CN110894298B - Preparation method of MOFs nano material and derivative thereof - Google Patents
Preparation method of MOFs nano material and derivative thereof Download PDFInfo
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Abstract
The invention belongs to the field of new materials and synthetic chemistry, and provides a preparation method of MOFs nano-materials, which comprises the following steps: s1, uniformly mixing a metal ion precursor and 2-methylimidazole in an alcohol solution to obtain a solution A; s2, adding a pyridine organic ligand methanol solution into the solution A, and uniformly stirring to obtain a solution B; and S3, placing the solution B in a reaction kettle, and carrying out hydrothermal reaction to obtain the MOFs material. The invention also provides a preparation method of the MOFs derivative nano material, and the prepared MOFs material is annealed to obtain the MOFs derivative nano material. The preparation process is convenient and fast, the repeatability is high, the controllability is strong, the obtained MOFs have the advantages of a two-dimensional nanosheet structure, a large specific surface area and the like, the derivative of the MOFs is a secondary particle nano structure assembled by nano particles, the derivative has the advantages of large specific surface area, high porosity, high conductivity and the like, and the MOFs have large application potential in the field of electrochemistry.
Description
Technical Field
The invention relates to the field of new materials and synthetic chemistry, in particular to a preparation method of a novel two-dimensional organic-inorganic network Structure (MOFs) nano material and a derivative thereof.
Background
The nanometer technology is advancing forward in depth level at present through the development process of more than twenty years. In the early 90 s of the 20 th century, pure inorganic or organic nanomaterials were of interest. In the last decade, research on organic-inorganic networks (MOFs) nanomaterials has been vigorously developed. Compared with pure inorganic or organic nano materials, the organic-inorganic network Structure (MOFs) nano material has the structure that ligands and metal ions are alternately arranged according to a certain period, and the size of an internal pore structure or an internal specific surface area can be changed by regulating the types and the sizes of units of the ligands and the metal ions, so that the adsorption capacity of the nano material on guest molecules and an electronic structure can be regulated. Compared with pure organic matter nano particles, the organic-inorganic net-shaped nano structure has better thermal stability and higher mechanical strength, and is beneficial to processing and repeated use of materials. The material has adjustable structure and function, large specific surface area and highly ordered pores, and is widely applied to the fields of gas storage, separation, catalysis, sensing, photoelectricity and the like.
At present, there are many methods for preparing organic-inorganic network Structure (MOFs) nanomaterials, which can be generally classified into: a solvent thermal method, an ultrasonic method, a microblog-assisted synthesis method, a reverse microemulsion method, a chemical precipitation method, a template method and the like. Different preparation methods and experimental conditions can affect the coordination mode of metal and organic ligand, crystal nucleation growth and self-assembly process, thereby obtaining products with different structures and appearances. Currently, the solvothermal method is the most common method for preparing two-dimensional MOFs materials. The annealing of MOFs materials under certain conditions to prepare MOFs derivative nano materials becomes a new research hotspot.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a preparation method of MOFs nano material and derivatives thereof, which solves the problem that the MOFs nano material is difficult to prepare.
The invention provides a preparation method of MOFs nano material, which comprises the following steps:
s1, uniformly mixing a metal ion precursor and 2-methylimidazole in an alcohol solution to obtain a solution A;
s2, adding a pyridine organic ligand methanol solution into the solution A, and uniformly stirring to obtain a solution B;
and S3, placing the solution B in a reaction kettle, and carrying out hydrothermal reaction to obtain the MOFs material.
In an embodiment of the invention, in the step S1, the metal ion precursor is at least one of cobalt nitrate, nickel nitrate and iron nitrate, and the alcohol solution is at least one of methanol, ethanol and isopropanol.
In one embodiment of the present invention, in the step S2, the novel pyridine organic ligand is represented by formula (I):
wherein R comprises amino (-NH2), cyano (-CN) or dimethylamino (-N (CH3) 2).
In an embodiment of the invention, in the step S3, the hydrothermal reaction temperature is 100 to 140 ℃ and the reaction time is 5 to 8 hours.
In one embodiment of the invention, the molar ratio of the metal ion precursor, the 2-methylimidazole and the pyridine organic ligand is 1:1:1 to 2:0.5: 3.
In one embodiment of the present invention, the mixing and stirring time for obtaining the solution a is 3 to 5 minutes, and the mixing and stirring time for obtaining the solution B is 45 to 50 minutes.
In one embodiment of the invention, the obtained MOFs material is a two-dimensional nanosheet structure, the size is 180-800nm, and the thickness size is not more than 30 nm.
The invention also provides a preparation method of the MOFs derivative nano material, and the MOFs material prepared by any one of the methods is annealed to obtain the MOFs derivative nano material.
In one embodiment of the invention, the annealing temperature is 550-650 ℃, the heating rate is 2-5 ℃/min, the heat preservation time is 1-6 h, and the calcining atmosphere is argon.
In one embodiment of the invention, the MOFs derivative nanometer material is a secondary particle assembled by nanometer particles, the size of the nanometer particle is 50-300nm, and the size of the secondary particle is 1.5-10 μm
The implementation of the invention has the following beneficial effects: the invention provides a preparation method of a novel two-dimensional organic-inorganic network Structure (MOFs) nano material and a derivative thereof, which comprises the steps of firstly preparing a precursor of metal ions and 2-methylimidazole, enabling each metal ion to form coordinate bonds with nitrogen atoms on 4 dimethylimidazoles in a two-dimensional xy plane respectively, forming a chessboard-shaped layered structure at the moment, adding a certain proportion of novel pyridine organic ligands into an alcohol solution of the precursor, stirring for a certain time, transferring to a high-pressure reaction kettle, and carrying out hydrothermal reaction for a certain time. At the moment, the metal ions and nitrogen atoms in 2 pyridine organic ligands form coordination bonds in the z direction, and layers are connected together to serve as supports, so that a regular two-dimensional nanosheet structure is finally formed. And after the reaction kettle is cooled, centrifugally drying the product to obtain solid powder, namely the MOFs material. And then, obtaining the derivative nano material of the MOFs material through a certain calcination process. The preparation process is convenient and fast, the repeatability is high, the controllability is strong, the obtained MOFs have the advantages of a two-dimensional nanosheet structure, a large specific surface area and the like, the derivative of the MOFs is a secondary particle nano structure assembled by nano particles, the derivative has the advantages of large specific surface area, high porosity, high conductivity and the like, and the MOFs have large application potential in the field of electrochemistry.
Drawings
FIG. 1 is a flow chart of a method for preparing novel two-dimensional organic-inorganic network Structure (MOFs) nano-materials and derivatives thereof provided by the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nano-materials synthesized in example 1 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nanomaterial derivative synthesized in example 1 of the present invention;
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nano-materials synthesized in example 4 of the present invention;
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nanomaterial derivative synthesized in example 4 of the present invention;
FIG. 6 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nano-materials synthesized in example 7 of the present invention;
FIG. 7 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nanomaterial derivative synthesized in example 7 of the present invention;
FIG. 8 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nano-materials synthesized in example 10 of the present invention;
FIG. 9 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nanomaterial derivative synthesized in example 10 of the present invention;
FIG. 10 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nano-materials synthesized in example 12 of the present invention;
FIG. 11 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network Structure (MOFs) nanomaterial derivative synthesized in example 12 of the present invention;
FIG. 12 is a Scanning Electron Microscope (SEM) photograph of novel two-dimensional organic-inorganic network (MOFs) materials synthesized in comparative example 1 according to the present invention;
FIG. 13 is a Scanning Electron Microscope (SEM) photograph of the novel two-dimensional organic-inorganic network (MOFs) material derivative synthesized by comparative example 2 of the present invention.
Detailed Description
The technical solution of the present invention is described in detail below with reference to the accompanying drawings and specific embodiments, but the description of the embodiments is only a part of the embodiments of the present invention, and most of them are not limited thereto.
Example 1
In this embodiment, the preparation method of the MOFs nanomaterial and the derivative thereof is as follows:
1.1, mixing 10mol of metal ion precursor cobalt nitrate and 10mol of 2-methylimidazole in a methanol solution, and stirring for 3 minutes to obtain a solution A; adding 10mol of 4-aminopyridine organic ligand methanol solution into the solution A, and stirring for 45 minutes to obtain solution B;
1.2, placing the solution B in a reaction kettle, reacting for 5 hours at 100 ℃, and finally, carrying out centrifugal separation and drying on a product to obtain the MOFs material;
1.3 annealing the MOFs material at 550 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 1h, and the calcining atmosphere is argon, so that the MOFs derivative nano material is obtained.
FIG. 2 is a Scanning Electron Microscope (SEM) image of the MOFs materials. As can be seen from the figure, the obtained MOFs have a two-dimensional nanosheet structure, the width dimension of the nanosheet is 250-600nm, and the thickness dimension does not exceed 20 nm; FIG. 3 is a Scanning Electron Microscope (SEM) image of the above MOFs derivative nano-material, from which it can be seen that the obtained MOFs derivative is a secondary particle structure composed of nanoparticles with a particle size of 100-300nm and a secondary particle size of 2.5-6 μm.
Example 2
The preparation method is the same as example 1, except that: the metal ion precursor is nickel nitrate, the alcohol solution is ethanol, and the pyridine organic ligand is 4-dimethylamino pyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 1, the width of the nanosheet is 250-650nm, and the thickness of the nanosheet is no more than 20 nm; the morphology of the secondary particles of the MOFs derivatives is the same as that of the secondary particles in the embodiment 1, the particle size of the nanoparticles is 100-300nm, and the size of the secondary particles is 2.5-6 μm.
Example 3
The preparation method is the same as example 1, except that: the metal ion precursor is ferric nitrate, the alcohol solution is isopropanol, and the pyridine organic ligand is 4-cyanopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 1, the width of the nanosheet is 300-650nm, and the thickness of the nanosheet is no more than 20 nm; the morphology of the secondary particles of the MOFs derivatives is the same as that of the secondary particles in the embodiment 1, the particle size of the nanoparticles is 100-300nm, and the size of the secondary particles is 2.5-6 μm.
Example 4
In this embodiment, the preparation method of the MOFs nanomaterial and the derivative thereof is as follows:
1.1, mixing 20mol of metal ion precursor nickel nitrate and 5mol of 2-methylimidazole in a methanol solution, and stirring for 5 minutes to obtain a solution A; adding 30mol of 4-cyanopyridine organic ligand methanol solution into the solution A, and stirring for 50 minutes to obtain a solution B;
1.2, placing the solution B in a reaction kettle, reacting for 8 hours at 140 ℃, and finally, carrying out centrifugal separation and drying on a product to obtain the MOFs material;
1.3 annealing the MOFs material at 650 ℃, wherein the heating rate is 5 ℃/min, the heat preservation time is 6h, and the calcining atmosphere is argon, so as to obtain the MOFs derivative nano material.
FIG. 4 is a Scanning Electron Microscope (SEM) image of the MOFs materials. As can be seen from the figure, the obtained MOFs has a two-dimensional nanosheet structure, the width dimension of the nanosheet is 180-250nm, and the thickness dimension does not exceed 25 nm; FIG. 5 is a Scanning Electron Microscope (SEM) image of the MOFs derivative nano-material, and it can be seen from the image that the obtained MOFs derivative material is a secondary particle structure composed of nanoparticles, the surface morphology of the material is uniform and regular, the particle size of the nanoparticles is 100-250nm, and the secondary particle size is 4.5-10 μm.
Example 5
The preparation method is the same as example 4, except that: the metal ion precursor is cobalt nitrate, the alcohol solution is ethanol, and the pyridine organic ligand is 4-dimethylamino pyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 4, the width of the nanosheet is 200-250nm, and the thickness of the nanosheet is not more than 25 nm; the obtained MOFs derivative secondary particle has the same appearance as that of the secondary particle obtained in the embodiment 4, the material has the characteristic of a secondary particle structure consisting of nanoparticles, the surface appearance of the material is uniform and regular, the particle size of the nanoparticles is 110-250nm, and the size of the secondary particle is 4.5-10 μm.
Example 6
The preparation method is the same as example 4, except that: the metal ion precursor is ferric nitrate, the alcohol solution is isopropanol, and the pyridine organic ligand is 4-aminopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 4, the width of the nanosheet is 220-300nm, and the thickness of the nanosheet is not more than 25 nm; the obtained MOFs derivative secondary particle has the same appearance as that of the secondary particle obtained in the embodiment 4, the material has the characteristic of a secondary particle structure consisting of nanoparticles, the surface appearance of the material is uniform and regular, the particle size of the nanoparticles is 150-250nm, and the size of the secondary particle is 4.5-10 μm.
Example 7
In this embodiment, the preparation method of the MOFs nanomaterial and the derivative thereof is as follows:
1.1, mixing 20mol of metal ion precursor ferric nitrate and 10mol of 2-methylimidazole in a methanol solution, and stirring for 4 minutes to obtain a solution A; adding 30mol of 4-dimethylaminopyridine organic ligand methanol solution into the solution A, and stirring for 47 minutes to obtain a solution B;
1.2, placing the solution B in a reaction kettle, reacting for 6 hours at 120 ℃, and finally, carrying out centrifugal separation and drying on a product to obtain the MOFs material;
1.3 annealing the MOFs material at 600 ℃, wherein the heating rate is 3 ℃/min, the heat preservation time is 3h, and the calcining atmosphere is argon, so that the MOFs derivative nano material is obtained.
FIG. 6 is a Scanning Electron Microscope (SEM) image of the MOFs materials. As can be seen from the figure, the obtained MOFs have a two-dimensional nanosheet structure, the nanosheets are non-uniform in size, the width dimension is 200-750nm, and the thickness dimension is not more than 20 nm; FIG. 7 is a Scanning Electron Microscope (SEM) image of the MOFs derivative nanoparticles, and it can be seen from the image that the obtained MOFs derivative material is a secondary particle structure composed of nanoparticles, the particle size of the nanoparticles is not more than 200nm, and the secondary particle size is 1.5-5 μm.
Example 8
The procedure was as in example 7, except that: the metal ion precursor is cobalt nitrate, the alcohol solution is ethanol, and the pyridine organic ligand is 4-cyanopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 7, the width size of the nanosheet is 250-750nm, and the thickness size of the nanosheet is not more than 20 nm; the morphology of the obtained MOFs derivative secondary particles is the same as that of the secondary particles in the embodiment 7, the material is a secondary particle structure formed by nano particles, the particle size of the nano particles is not more than 200nm, and the size of the secondary particles is 1.5-5 microns.
Example 9
The procedure was as in example 7, except that: the metal ion precursor is nickel nitrate, the alcohol solution is isopropanol, and the pyridine organic ligand is 4-aminopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 7, the width size of the nanosheet is 250-800nm, and the thickness size of the nanosheet is not more than 20 nm; the morphology of the obtained MOFs derivative secondary particles is the same as that of the secondary particles in the embodiment 7, the material is a secondary particle structure formed by nano particles, the particle size of the nano particles is not more than 200nm, and the size of the secondary particles is 1.5-5 microns.
Example 10
The preparation method is the same as example 1, except that: the pyridine organic ligand is 4-dimethylamino pyridine. FIG. 8 is a Scanning Electron Microscope (SEM) image of the MOFs materials. As can be seen from the figure, the obtained MOFs has a two-dimensional nanosheet structure, the width dimension of the nanosheet is 100-500nm, and the thickness dimension is 15-20 nm; FIG. 9 is a Scanning Electron Microscope (SEM) image of the MOFs derivative nano-material, and it can be seen from the image that the obtained MOFs derivative is a secondary particle structure composed of nanoparticles, the particle size of the nanoparticles is 50-250nm, and the secondary particle size is 4-8 μm.
Example 11
The preparation method is the same as example 1, except that: the pyridine organic ligand is 4-cyanopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 10, the width of the nanosheet is 150-500nm, and the thickness of the nanosheet is 15-20 nm; the morphology of the obtained MOFs derivative secondary particles is the same as that of the secondary particles in the embodiment 10, the material is a secondary particle structure formed by nano particles, the particle size of the nano particles is 50-250nm, and the size of the secondary particles is 4-8 microns.
Example 12
The preparation method is the same as example 4, except that: the pyridine organic ligand is 4-aminopyridine. FIG. 10 is a Scanning Electron Microscope (SEM) image of the MOFs materials. As can be seen from the figure, the obtained MOFs has a two-dimensional nanosheet structure, the width dimension of the nanosheet is 200-400nm, and the thickness dimension is 20-30 nm; FIG. 11 is a Scanning Electron Microscope (SEM) image of the above MOFs derivative nano-material, from which it can be seen that the obtained MOFs derivative is a secondary particle structure composed of nanoparticles with a particle size of 100-300nm and a secondary particle size of 1.5-4 μm.
Example 13
The preparation method is the same as example 4, except that: the pyridine organic ligand is 4-dimethylamino pyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 12, the width dimension of the nanosheet is 200-450nm, and the thickness dimension is 20-30 nm; the morphology of the obtained MOFs derivative secondary particle is the same as that of the secondary particle in the embodiment 12, the material is a secondary particle structure consisting of nanoparticles, the particle size of the nanoparticles is 100-300nm, and the size of the secondary particle is 1.5-4 μm.
Example 14
The procedure was as in example 7, except that: the pyridine organic ligand is 4-aminopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 7, the width size of the nanosheet is 300-800nm, and the thickness size is not more than 20 nm; the morphology of the obtained MOFs derivative secondary particle is the same as that of the secondary particle in the embodiment 7, the material is a secondary particle structure consisting of nanoparticles, the particle size of the nanoparticles is 200-300nm, and the size of the secondary particle is 1.5-5 μm.
Example 15
The procedure was as in example 7, except that: the pyridine organic ligand is 4-cyanopyridine. The obtained MOFs two-dimensional nanosheet structure is the same as that in the embodiment 7, the width of the nanosheet is 350-800nm, and the thickness of the nanosheet is no more than 20 nm; the morphology of the obtained secondary particle of the MOFs derivative is the same as that of the secondary particle of the embodiment 7, the material is a secondary particle structure consisting of nanoparticles, the particle size of the nanoparticles is 200-300nm, and the size of the secondary particle is 1.5-5.5 μm.
Comparative example 1
The preparation method is the same as example 1, except that: the amounts of the metal ion precursor cobalt nitrate, 2-methylimidazole and 4-aminopyridine organic ligand were 30mol, 20mol and 10mol, respectively. FIG. 12 is a Scanning Electron Microscope (SEM) image of the MOFs material, and it can be seen from the image that the MOFs material prepared under the condition is in a nanometer sheet shape, but the nanometer sheet structure is irregular, the width size range is very large and exceeds 1 μm, and the reaction is incomplete.
Comparative example 2
The preparation method is the same as example 2, except that: and placing the solution B in a reaction kettle, and reacting for 10 hours at 80 ℃. FIG. 13 is a Scanning Electron Microscope (SEM) image of the MOFs derivative nano-material, and it can be seen from the image that the obtained MOFs derivative nano-particles have irregular shapes, more impurities and incomplete reaction.
The foregoing examples further illustrate the present invention but are not to be construed as limiting thereof. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Claims (6)
1. A preparation method of MOFs nano material is characterized by comprising the following steps:
s1, uniformly mixing a metal ion precursor and 2-methylimidazole in an alcohol solution to obtain a solution A, wherein each metal ion forms a coordination bond with nitrogen atoms on 4 2-methylimidazole in a two-dimensional xy plane; the metal ion precursor is at least one of cobalt nitrate, nickel nitrate and ferric nitrate, and the alcohol solution is at least one of methanol, ethanol and isopropanol;
s2, adding a pyridine organic ligand methanol solution into the solution A, and uniformly stirring to obtain a solution B; the hydrothermal reaction temperature is 100-140 ℃, and the reaction time is 5-8 h; the pyridine organic ligand is at least one of 4-aminopyridine, 4-dimethylamino pyridine and 4-cyanopyridine;
s3, placing the solution B into a reaction kettle, enabling the molar ratio of the metal ion precursor to the 2-methylimidazole to the pyridine organic ligand to be 1:1: 1-2: 0.5:3, enabling metal ions to form coordinate bonds with nitrogen atoms in the 2 pyridine organic ligands in the z direction, and carrying out hydrothermal reaction to obtain the MOFs material.
2. The method according to claim 1, wherein the mixing and stirring time for obtaining the solution a is 3 to 5 minutes, and the mixing and stirring time for obtaining the solution B is 45 to 50 minutes.
3. The preparation method according to claim 1, wherein the obtained MOFs material is a two-dimensional nanosheet structure, the size is 180-800nm, and the thickness size is not more than 30 nm.
4. A preparation method of MOFs derivative nanometer material is characterized in that the MOFs material prepared according to any one of claims 1-3 is subjected to annealing treatment to obtain the MOFs derivative nanometer material.
5. The preparation method of claim 4, wherein the annealing temperature is 550-650 ℃, the heating rate is 2-5 ℃/min, the holding time is 1-6 h, and the calcining atmosphere is argon.
6. The preparation method according to claim 5, wherein the MOFs derivative nano-materials are secondary particles assembled by nano-particles, the size of the nano-particles is 50-300nm, and the size of the secondary particles is 1.5-10 μm.
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