CN102872728B - Method for preparing metal organic framework film by using hydroxide nanowires and organic ligands - Google Patents
Method for preparing metal organic framework film by using hydroxide nanowires and organic ligands Download PDFInfo
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Abstract
The invention discloses a method for preparing a metal organic framework film by using hydroxide nanowires and organic ligands. The method includes steps: (1) under magnetic stirring, ethanol amine water solution is filled into cupric nitrate, zinc nitrate or cadmium nitrate water solution with the same volume, the stirring speed is slowed, corresponding copper hydroxide, zinc hydroxide or cadmium hydroxide nanowire solution is obtained, and the nanowire solution is directly filtered on a porous alumina film to form a nanowire layer; (2) the nanowire layer is filled into organic ligand solution with ethanol or N,N-dimethylformamide serving as the solvent, and a seed crystal layer is obtained after heat treatment; and (3) the seed crystal layer is filled into organic ligand mixed solution containing cupric nitrate, zinc nitrate or cadmium nitrate, and the metal organic framework film is obtained after heat treatment. The seed crystal layer can directly grow on a porous substrate; and the method is simple to operate and low in cost, can be used for preparing films with large area and capable of existing stably, and enlarges the application range of the metal organic framework film.
Description
Technical field
The present invention relates to the preparation method of microporous membrane, relate in particular to a kind of method that hydroxide nano line and organic ligand are prepared metal organic frame thing film.
Background technology
Metal organic frame thing film, because it has the chemical stability that high porosity is become reconciled, has good application prospect in many fields such as adsorbing separation, catalytic reaction, pharmaceutical carrier and optical materials.The preparation method of metal current organic frame thing film has a lot, wherein has more traditional solvent-thermal method, layer by layer, and sol-gal process, colloidal deposition method and more novel microwave process for synthesizing, electrochemical synthesis etc.But these methods still exist many drawbacks: although as easier in solvent-thermal method preparation, its synthetic, take powder as main, is difficult to produce fine and close film; The more difficult unification of film thickness that sol-gal process and colloidal deposition legal system are standby, uniformity is bad; Layer by layer step is more loaded down with trivial details, and the film growth cycle is long; Microwave process for synthesizing and electrochemical synthesis immature development, production cost is higher.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of hydroxide nano line and organic ligand to prepare the method for metal organic frame thing film.
The step of method that a kind of hydroxide nano line and organic ligand are prepared metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer is joined to contain 10～20ml concentration be 10mM, solvent is in the trimesic acid solution of ethanol or DMF, and 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 3mM, the trimesic acid of 2mM, in the mixed solution that solvent is ethanol, 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand are prepared metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer is joined to contain 10～20ml concentration be 10mM, in the terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 2mM, the terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand are prepared metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 10～20ml concentration be 10mM, in 2-certain herbaceous plants with big flowers base-terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 2mM, 2-certain herbaceous plants with big flowers base-terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
The present invention reacts generation one deck inculating crystal layer by filtering nano wire with organic ligand, then generates metal organic frame thing film by diauxic growth.This legal system is low for the cost of film, simple to operate, can stable existence, and repeatable strong, be convenient to large-scale promotion, expand the range of application of metal organic frame thing film.Especially the introducing of nano wire layer can obtain by simple filter method in macropore substrate, its surface with positive charge can carry out complexing effectively with carboxylate radical in organic ligand, generate the inculating crystal layer of one deck densification, be conducive to diauxic growth subsequently.
Accompanying drawing explanation
Fig. 1 is that metallic hydrogen cupric oxide nano line and organic ligand are prepared metal organic frame thing film flow chart;
Fig. 2 is the surperficial SEM photo of the inculating crystal layer of Kocide SD nano wire and trimesic acid formation;
Fig. 3 is the surperficial SEM photo of the metal organic frame thing film of Kocide SD nano wire and trimesic acid formation.
The specific embodiment
The step of method that a kind of hydroxide nano line and organic ligand are prepared metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer is joined to contain 10～20ml concentration be 10mM, solvent is in the trimesic acid solution of ethanol or DMF, and 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 3mM, the trimesic acid of 2mM, in the mixed solution that solvent is ethanol, 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand are prepared metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer is joined to contain 10～20ml concentration be 10mM, in the terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 2mM, the terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand are prepared metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 10～20ml concentration be 10mM, in 2-certain herbaceous plants with big flowers base-terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 2mM, 2-certain herbaceous plants with big flowers base-terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
Further illustrate the present invention below in conjunction with example.
Embodiment 1
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrate aqueous solutions, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD nano wire solution, Kocide SD nano wire solution 30 ml are directly filtered and on multiaperture pellumina, form filtering layer that one deck 300nm is thick as nano wire layer, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 10ml concentration be 10mM, in the trimesic acid solution that solvent is ethanol, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer; See Fig. 2;
3) inculating crystal layer of gained is joined to contain 20ml concentration be the copper nitrate of 3mM and the trimesic acid of 2mM, in the mixed solution that solvent is ethanol, 120 ℃ of heat treatments obtain the metal organic frame thing film that 12.5 μ m are thick after 24 hours.
Embodiment 2
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrate aqueous solutions, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD nano wire solution, Kocide SD nano wire solution 60 ml are directly filtered and on multiaperture pellumina, form filtering layer that one deck 600nm is thick as nano wire layer, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 20ml concentration be 10mM, in the trimesic acid solution that solvent is ethanol, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer; See Fig. 2.
3) inculating crystal layer of gained is joined to contain 40ml concentration be the copper nitrate of 3mM and the trimesic acid of 2mM, in the mixed solution that solvent is ethanol, 120 ℃ of heat treatments obtain the metal organic frame thing film that 25 μ m are thick after 24 hours.See Fig. 3.
Embodiment 3
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrate aqueous solutions, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD nano wire solution, Kocide SD nano wire solution 60 ml are directly filtered and on multiaperture pellumina, form filtering layer that one deck 600nm is thick as nano wire layer, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 20ml concentration be 10mM, in the terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer of gained is joined to contain 40ml concentration be the copper nitrate of 2mM and the terephthalic acids of 2mM, in the mixed solution that solvent is DMF, 120 ℃ of heat treatments obtain the metal organic frame thing film that 25 μ m are thick after 24 hours.
Embodiment 4
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrate aqueous solutions, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD nano wire solution, Kocide SD nano wire solution 60 ml are directly filtered and on multiaperture pellumina, form filtering layer that one deck 600nm is thick as nano wire layer, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 20ml concentration be 10mM, in 2-certain herbaceous plants with big flowers base-terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer of gained is joined and contain copper nitrate that 40ml concentration is 2mM and 2-certain herbaceous plants with big flowers base-terephthalic acids of 2mM, in the mixed solution that solvent is DMF, 120 ℃ of heat treatments obtain the metal organic frame thing film that 25 μ m are thick after 24 hours.
Embodiment 5
1) under magnetic agitation, the 2.4 mM monoethanolamine aqueous solution are added in same volume 4 mM zinc nitrate aqueous solutions, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 30 minutes, obtain zinc hydroxide nano-wire solution, zinc hydroxide nano-wire solution 60 ml are directly filtered and on multiaperture pellumina, form filtering layer that one deck 600nm is thick as nano wire layer, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 20ml concentration be 10mM, in the trimesic acid solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer of gained is joined to contain 40ml concentration be the zinc nitrate of 3mM and the trimesic acid of 2mM, in the mixed solution that solvent is DMF, 120 ℃ of heat treatments obtain the metal organic frame thing film that 25 μ m are thick after 24 hours.
Embodiment 6
1) under magnetic agitation, the 1.6 mM monoethanolamine aqueous solution are added in the same volume 4 mM cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 30 minutes, obtain cadmium hydroxide nanowires solution, cadmium hydroxide nanowires solution 60 ml are directly filtered and on multiaperture pellumina, form filtering layer that one deck 600nm is thick as nano wire layer, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 20ml concentration be 10mM, in the trimesic acid solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer of gained is joined to contain 40ml concentration be the cadmium nitrate of 3mM and the trimesic acid of 2mM, in the mixed solution that solvent is DMF, 120 ℃ of heat treatments obtain the metal organic frame thing film that 25 μ m are thick after 24 hours.
Claims (3)
1. hydroxide nano line and organic ligand are prepared a method for metal organic frame thing film, it is characterized in that its step is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 mL are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer is joined to contain 10～20mL concentration be 10mM, solvent is in the trimesic acid solution of ethanol or DMF, and 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40mL concentration is 3mM, the trimesic acid of 2mM, in the mixed solution that solvent is ethanol, 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
2. hydroxide nano line and organic ligand are prepared a method for metal organic frame thing film, it is characterized in that its step is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 mL are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer is joined to contain 10～20mL concentration be 10mM, in the terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40mL concentration is 2mM, the terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
3. hydroxide nano line and organic ligand are prepared a method for metal organic frame thing film, it is characterized in that its step is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added in same volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel is sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 mL are directly filtered and on multiaperture pellumina, form the nano wire layer that one deck 300～600nm is thick, the diameter of multiaperture pellumina is 2.5 cm, aperture 200 nm, porosity 25～50%;
2) nano wire layer of gained is joined to contain 10～20mL concentration be 10mM, in 2-certain herbaceous plants with big flowers base-terephthalic acids solution that solvent is DMF, 120 ℃ of heat treatments, after 48 hours, obtain inculating crystal layer;
3) inculating crystal layer is joined and contain copper nitrate, zinc nitrate or the cadmium nitrate that 40mL concentration is 2mM, 2-certain herbaceous plants with big flowers base-terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the metal organic frame thing film that 10～25 μ m are thick after 24 hours.
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| CN103570755A (en) * | 2013-10-25 | 2014-02-12 | 浙江大学 | Method of assisted-synthesizing metallic aluminum organic framework object nanorod array on aluminum oxide macroporous substrate through hydroxide nanowire |
| CN104230962B (en) * | 2014-08-21 | 2016-06-08 | 浙江大学 | A kind of method preparing mesoporous metal organic framework structure crystal |
| CN104497017B (en) * | 2014-12-11 | 2016-08-24 | 浙江大学 | A kind of method growing Metal-organic frame seed in gelatin layer |
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| CN109208030B (en) * | 2018-11-16 | 2020-04-17 | 北京师范大学 | Metal hydroxide-metal organic framework composite material and preparation method thereof |
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| CN109776831B (en) * | 2019-03-20 | 2022-04-05 | 福州大学 | Rapid preparation method of self-supporting hydroxide film and metal organic framework film |
| CN112646212B (en) * | 2020-10-29 | 2021-11-09 | 浙江大学 | Preparation method of polyaniline-coated metal organic framework nano-array film, product and application thereof |
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| CN102489183B (en) * | 2011-12-16 | 2015-05-20 | 中国科学院宁波材料技术与工程研究所 | Metal-organic framework (MOF) material for permeating and separating gases and preparation method thereof |
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