CN115028847B - CoNi alloy MOF porous material and preparation and application thereof - Google Patents

CoNi alloy MOF porous material and preparation and application thereof Download PDF

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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
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porous material
mof
coni alloy
acetate tetrahydrate
mixed solution
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CN115028847A (en
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车仁超
李莹
罗开成
张捷
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Fudan University
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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

CoNi alloy MOF porous material and preparation and application thereof
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.
CN202210532317.4A 2022-05-09 2022-05-09 CoNi alloy MOF porous material and preparation and application thereof Active CN115028847B (en)

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