentration is 1-4 g/L;
in the step (2), the temperature of the hydrothermal reaction is 60-130 ℃ and the time is 5-12 h;
in the step (3), the high-temperature reduction temperature is 400-600 ℃ and the time is 1-3h;
in the step (2), the washing process is as follows: centrifugal washing with deionized water and ethanol at 8000-10000rpm for several times;
in the step (2), the drying process is specifically: vacuum drying at 60-80 deg.c.
2. The CoNi alloy MOF porous material prepared by the preparation method of claim 1, which is characterized in that the CoNi alloy MOF porous material is in a cube fluffy shape, has a size of 0.4-0.6 mu m, and has a regular and ordered pore structure distributed on the surface.
3. The use of a CoNi alloy MOF porous material according to claim 2, wherein the CoNi alloy MOF porous material is used in the fields of microwave absorption, catalysis or sensors.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210532317.4A CN115028847B (en) | 2022-05-09 | 2022-05-09 | CoNi alloy MOF porous material and preparation and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210532317.4A CN115028847B (en) | 2022-05-09 | 2022-05-09 | CoNi alloy MOF porous material and preparation and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115028847A CN115028847A (en) | 2022-09-09 |
| CN115028847B true CN115028847B (en) | 2024-01-26 |
Family
ID=83121711
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210532317.4A Active CN115028847B (en) | 2022-05-09 | 2022-05-09 | CoNi alloy MOF porous material and preparation and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115028847B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115725084B (en) * | 2022-11-22 | 2024-05-24 | 浙江理工大学 | Flake nickel-cobalt bimetallic organic framework crystal material and preparation method thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610913A (en) * | 2015-03-04 | 2015-05-13 | 南京航空航天大学 | Preparation method of microwave absorbing material taking MOFs molecular structure as template |
| CN108417845A (en) * | 2018-03-07 | 2018-08-17 | 上海应用技术大学 | A kind of porous carbon composite and preparation method thereof containing cobalt and nickel |
| CN109705808A (en) * | 2019-02-02 | 2019-05-03 | 南京航空航天大学 | A kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material and preparation method thereof |
| CN112449568A (en) * | 2020-12-23 | 2021-03-05 | 南昌航空大学 | Method for preparing hollow cobalt-nickel alloy/porous carbon composite wave-absorbing material |
| CN112920773A (en) * | 2021-01-29 | 2021-06-08 | 安徽理工大学 | Tri-metal organic framework derived hollow core-shell NiCo alloy @ C ultrathin wave absorbing agent and preparation method thereof |
| CN113174143A (en) * | 2021-06-10 | 2021-07-27 | 鲁东大学 | Metal organic framework/multilayer carbon composite wave-absorbing material and preparation method thereof |
| CN113248725A (en) * | 2021-05-13 | 2021-08-13 | 青岛理工大学 | Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material |
| CN113999651A (en) * | 2021-11-18 | 2022-02-01 | 北京化工大学 | Nickel-cobalt dual-ligand metal-organic framework material and preparation method and application thereof |
| CN114390884A (en) * | 2022-01-27 | 2022-04-22 | 合肥工业大学 | Light iron-nickel alloy based magnetic composite wave-absorbing material and preparation method thereof |
| CN114449877A (en) * | 2021-11-06 | 2022-05-06 | 贵州大学 | Core-shell Ni/Co alloy @ nitrogen-doped carbon-based wave-absorbing composite material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3728411B2 (en) * | 2001-09-18 | 2005-12-21 | ソニー株式会社 | Method for producing magnetic particle, magnetic particle and magnetic material |
-
2022
- 2022-05-09 CN CN202210532317.4A patent/CN115028847B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610913A (en) * | 2015-03-04 | 2015-05-13 | 南京航空航天大学 | Preparation method of microwave absorbing material taking MOFs molecular structure as template |
| CN108417845A (en) * | 2018-03-07 | 2018-08-17 | 上海应用技术大学 | A kind of porous carbon composite and preparation method thereof containing cobalt and nickel |
| CN109705808A (en) * | 2019-02-02 | 2019-05-03 | 南京航空航天大学 | A kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material and preparation method thereof |
| CN112449568A (en) * | 2020-12-23 | 2021-03-05 | 南昌航空大学 | Method for preparing hollow cobalt-nickel alloy/porous carbon composite wave-absorbing material |
| CN112920773A (en) * | 2021-01-29 | 2021-06-08 | 安徽理工大学 | Tri-metal organic framework derived hollow core-shell NiCo alloy @ C ultrathin wave absorbing agent and preparation method thereof |
| CN113248725A (en) * | 2021-05-13 | 2021-08-13 | 青岛理工大学 | Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material |
| CN113174143A (en) * | 2021-06-10 | 2021-07-27 | 鲁东大学 | Metal organic framework/multilayer carbon composite wave-absorbing material and preparation method thereof |
| CN114449877A (en) * | 2021-11-06 | 2022-05-06 | 贵州大学 | Core-shell Ni/Co alloy @ nitrogen-doped carbon-based wave-absorbing composite material and preparation method thereof |
| CN113999651A (en) * | 2021-11-18 | 2022-02-01 | 北京化工大学 | Nickel-cobalt dual-ligand metal-organic framework material and preparation method and application thereof |
| CN114390884A (en) * | 2022-01-27 | 2022-04-22 | 合肥工业大学 | Light iron-nickel alloy based magnetic composite wave-absorbing material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| Cuihua An等.Novel three-dimensional NiCo2O4 hierarchitectures: solvothermal synthesis and electrochemical properties.《CrystEngComm》.2013,第16卷第385–392页. * |
| Hongjing Wu等.NiCo2O4 constructed by different dimensions of building blocks with superior electromagnetic wave absorption performance.《Composites Part B》.2019,第182卷第1-10页. * |
| 王瑞丽.碳基复合材料的制备及其微波吸收性能研究.《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》.2022,(第1期),第B020-387页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115028847A (en) | 2022-09-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112961650B (en) | Three-metal organic framework derived iron-nickel alloy/porous carbon ultrathin wave absorber and preparation method thereof | |
| CN112251193A (en) | Composite wave-absorbing material based on MXene and metal organic framework and preparation method and application thereof | |
| CN112087939B (en) | FeCoNi @ C/carbon nanotube magnetic composite wave-absorbing material and application | |
| CN113248725A (en) | Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material | |
| CN112143460A (en) | Composite wave-absorbing material based on metal organic framework material and preparation method and application thereof | |
| CN115028847B (en) | CoNi alloy MOF porous material and preparation and application thereof | |
| CN115491177A (en) | MOF-derived carbon-based magnetic nanocomposite electromagnetic wave absorption material and preparation method thereof | |
| CN110669474B (en) | NiCo/C @ CNT double-conductive-network hierarchical structure material as well as preparation method and application thereof | |
| CN113285243A (en) | Covalent organic framework composite material and preparation method and application thereof | |
| CN109652013B (en) | Composite microwave absorbent | |
| CN114845538A (en) | Magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide and preparation method thereof | |
| CN114501966A (en) | Wave-absorbing material with zero-dimension/one-dimension/two-dimension composite nanostructure and preparation method and application thereof | |
| CN115215325B (en) | Composite electromagnetic wave absorbing material and preparation method and application thereof | |
| CN109251728B (en) | Wave-absorbing material and preparation method thereof | |
| CN115101736B (en) | Three-dimensional NiPc-NiFe@Ti 3 C 2 T x Preparation method of MXene composite material, and product and application thereof | |
| CN114614272A (en) | MXene/Co/C composite wave-absorbing material derived from MOF and preparation method thereof | |
| CN113415796B (en) | Application of Cu/C composite material as electromagnetic wave absorption material | |
| CN113708085B (en) | Preparation method of nano porous carbon coated magnetic nanoparticle compound | |
| CN112280533B (en) | Preparation method of ternary composite wave-absorbing material with hollow structure | |
| CN114206091A (en) | CoFe/C-CNT wave-absorbing material and preparation process and application thereof | |
| CN114479762A (en) | Magnetic metal/metal oxide/carbon nano composite material, preparation method and application thereof | |
| CN115322744B (en) | Nickel-carbon composite material for absorbing electromagnetic waves and preparation method thereof | |
| CN115740436B (en) | One-dimensional core-shell structure carbon-coated ferromagnetic nanowire, preparation method and application thereof | |
| CN112811422A (en) | Biomass core-shell wave-absorbing material, preparation method and application thereof | |
| CN115318210B (en) | Preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding |
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 |