CN113234431A - Photochromic metal-organic framework two-dimensional nanosheet and preparation method thereof - Google Patents

Photochromic metal-organic framework two-dimensional nanosheet and preparation method thereof Download PDF

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CN113234431A
CN113234431A CN202110470807.1A CN202110470807A CN113234431A CN 113234431 A CN113234431 A CN 113234431A CN 202110470807 A CN202110470807 A CN 202110470807A CN 113234431 A CN113234431 A CN 113234431A
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石乃恩
任于宝
黄维
丁震
宋钊
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Nanjing University of Posts and Telecommunications
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Abstract

The invention discloses a photochromic metal organic framework two-dimensional nanosheet, which has the chemical formula: [ Eu ] as a source of electric potential2(OH)2(H2O)2L]Cl2⋅8H2O, wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine. The thickness of each single piece of the photochromic metal organic framework two-dimensional nanosheet is 10-50 mm, and the side length of each single piece is 400-2000 nm. The photochromic metal organic framework two-dimensional nanosheet has excellent optical response characteristics, can generate reversible photochromic phenomenon under the irradiation of an ultraviolet lamp, can be applied to the fields of light-operated catalysis, optical information storage, photonic switches and the like, and has wide market prospect.

Description

Photochromic metal-organic framework two-dimensional nanosheet and preparation method thereof
Technical Field
The invention discloses a photochromic metal organic framework two-dimensional nanosheet and a preparation method thereof, and relates to the technical field of metal organic frameworks.
Background
Metal Organic Framework (MOF) is a novel porous crystalline material with a periodic network structure formed by self-assembly of Metal ions/clusters and Organic bridging ligands, and due to the ultrahigh porosity and the ultrahigh specific surface area, the MOF material has great application potential in a plurality of fields such as catalysis, energy storage, biomedical treatment and the like. Among many MOF materials, two-dimensional nanomaterials have received much attention from the industry due to their advantages of large specific surface area, many active sites, short charge transport paths, and easy processing into films.
In the prior art, most of the methods for synthesizing MOF materials are synthesized by using a metal salt solution as a metal source, and through the synthesis mode, the reaction can be performed rapidly, the MOF nucleation and growth processes are difficult to control, and the MOF materials with nanometer morphology are difficult to obtain. In contrast, solid precursor conversion methods for the synthesis of MOF materials using solid precursors are more appropriate, in which, first of all, upon solvothermal reaction, the solid phase material provides metal cations in a spatially and temporally controlled manner, the nucleation sites of which are not uniformly distributed throughout the solution, but are more confined to the local surroundings of the solid precursor, which makes it possible to control the MOF nucleation and growth process in which homogeneous nucleation in solution is essentially suppressed. Thus, the solid precursor can not only provide metal ions, but can also act as a structure directing agent, thereby making it possible to replicate the morphology or pattern of the solid precursor into the synthesized MOF material.
In summary, if a solid precursor conversion method can be effectively applied to prepare MOF two-dimensional nanosheets with photochromic properties, it is inevitable to provide help for the development of the whole MOF material field.
Disclosure of Invention
In view of the above defects in the prior art, the present invention aims to provide a photochromic metal-organic framework two-dimensional nanosheet and a preparation method thereof, which are as follows.
A photochromic metal-organic framework two-dimensional nanosheet having a chemical formula:
[Eu2(OH)2(H2O)2L]Cl2⋅8H2O，
wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine.
Preferably, the thickness of a single piece of the photochromic metal organic framework two-dimensional nanosheet is 10-50 mm, and the side length of the single piece is 400-2000 nm.
Preferably, under the condition of ultraviolet lamp irradiation, the photochromic metal-organic framework two-dimensional nanoplatelets can generate reversible photochromic phenomenon.
A preparation method of a photochromic metal organic framework two-dimensional nanosheet is used for preparing the photochromic metal organic framework two-dimensional nanosheet, and comprises the following steps:
s1, adding Eu2O3Adding the nanorods into a mixed reagent of acetonitrile and water, and ultrasonically dissolving for 2-10 min to obtain uniform Eu2O3A nanorod dispersion;
s2, adding Eu by using N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride as a ligand2O3Formation of Eu in nanorod dispersion2O3Ultrasonically dissolving the mixed solution of the nano-rods and the ligand for 5-10 min to obtain uniform Eu2O3Dispersion of nanorods and ligands;
s3, adding Eu2Transferring the O3 nanorod and ligand dispersion liquid into an autoclave, placing the autoclave in an oven, heating to 100-120 ℃, carrying out solvothermal reaction, standing for 48-72 h, and naturally cooling to room temperature to obtain a reaction product;
and S4, repeatedly carrying out centrifugal separation and ultrasonic washing on the reaction product at room temperature for multiple times, removing surface impurities of the reaction product, and then placing the washed reaction product in a vacuum oven for drying treatment to finally obtain the photochromic metal organic framework two-dimensional nanosheet.
Preferably, the Eu2O3The nano-rod is composed ofPrepared by a solid-phase thermal decomposition method, the Eu2O3The length of the nano rod is 500 nm-800 nm, and the diameter of the nano rod is 80 nm-150 nm.
Preferably, the mixing volume ratio of the mixed reagent of the acetonitrile and the water is that the ratio of acetonitrile: water = (2-4): 1.
preferably, the Eu2O3The mass ratio of the nanorod to the N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride is 1: (1-2).
Compared with the prior art, the invention has the advantages that:
the photochromic metal organic framework two-dimensional nanosheet provided by the invention has excellent optical response characteristics, and can generate reversible photochromic phenomenon under the irradiation of an ultraviolet lamp. By means of the material characteristics, the photochromic metal organic framework two-dimensional nanosheet can be applied to the fields of photo-control catalysis, optical information storage, photonic switches and the like, and has a wide market prospect.
Correspondingly, the preparation method of the photochromic metal organic framework two-dimensional nanosheet effectively utilizes a solid precursor conversion method and Eu2O3The nano-rods are used as solid precursors, so that metal ions in a reaction solution become rare, the nucleation and growth processes of the MOF can be effectively controlled, the continuous and stable proceeding of the preparation process is guaranteed, the yield of the preparation is improved, and the photochromic metal organic framework two-dimensional nano-plate with the special optical response performance is finally obtained.
In addition, the invention can also be used as a reference basis for subsequent research, and has reference value and deployment significance for searching and preparing related materials by researchers in the industry in the future.
The following detailed description of the embodiments of the present invention is provided in connection with the accompanying drawings to make the technical solutions of the present invention easier to understand and master.
Drawings
FIG. 1 shows Eu used in the present invention2O3Scanning electron microscope image of the nano rod;
FIG. 2 is an X-ray diffraction diagram of a photochromic metal-organic framework two-dimensional nanosheet obtained in example 1 of the present invention;
fig. 3 is a scanning electron microscope image of a photochromic metal-organic framework two-dimensional nanosheet obtained in example 1 of the present invention;
fig. 4 is a transmission electron microscope image of a photochromic metal-organic framework two-dimensional nanosheet obtained in example 1 of the present invention;
fig. 5 is an atomic force electron microscope image of a photochromic metal-organic framework two-dimensional nanosheet obtained in example 1 of the present invention;
fig. 6 is a scanning electron microscope image of a photochromic metal-organic framework two-dimensional nanosheet obtained in example 2 of the present invention;
fig. 7 is a scanning electron microscope image of a photochromic metal-organic framework two-dimensional nanosheet obtained in embodiment 3 of the present invention.
Detailed Description
The invention uses Eu2O3The nano-rod is used as a solid precursor, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridyl dichloride is used as a ligand, and a photochromic metal organic framework two-dimensional nano-sheet is prepared in a controllable state by using a solid precursor conversion method. The invention utilizes the special photochromic capacity of the dichloro-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridyl ligand to further obtain the photochromic metal organic framework two-dimensional nanosheet, and the two-dimensional structure is favorable for film forming and can be conveniently applied subsequently.
Specifically, the invention provides a photochromic metal organic framework two-dimensional nanosheet and a preparation method thereof, and the scheme is as follows.
A photochromic metal-organic framework two-dimensional nanosheet having a chemical formula:
[Eu2(OH)2(H2O)2L]Cl2⋅8H2O，
wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine.
The thickness of each single piece of the photochromic metal organic framework two-dimensional nanosheet is 10-50 mm, and the side length of each single piece is 400-2000 nm.
It should be noted that, under the irradiation condition of the ultraviolet lamp, the photochromic metal-organic framework two-dimensional nanoplatelets can generate a reversible photochromic phenomenon.
In conclusion, the photochromic metal organic framework two-dimensional nanosheet provided by the invention has excellent optical response characteristics, and a reversible photochromic phenomenon can occur in the material under the irradiation of an ultraviolet lamp. By means of the material characteristics, the photochromic metal organic framework two-dimensional nanosheet can be applied to the fields of photo-control catalysis, optical information storage, photonic switches and the like, and has a wide market prospect.
A preparation method of a photochromic metal organic framework two-dimensional nanosheet is used for preparing the photochromic metal organic framework two-dimensional nanosheet, and comprises the following steps:
s1, adding Eu2O3Adding the nanorods into a mixed reagent of acetonitrile and water, and ultrasonically dissolving for 2-10 min to obtain uniform Eu2O3A nanorod dispersion.
In this step, the Eu2O3The nano-rod is a novel nano-material prepared by a solid-phase thermal decomposition method and used as a solid precursor, and the Eu is2O3The length of the nano rod is 500 nm-800 nm, and the diameter of the nano rod is 80 nm-150 nm. The mixed volume ratio of the acetonitrile to the mixed reagent of water is as follows: water = (2-4): 1. the water here is preferably deionized water.
FIG. 1 shows Eu used in the present embodiment2O3View of the nanorods under a scanning electron microscope, it can be seen that Eu2O3Is of nanorod structure, Eu2O3The length of the nano-rod is 300 nm-1000 nm, and the diameter is 80 nm-200 nm.
S2, adding Eu by using N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride as a ligand2O3Formation of Eu in nanorod dispersion2O3Ultrasonically dissolving the mixed solution of the nano-rods and the ligand for 5-10 min to obtain uniform Eu2O3Of nanorods with ligandsAnd (3) dispersing the mixture.
In this step, it should be noted that the Eu should be controlled when the material addition is performed2O3The mass ratio of the nano-rod to the N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridyl dichloride is 1: (1-2).
S3, adding Eu2Transferring the O3 nanorod and ligand dispersion liquid into an autoclave, placing the autoclave in an oven, heating to 100-120 ℃, carrying out solvothermal reaction, standing for 48-72 h, and naturally cooling to room temperature to obtain a reaction product.
And S4, repeatedly carrying out centrifugal separation and ultrasonic washing on the reaction product at room temperature for multiple times, removing surface impurities of the reaction product, and then placing the washed reaction product in a vacuum oven for drying treatment to finally obtain the photochromic metal organic framework two-dimensional nanosheet.
Correspondingly, the preparation method of the photochromic metal organic framework two-dimensional nanosheet effectively utilizes a solid precursor conversion method and Eu2O3The nano-rods are used as solid precursors, so that metal ions in a reaction solution become rare, the nucleation and growth processes of the MOF can be effectively controlled, the continuous and stable proceeding of the preparation process is guaranteed, the yield of the prepared product is improved, and the photochromic metal organic framework two-dimensional nano-plate with special optical response performance is finally obtained.
To demonstrate the effectiveness of the above approach, three specific examples are provided herein as references.
Example 1
A preparation method of a photochromic metal organic framework two-dimensional nanosheet comprises the following steps:
s1, adding Eu2O3Adding the nanorods into a mixed reagent of acetonitrile and water, and ultrasonically dissolving for 2-10 min to obtain uniform Eu2O3A nanorod dispersion. In this example, the mixed reagent of acetonitrile and water contained 2mL of acetonitrile and 1mL of deionized water.
S2, mixing N, N ' -bis (3, 5-dicarboxybenzylidene) -4,4' dichloride '-bipyridine as ligand, adding Eu2O3Formation of Eu in nanorod dispersion2O3Ultrasonically dissolving the mixed solution of the nano-rods and the ligand for 5-10 min to obtain uniform Eu2O3Dispersion of nanorods and ligands. Eu as defined herein2O3The mass ratio of the nanorod to the N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride is 1: 1.5.
s3, adding Eu2Transferring the dispersion liquid of the O3 nano-rod and the ligand into an autoclave, placing the autoclave in an oven, heating to 120 ℃, carrying out solvothermal reaction, standing for 72 hours, and naturally cooling to room temperature to obtain a reaction product.
And S4, repeatedly carrying out centrifugal separation and ultrasonic washing on the reaction product at room temperature for multiple times, removing surface impurities of the reaction product, and then placing the washed reaction product in a vacuum oven for drying treatment to finally obtain the photochromic metal organic framework two-dimensional nanosheet.
Fig. 2 is a result diagram of structural analysis performed on the photochromic metal-organic framework two-dimensional nanosheet obtained in the present embodiment by using an X-ray powder diffractometer, and XRD diffraction peaks in the diagram correspond to standard cards one to one, which proves that the photochromic metal-organic framework two-dimensional nanosheet is successfully prepared in the present embodiment. 3 distinct sharp diffraction peaks are observed at 6 °, 9 ° and 13 °, which can be assigned to the (020), (110) and (011) crystal planes of the Eu orthorhombic system.
Fig. 3, 4 and 5 are graphs showing the results of performing morphology analysis on the photochromic metal-organic framework two-dimensional nanosheet obtained in the present embodiment by using a scanning electron microscope, a transmission electron microscope and an atomic force microscope, respectively, and it can be seen from the graphs that the thickness of the single photochromic metal-organic framework two-dimensional nanosheet is 10nm to 50nm, and the side length is 400nm to 2000 nm.
And then, the optical response performance of the photochromic metal-organic framework two-dimensional nanosheet obtained by a researcher is researched. Irradiating the photochromic metal organic framework two-dimensional nanosheet after vacuum drying by using an ultraviolet lamp, wherein the sample is changed from bright yellow to gray yellow after 60 s and is changed into brown after 300 s, and the original color of the sample is gradually recovered after the sample is placed in the air for 15 min. In addition, researchers also find that when the photochromic metal-organic framework two-dimensional nanosheet is dispersed in an ethanol solution and irradiated by an ultraviolet lamp, the color of the sample changes from bright yellow to yellow green after 150 seconds, the color of the sample changes to black green after 300 seconds, and after the irradiation is stopped, the original color of the sample is gradually recovered.
Example 2
A preparation method of a photochromic metal organic framework two-dimensional nanosheet comprises the following steps:
s1, adding Eu2O3Adding the nanorods into a mixed reagent of acetonitrile and water, and ultrasonically dissolving for 2-10 min to obtain uniform Eu2O3A nanorod dispersion. In this example, the mixed reagent of acetonitrile and water contained 2mL of acetonitrile and 1mL of deionized water.
S2, adding Eu by using N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride as a ligand2O3Formation of Eu in nanorod dispersion2O3Ultrasonically dissolving the mixed solution of the nano-rods and the ligand for 5-10 min to obtain uniform Eu2O3Dispersion of nanorods and ligands. Eu as defined herein2O3The mass ratio of the nanorod to the N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride is 1: 1.
s3, adding Eu2Transferring the dispersion liquid of the O3 nano-rod and the ligand into an autoclave, placing the autoclave in an oven, heating to 120 ℃, carrying out solvothermal reaction, standing for 72 hours, and naturally cooling to room temperature to obtain a reaction product.
And S4, repeatedly carrying out centrifugal separation and ultrasonic washing on the reaction product at room temperature for multiple times, removing surface impurities of the reaction product, and then placing the washed reaction product in a vacuum oven for drying treatment to finally obtain the photochromic metal organic framework two-dimensional nanosheet.
Fig. 6 is a diagram showing the result of performing morphology analysis on the photochromic metal-organic framework two-dimensional nanosheet obtained in the present embodiment by using a scanning electron microscope, and it can be seen from the diagram that the photochromic metal-organic framework two-dimensional nanosheet maintains the original sheet-like structure and morphology. The photochromic metal organic framework two-dimensional nanosheet prepared in the embodiment also has excellent optical response characteristics, and reversible photochromic phenomena occur in both a solid powder sample after vacuum drying and a sample dispersed in an ethanol solution under the irradiation of an ultraviolet lamp.
Example 3
A preparation method of a photochromic metal organic framework two-dimensional nanosheet comprises the following steps:
s1, adding Eu2O3Adding the nanorods into a mixed reagent of acetonitrile and water, and ultrasonically dissolving for 2-10 min to obtain uniform Eu2O3A nanorod dispersion. In this example, the mixed reagent of acetonitrile and water contained 2mL of acetonitrile and 0.5mL of deionized water.
S2, adding Eu by using N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride as a ligand2O3Formation of Eu in nanorod dispersion2O3Ultrasonically dissolving the mixed solution of the nano-rods and the ligand for 5-10 min to obtain uniform Eu2O3Dispersion of nanorods and ligands. Eu as defined herein2O3The mass ratio of the nanorod to the N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride is 1: 1.5.
s3, adding Eu2Transferring the dispersion liquid of the O3 nano-rod and the ligand into an autoclave, placing the autoclave in an oven, heating to 120 ℃, carrying out solvothermal reaction, standing for 72 hours, and naturally cooling to room temperature to obtain a reaction product.
And S4, repeatedly carrying out centrifugal separation and ultrasonic washing on the reaction product at room temperature for multiple times, removing surface impurities of the reaction product, and then placing the washed reaction product in a vacuum oven for drying treatment to finally obtain the photochromic metal organic framework two-dimensional nanosheet.
Fig. 7 is a diagram showing the result of performing morphology analysis on the photochromic metal-organic framework two-dimensional nanosheet obtained in the present embodiment by using a scanning electron microscope, and it can be seen from the diagram that the photochromic metal-organic framework two-dimensional nanosheet maintains the original sheet structure, but is more densely stacked, which is the reason for the reduction of the solvent content in the reaction system. The photochromic metal organic framework two-dimensional nanosheet prepared in the embodiment also has excellent optical response characteristics, and reversible photochromic phenomena occur in both a solid powder sample after vacuum drying and a sample dispersed in an ethanol solution under the irradiation of an ultraviolet lamp.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Finally, it should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should integrate the description, and the technical solutions in the embodiments can be appropriately combined to form other embodiments understood by those skilled in the art.

Claims (7)

1. A photochromic metal-organic framework two-dimensional nanosheet, wherein the photochromic metal-organic framework two-dimensional nanosheet has the chemical formula: [ Eu ] as a source of electric potential2(OH)2(H2O)2L]Cl2⋅8H2O, wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine.
2. Photochromic metal-organic framework two-dimensional nanoplatelets according to claim 1 characterized in that: the thickness of each single piece of the photochromic metal organic framework two-dimensional nanosheet is 10-50 mm, and the side length of each single piece is 400-2000 nm.
3. Photochromic metal-organic framework two-dimensional nanoplatelets according to claim 1 characterized in that: under the condition of ultraviolet lamp irradiation, the photochromic metal-organic framework two-dimensional nanoplatelets can generate reversible photochromic phenomenon.
4. A preparation method of photochromic metal organic framework two-dimensional nanosheets, which is used for preparing the photochromic metal organic framework two-dimensional nanosheets as claimed in any one of claims 1 to 3, and is characterized by comprising the following steps:
s1, adding Eu2O3Adding the nanorods into a mixed reagent of acetonitrile and water, and ultrasonically dissolving for 2-10 min to obtain uniform Eu2O3A nanorod dispersion;
s2, adding Eu by using N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride as a ligand2O3Formation of Eu in nanorod dispersion2O3Ultrasonically dissolving the mixed solution of the nano-rods and the ligand for 5-10 min to obtain uniform Eu2O3Dispersion of nanorods and ligands;
s3, adding Eu2Transferring the O3 nanorod and ligand dispersion liquid into an autoclave, placing the autoclave in an oven, heating to 100-120 ℃, carrying out solvothermal reaction, standing for 48-72 h, and naturally cooling to room temperature to obtain a reaction product;
and S4, repeatedly carrying out centrifugal separation and ultrasonic washing on the reaction product at room temperature for multiple times, removing surface impurities of the reaction product, and then placing the washed reaction product in a vacuum oven for drying treatment to finally obtain the photochromic metal organic framework two-dimensional nanosheet.
5. The preparation method of photochromic metal-organic framework two-dimensional nanoplates as in claim 4, wherein: the Eu being2O3The nano-rod is prepared by a solid-phase thermal decomposition method, and the Eu is2O3The length of the nano rod is 500 nm-800 nm, and the diameter of the nano rod is 80 nm-150 nm.
6. The preparation method of photochromic metal-organic framework two-dimensional nanoplates as in claim 4, wherein: the mixed volume ratio of the acetonitrile to the mixed reagent of water is as follows: water = (2-4): 1.
7. the preparation method of photochromic metal-organic framework two-dimensional nanoplates as in claim 4, wherein: the Eu being2O3The mass ratio of the nanorod to the N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride is 1: (1-2).
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