CN113234431B - Photochromic metal-organic framework two-dimensional nano sheet and preparation method thereof - Google Patents
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Abstract
The invention discloses a two-dimensional nano sheet of a photochromic metal-organic framework, which has the chemical formula: [ Eu ] 2 (OH) 2 (H 2 O) 2 L]Cl 2 ⋅8H 2 O, wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine. The thickness of a single piece of the two-dimensional nano sheet of the photochromic metal-organic frame is 10 mm-50 mm, and the side length of the single piece is 400 nm-2000 nm. The photochromic metal-organic framework two-dimensional nano sheet 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 control catalysis, optical information storage, optical molecular switches and the like, and has wide market prospect.
Description
Technical Field
The invention discloses a two-dimensional nano sheet of a photochromic metal-organic framework and a preparation method thereof, and relates to the technical field of metal-organic frameworks.
Background
The metal organic frameworks (Metal Organic Framework, MOF) are novel porous crystal materials which are formed by self-assembly of metal ions/clusters and organic bridging ligands and have periodic network structures, and the application potential of the MOF materials is very large in various fields of catalysis, energy storage, biomedical treatment and the like due to the ultrahigh porosity and the ultrahigh specific surface area of the novel porous crystal materials. Among the MOF materials, two-dimensional nanomaterials have received much attention from the industry due to their large specific surface area, many active sites, short charge transport paths, and easier processing into films.
In the prior art, most of the methods for synthesizing MOF materials are performed by using metal salt solution as a metal source, and by adopting the synthesis mode, the reaction can be performed relatively rapidly, the nucleation and growth processes of the MOF are difficult to control, and the MOF materials with the nano morphology are difficult to obtain. In comparison, a solid precursor conversion process for synthesizing MOF materials using solid precursors is more appropriate, in which, first, upon solvothermal reaction, the solid phase species provide metal cations in a spatially and temporally controlled manner, with nucleation sites that are not uniformly distributed throughout the solution, but rather are more confined to localized surroundings of the solid precursor, which in turn allows homogeneous nucleation in the solution to be essentially inhibited, and the nucleation and growth process of the MOF to become controllable. Thus, the solid precursor can not only provide metal ions, but also act as a structure directing agent, thereby potentially replicating the morphology or pattern of the solid precursor into the synthesized MOF material.
In summary, if the solid precursor conversion method can be effectively applied to prepare the MOF two-dimensional nano-sheet with photochromic performance, the method can be helpful to the development of the whole MOF material field.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a two-dimensional nano-sheet of a photochromic metal-organic framework and a preparation method thereof, which are specifically as follows.
A photochromic metal-organic framework two-dimensional nanoplatelet having the formula:
[Eu 2 (OH) 2 (H 2 O) 2 L]Cl 2 ⋅8H 2 O，
wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine.
Preferably, the thickness of a single piece of the two-dimensional nano sheet of the photochromic metal-organic frame is 10 mm-50 mm, and the side length of the single piece is 400 nm-2000 nm.
Preferably, under the condition of ultraviolet light irradiation, the two-dimensional nano sheet of the photochromic metal-organic framework can generate reversible photochromic phenomenon.
A method for preparing a two-dimensional nano-sheet of a photochromic metal-organic framework, which is used for preparing the two-dimensional nano-sheet of the photochromic metal-organic framework, and comprises the following steps:
s1, eu is added 2 O 3 Adding the nanorods into a mixed reagent of acetonitrile and water, and performing ultrasonic dissolution for 2-10 min to obtain uniform Eu 2 O 3 A nanorod dispersion;
s2, adding Eu into N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride serving as a ligand 2 O 3 Eu formation in nanorod dispersion 2 O 3 Ultrasonic dissolving the mixed solution of the nanorods and the ligand for 5-10 min to obtain uniform Eu 2 O 3 A dispersion of nanorods and ligands;
s3, eu is added 2 Transferring the dispersion liquid of the O3 nanorods and the ligand into an autoclave, placing the autoclave into an oven, heating to 100-120 ℃, performing solvothermal reaction, then standing for 48-72 h, and naturally cooling to room temperature to obtain a reaction product;
s4, carrying out repeated centrifugal separation and ultrasonic washing on the reaction product for a plurality of times at room temperature, 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 nano-sheet.
Preferably, the Eu 2 O 3 The nanorods are prepared by a solid-phase thermal decomposition method, and the Eu is prepared by a solid-phase thermal decomposition method 2 O 3 The length of the nanorods is 500-800 nm, and the diameter of the nanorods is 80-150 nm.
Preferably, the mixing volume ratio of the acetonitrile and water mixed reagent is that acetonitrile: water= (2-4): 1.
preferably, the Eu 2 O 3 The mass ratio of the nanorods to the di-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine is 1: (1-2).
Compared with the prior art, the invention has the advantages that:
the two-dimensional nano sheet of the photochromic metal-organic framework has excellent optical response characteristics, and the material can generate reversible photochromic phenomenon under the irradiation of an ultraviolet lamp. By virtue of the characteristics of the materials, the photochromic metal-organic framework two-dimensional nanosheets can be applied to the fields of light control catalysis, optical information storage, optical molecular switches and the like, and have wide market prospect.
Correspondingly, the invention provides a photochromic metal organic compoundThe preparation method of the two-dimensional nano-sheet of the framework effectively uses a solid precursor conversion method and utilizes Eu 2 O 3 The nanorods are used as solid precursors, so that metal ions in a reaction solution become rare, the nucleation and growth process of MOF can be effectively controlled, the continuous and stable preparation process is ensured, the preparation yield is improved, and the photochromic metal-organic framework two-dimensional nanosheets with special optical response performance are finally obtained.
In addition, the invention can also be used as a reference basis for subsequent researches, and has reference value and deployment significance for later searching and preparing related materials by researchers in the industry.
The following detailed description of the invention is provided with reference to the accompanying drawings, so that the technical scheme of the invention can be more easily understood and mastered.
Drawings
FIG. 1 shows Eu used in the present invention 2 O 3 Scanning electron microscope pictures of the nanorods;
FIG. 2 is an X-ray diffraction pattern of a two-dimensional nanoplatelet of a photochromic metal-organic framework obtained in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of a two-dimensional nanosheet of a photochromic metal-organic framework obtained in example 1 of the present invention;
FIG. 4 is a transmission electron microscope image of a two-dimensional nanoplatelet of a photochromic metal-organic framework obtained in example 1 of the present invention;
FIG. 5 is an atomic force microscope image of a two-dimensional nanoplatelet of a photochromic metal-organic framework obtained in example 1 of the present invention;
FIG. 6 is a scanning electron microscope image of a two-dimensional nanoplatelet of a photochromic metal-organic framework obtained in example 2 of the present invention;
FIG. 7 is a scanning electron microscope image of a two-dimensional nanoplatelet of a photochromic metal-organic framework obtained in example 3 of the present invention.
Detailed Description
The invention uses Eu 2 O 3 The nanorod is a solid precursor, and N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride is used as a solid precursorThe ligand is prepared into a photochromic metal-organic framework two-dimensional nano-sheet in a controllable state by using a solid precursor conversion method. The invention utilizes the special photochromic capability of the dichloro-N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine ligand to further obtain the photochromic metal-organic framework two-dimensional nano-sheet, and the two-dimensional structure is favorable for film formation and can facilitate the subsequent application.
Specifically, the invention provides a two-dimensional nano sheet of a photochromic metal-organic framework and a preparation method thereof, and the scheme is as follows.
A photochromic metal-organic framework two-dimensional nanoplatelet having the formula:
[Eu 2 (OH) 2 (H 2 O) 2 L]Cl 2 ⋅8H 2 O，
wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine.
The thickness of a single piece of the two-dimensional nano sheet of the photochromic metal-organic frame is 10 mm-50 mm, and the side length of the single piece is 400 nm-2000 nm.
Under the condition of ultraviolet light irradiation, the two-dimensional nano sheet of the photochromic metal-organic framework can generate reversible photochromic phenomenon.
In summary, the two-dimensional nano sheet of the photochromic metal-organic framework provided by the invention has excellent optical response characteristics, and the material can generate reversible photochromic phenomenon under the irradiation of an ultraviolet lamp. By virtue of the characteristics of the materials, the photochromic metal-organic framework two-dimensional nanosheets can be applied to the fields of light control catalysis, optical information storage, optical molecular switches and the like, and have wide market prospect.
A method for preparing a two-dimensional nano-sheet of a photochromic metal-organic framework, which is used for preparing the two-dimensional nano-sheet of the photochromic metal-organic framework, and comprises the following steps:
s1, eu is added 2 O 3 Adding the nanorods into a mixed reagent of acetonitrile and water, and performing ultrasonic dissolution for 2-10 min to obtain uniform Eu 2 O 3 Nanometer scaleBar dispersion.
In this step, the Eu 2 O 3 The nanorod is a novel nanomaterial prepared by a solid-phase thermal decomposition method and is used as a solid precursor, and the Eu is 2 O 3 The length of the nanorods is 500-800 nm, and the diameter of the nanorods is 80-150 nm. The mixing volume ratio of the acetonitrile and water mixed reagent is that: water= (2-4): 1. the water here is preferably deionized water.
FIG. 1 shows Eu used in the present embodiment 2 O 3 As can be seen from the view of the nanorods under a scanning electron microscope, eu 2 O 3 Is of a nano rod structure and Eu 2 O 3 The length of the nanorods is 300 nm-1000 nm, and the diameter is 80 nm-200 nm.
S2, adding Eu into N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride serving as a ligand 2 O 3 Eu formation in nanorod dispersion 2 O 3 Ultrasonic dissolving the mixed solution of the nanorods and the ligand for 5-10 min to obtain uniform Eu 2 O 3 A dispersion of nanorods and ligands.
In this step, it is noted that the Eu should be controlled when the material addition is performed 2 O 3 The mass ratio of the nanorods to the di-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine is 1: (1-2) in the section.
S3, eu is added 2 Transferring the dispersion liquid of the O3 nanorods and the ligand into an autoclave, placing the autoclave into an oven, heating to 100-120 ℃, performing solvothermal reaction, then standing for 48-72 h, and naturally cooling to room temperature to obtain a reaction product.
S4, carrying out repeated centrifugal separation and ultrasonic washing on the reaction product for a plurality of times at room temperature, 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 nano-sheet.
Correspondingly, the preparation method of the photochromic metal-organic framework two-dimensional nanosheets effectively uses solid precursorsConversion process using Eu 2 O 3 The nanorods are used as solid precursors, so that metal ions in a reaction solution become rare, the nucleation and growth process of MOF can be effectively controlled, the continuous and stable operation of the preparation process is ensured, the yield of the prepared product is improved, and finally the photochromic metal-organic framework two-dimensional nanosheets with special optical response performance are obtained.
To demonstrate the effectiveness of the above-described scheme, three specific embodiments are provided herein by reference.
Example 1
A preparation method of a two-dimensional nano sheet of a photochromic metal-organic framework comprises the following steps:
s1, eu is added 2 O 3 Adding the nanorods into a mixed reagent of acetonitrile and water, and performing ultrasonic dissolution for 2-10 min to obtain uniform Eu 2 O 3 A nanorod dispersion. Here, the acetonitrile and water mixed reagent was 2mL of acetonitrile and 1mL of deionized water.
S2, adding Eu into N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride serving as a ligand 2 O 3 Eu formation in nanorod dispersion 2 O 3 Ultrasonic dissolving the mixed solution of the nanorods and the ligand for 5-10 min to obtain uniform Eu 2 O 3 A dispersion of nanorods and ligands. Eu as described herein 2 O 3 The mass ratio of the nanorods to the di-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine is 1:1.5.
s3, eu is added 2 Transferring the dispersion liquid of the O3 nano rod and the ligand into an autoclave, placing the autoclave into an oven, heating to 120 ℃, carrying out solvothermal reaction, then standing for 72h, and naturally cooling to room temperature to obtain a reaction product.
S4, carrying out repeated centrifugal separation and ultrasonic washing on the reaction product for a plurality of times at room temperature, 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 nano-sheet.
Fig. 2 is a graph of the result of structural analysis of the photochromic metal-organic framework two-dimensional nano-sheet obtained in the present embodiment by using an X-ray powder diffractometer, and XRD diffraction peaks in the graph correspond to standard cards one by one, which proves that the photochromic metal-organic framework two-dimensional nano-sheet is successfully prepared in the present embodiment. 3 distinct sharp diffraction peaks were observed at 6 °, 9 °, 13 °, and can be attributed to the (020), (110), and (011) crystal planes of the Eu-orthorhombic crystal system.
Fig. 3, fig. 4, and fig. 5 are graphs showing the results of morphological analysis of the photochromic metal-organic framework two-dimensional nanosheets obtained in this example 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 a single piece of the photochromic metal-organic framework two-dimensional nanosheets is 10nm to 50nm, and the side length is 400nm to 2000nm.
The optical response properties of the photochromic metal-organic framework two-dimensional nanoplatelets obtained by the researchers were then studied. The vacuum dried photochromic metal-organic frame two-dimensional nano sheet is irradiated by an ultraviolet lamp, the sample is changed from bright yellow to grey yellow after 60 s and changed to 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, the researchers also found that the photochromic metal-organic framework two-dimensional nano-sheets were dispersed in ethanol solution and irradiated with an ultraviolet lamp, the color of the sample changed from bright yellow to yellow-green after 150s, changed to black-green after 300 s, and the original color of the sample was gradually restored after stopping irradiation.
Example 2
A preparation method of a two-dimensional nano sheet of a photochromic metal-organic framework comprises the following steps:
s1, eu is added 2 O 3 Adding the nanorods into a mixed reagent of acetonitrile and water, and performing ultrasonic dissolution for 2-10 min to obtain uniform Eu 2 O 3 A nanorod dispersion. Here, the acetonitrile and water mixed reagent was 2mL of acetonitrile and 1mL of deionized water.
S2, adding Eu into N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride serving as a ligand 2 O 3 Eu formation in nanorod dispersion 2 O 3 Ultrasonic dissolving the mixed solution of the nanorods and the ligand for 5-10 min to obtain uniform Eu 2 O 3 A dispersion of nanorods and ligands. Eu as described herein 2 O 3 The mass ratio of the nanorods to the di-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine is 1:1.
s3, eu is added 2 Transferring the dispersion liquid of the O3 nano rod and the ligand into an autoclave, placing the autoclave into an oven, heating to 120 ℃, carrying out solvothermal reaction, then standing for 72h, and naturally cooling to room temperature to obtain a reaction product.
S4, carrying out repeated centrifugal separation and ultrasonic washing on the reaction product for a plurality of times at room temperature, 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 nano-sheet.
Fig. 6 is a graph showing the result of morphological analysis of the photochromic metal-organic framework two-dimensional nanosheets obtained in this example by using a scanning electron microscope, and it can be seen from the graph that the photochromic metal-organic framework two-dimensional nanosheets maintain the original lamellar structure and morphology. The photochromic metal-organic framework two-dimensional nano-sheet prepared in the embodiment also has excellent optical response characteristics, and the solid powder sample after vacuum drying and the sample dispersed in the ethanol solution all have reversible photochromic phenomena under the irradiation of an ultraviolet lamp.
Example 3
A preparation method of a two-dimensional nano sheet of a photochromic metal-organic framework comprises the following steps:
s1, eu is added 2 O 3 Adding the nanorods into a mixed reagent of acetonitrile and water, and performing ultrasonic dissolution for 2-10 min to obtain uniform Eu 2 O 3 A nanorod dispersion. Here, acetonitrile was 2mL and deionized water was 0.5mL in the acetonitrile and water mixed reagent.
S2, adding Eu into N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride serving as a ligand 2 O 3 Eu formation in nanorod dispersion 2 O 3 Ultrasonic dissolving the mixed solution of the nanorods and the ligand for 5-10 min to obtain uniform Eu 2 O 3 A dispersion of nanorods and ligands. Eu as described herein 2 O 3 The mass ratio of the nanorods to the di-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine is 1:1.5.
s3, eu is added 2 Transferring the dispersion liquid of the O3 nano rod and the ligand into an autoclave, placing the autoclave into an oven, heating to 120 ℃, carrying out solvothermal reaction, then standing for 72h, and naturally cooling to room temperature to obtain a reaction product.
S4, carrying out repeated centrifugal separation and ultrasonic washing on the reaction product for a plurality of times at room temperature, 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 nano-sheet.
Fig. 7 is a graph showing the result of morphological analysis of the two-dimensional nanoplatelets of the photochromic metal-organic framework obtained in this example by using a scanning electron microscope, and it can be seen from the graph that the two-dimensional nanoplatelets of the photochromic metal-organic framework maintain the original lamellar structure, but are densely stacked, which is why the solvent content of the reaction system is reduced. The photochromic metal-organic framework two-dimensional nano-sheet prepared in the embodiment also has excellent optical response characteristics, and the solid powder sample after vacuum drying and the sample dispersed in the ethanol solution all have reversible photochromic phenomena 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 characteristics 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 disclosure describes embodiments, not every embodiment is intended to include only a single embodiment, and that this description is for clarity only, and that those skilled in the art will recognize that the embodiments described herein may be suitably combined to form other embodiments as would be understood by those skilled in the art.
Claims (5)
1. The preparation method of the photochromic metal-organic framework two-dimensional nanosheets is characterized by comprising the following steps of:
s1, eu is added 2 O 3 Adding the nanorods into a mixed reagent of acetonitrile and water, and performing ultrasonic dissolution for 2-10 min to obtain uniform Eu 2 O 3 A nanorod dispersion;
s2, adding Eu into N, N '-di (3, 5-dicarboxybenzylidene) -4,4' -bipyridine dichloride serving as a ligand 2 O 3 Eu formation in nanorod dispersion 2 O 3 Ultrasonic dissolving the mixed solution of the nano rod and the ligand for 5-10 min to obtain uniform Eu 2 O 3 A dispersion of nanorods and ligands; the Eu 2 O 3 The mass ratio of the nanorods to the di-N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine is 1: (1-2);
s3, eu is added 2 O 3 Transferring the dispersion liquid of the nanorods and the ligand into an autoclave, placing the autoclave into an oven, heating to 100-120 ℃, performing solvothermal reaction, then standing for 48-72 h, and naturally cooling to room temperature to obtain a reaction product;
s4, carrying out repeated centrifugal separation and ultrasonic washing on the reaction product for a plurality of times at room temperature, 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 nano-sheet, wherein the chemical formula of the photochromic metal-organic framework two-dimensional nano-sheet is as follows:
[Eu 2 (OH) 2 (H 2 O) 2 L]Cl 2 ·8H 2 O，
wherein L is N, N '-bis (3, 5-dicarboxybenzylidene) -4,4' -bipyridine.
2. The method for preparing the two-dimensional nano-sheet of the photochromic metal-organic framework according to claim 1, which is characterized in that: the Eu 2 O 3 The nanorods are prepared by a solid-phase thermal decomposition method, and the Eu is prepared by a solid-phase thermal decomposition method 2 O 3 The length of the nano rod is 500 nm-800 nm, and the diameter is 80 nm-150 nm.
3. The method for preparing the two-dimensional nano-sheet of the photochromic metal-organic framework according to claim 1, which is characterized in that: the mixing volume ratio of the acetonitrile and water mixed reagent is that: water= (2-4): 1.
4. a photochromic metal-organic framework two-dimensional nanoplatelet made by the method of claim 1, characterized in that: the thickness of a single piece of the two-dimensional nano sheet of the photochromic metal-organic framework is 10 nm-50 nm, and the side length of the single piece is 400 nm-2000 nm.
5. The photochromic metal-organic framework two-dimensional nanoplatelets of claim 4, wherein: under the condition of ultraviolet lamp irradiation, the two-dimensional nano sheet of the photochromic metal-organic framework can generate reversible photochromic phenomenon.
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