CN102872728A - 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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- CN102872728A CN102872728A CN2012103834665A CN201210383466A CN102872728A CN 102872728 A CN102872728 A CN 102872728A CN 2012103834665 A CN2012103834665 A CN 2012103834665A CN 201210383466 A CN201210383466 A CN 201210383466A CN 102872728 A CN102872728 A CN 102872728A
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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 the method that a kind of hydroxide nano line and organic ligand prepare metal organic frame thing film.
Background technology
Metal organic frame thing film has preferably application prospect because it has the chemical stability that high porosity is become reconciled in many fields such as adsorbing separation, catalytic reaction, pharmaceutical carrier and optical materials.Metal current organic frame thing thin film technology method has a lot, and more traditional solvent-thermal method, layer by layer are wherein arranged, and sol-gal process, colloidal deposition method and relatively more novel microwave process for synthesizing, electrochemical synthesis etc.But these methods still exist many drawbacks: although easier such as the solvent-thermal method preparation, its synthetic is difficult to produce fine and close film take powder as main; The difficult unification of film thickness that sol-gal process and colloidal deposition legal system are standby, uniformity is bad; The 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 objective 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 prepare metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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 obtained inculating crystal layer after 48 hours;
3) inculating crystal layer is joined contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 3mM, the trimesic acid of 2mM, solvent are in the mixed solution of ethanol, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 10～25 μ m after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand prepare metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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 terephthalic acids solution of DMF, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours;
3) inculating crystal layer is joined 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 thick metal organic frame thing film of 10～25 μ m after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand prepare metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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, solvent is that 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours in the 2-certain herbaceous plants with big flowers base-terephthalic acids solution of DMF;
3) inculating crystal layer is joined 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 thick metal organic frame thing film of 10～25 μ m after 24 hours.
The present invention generates one deck inculating crystal layer by filtering the reaction of nano wire and organic ligand, generates metal organic frame thing film by diauxic growth again.The cost of the standby film of this legal system is low, simple to operate, can stable existence, and repeatable strong, be convenient to large-scale promotion, enlarged the range of application of metal organic frame thing film.Especially the introducing of nano wire layer can obtain by simple filter method in the macropore substrate, its surface with positive charge can carry out effectively complexing with carboxylate radical in the organic ligand, generate the inculating crystal layer of one deck densification, be conducive to diauxic growth subsequently.
Description of drawings
Fig. 1 is that metallic hydrogen cupric oxide nano line and organic ligand prepare 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 prepare metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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 obtained inculating crystal layer after 48 hours;
3) inculating crystal layer is joined contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 3mM, the trimesic acid of 2mM, solvent are in the mixed solution of ethanol, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 10～25 μ m after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand prepare metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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 terephthalic acids solution of DMF, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours;
3) inculating crystal layer is joined 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 thick metal organic frame thing film of 10～25 μ m after 24 hours.
The step of method that another kind of hydroxide nano line and organic ligand prepare metal organic frame thing film is as follows:
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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, solvent is that 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours in the 2-certain herbaceous plants with big flowers base-terephthalic acids solution of DMF;
3) inculating crystal layer is joined 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 thick metal organic frame thing film of 10～25 μ m after 24 hours.
Further specify the present invention below in conjunction with example.
Embodiment 1
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in the 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 at multiaperture pellumina form the thick filtering layer of one deck 300nm 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, solvent is in the trimesic acid solution of ethanol, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours; 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, solvent is in the mixed solution of ethanol, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 12.5 μ m after 24 hours.
Embodiment 2
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in the 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 at multiaperture pellumina form the thick filtering layer of one deck 600nm 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, solvent is in the trimesic acid solution of ethanol, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours; 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, solvent is in the mixed solution of ethanol, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 25 μ m after 24 hours.See Fig. 3.
Embodiment 3
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in the 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 at multiaperture pellumina form the thick filtering layer of one deck 600nm 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, solvent is in the terephthalic acids solution of DMF, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours;
3) inculating crystal layer of gained is joined to contain 40ml concentration be the copper nitrate of 2mM and the terephthalic acids of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 25 μ m after 24 hours.
Embodiment 4
1) under magnetic agitation, the 1.4 mM monoethanolamine aqueous solution are added with in the 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 at multiaperture pellumina form the thick filtering layer of one deck 600nm 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, solvent is that 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours in the 2-certain herbaceous plants with big flowers base-terephthalic acids solution of DMF;
3) inculating crystal layer of gained is joined contain copper nitrate that 40ml concentration is 2mM and 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 thick metal organic frame thing film of 25 μ m after 24 hours.
Embodiment 5
1) under magnetic agitation, the 2.4 mM monoethanolamine aqueous solution are added with in the 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 at multiaperture pellumina form the thick filtering layer of one deck 600nm 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, solvent is in the trimesic acid solution of DMF, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours;
3) inculating crystal layer of gained is joined to contain 40ml concentration be the zinc nitrate of 3mM and the trimesic acid of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 25 μ m after 24 hours.
Embodiment 6
1) under magnetic agitation, the 1.6 mM monoethanolamine aqueous solution are added with in the 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 at multiaperture pellumina form the thick filtering layer of one deck 600nm 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, solvent is in the trimesic acid solution of DMF, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours;
3) inculating crystal layer of gained is joined to contain 40ml concentration be the cadmium nitrate of 3mM and the trimesic acid of 2mM, solvent is in the mixed solution of DMF, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 25 μ m after 24 hours.
Claims (3)
1. a hydroxide nano line and organic ligand prepare the 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 with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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 obtained inculating crystal layer after 48 hours;
3) inculating crystal layer is joined contain copper nitrate, zinc nitrate or the cadmium nitrate that 40ml concentration is 3mM, the trimesic acid of 2mM, solvent are in the mixed solution of ethanol, and 120 ℃ of heat treatments obtain the thick metal organic frame thing film of 10～25 μ m after 24 hours.
2. a hydroxide nano line and organic ligand prepare the 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 with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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 terephthalic acids solution of DMF, and 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours;
3) inculating crystal layer is joined 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 thick metal organic frame thing film of 10～25 μ m after 24 hours.
3. a hydroxide nano line and organic ligand prepare the 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 with in volume 4 mM copper nitrates, zinc nitrate or the cadmium nitrate aqueous solution, after 1 minute, slow down mixing speed, and reaction vessel sealed, after 12～36 hours, obtain Kocide SD, zinc hydroxide or cadmium hydroxide nanowires solution, nano wire solution 10～25 ml are directly filtered the thick nano wire layer at multiaperture pellumina formation one deck 300～600nm, 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, solvent is that 120 ℃ of heat treatments obtained inculating crystal layer after 48 hours in the 2-certain herbaceous plants with big flowers base-terephthalic acids solution of DMF;
3) inculating crystal layer is joined 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 thick metal organic frame thing film of 10～25 μ m after 24 hours.
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| CN104497017A (en) * | 2014-12-11 | 2015-04-08 | 浙江大学 | Method for growing metal-organic framework seeds in gelatin layer |
| 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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