CN109205567A - A method of metal oxide multilevel structure is prepared using the derivative bimetallic oxide template of MOF - Google Patents
A method of metal oxide multilevel structure is prepared using the derivative bimetallic oxide template of MOF Download PDFInfo
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Abstract
The present invention relates to technical field of nano material more particularly to a kind of methods for preparing metal oxide multilevel structure using the derivative bimetallic oxide template of MOF, and the derivative bimetallic oxide template of MOF is obtained metal oxide multilevel structure by alkali process；M is set as the metal in the metal oxide multilevel structure, the derivative bimetallic oxide template of the MOF is MMoO4- MOF derives bimetallic oxide, and the metal oxide multilevel structure is MxOy.Preparation process of the present invention is simple, mild, pervasive, to equipment without particular/special requirement, does not use surfactant, can large-scale industrialized production；The metal oxide multilevel structure size uniformity prepared using this method, stable structure, composite distribution are uniform.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of derivative bimetallic oxide template systems of utilization MOF
The method of standby metal oxide multilevel structure.
Background technique
The nano material of multilevel structure studies this concern since its excellent physicochemical properties has caused extensively.
It can be the whole knot of material since nanoscale basic unit provides high surface area, high surface volume ratio, surface functional group
Structure provides ideal mechanical performance and chemical property.Provide for material supply section scholar is by stringent group from molecule to macro-scale
It knits principle and forms structure, the multistage material formed in any level can produce functional material more.
Micro-nano multi-level structure metal oxide has unique physicochemical properties, in many necks such as the energy, environment, catalysis
Domain has broad application prospects, it has also become the focus and emphasis of current nano materials research.Existing multilevel structure metal oxygen
Compound is prepared with sol-gal process, hydro-thermal method etc., and it is soft template that the above method, which mostly uses surfactant, in preparation process
In there is template removal is not clean, the problems such as being easily introduced impurity, need individually to go the processing step of removing template, greatly increase
The complication of technique, and it is few to prepare yield, is unfavorable for extensive industrialized development；Hydro-thermal method some need to have using toxic
Solvent is unfavorable for environmental protection.
Summary of the invention
The present invention is in order to overcome INVENTIONConventional metal-oxide multilevel structure preparation process multiple dependent on surfactant, technique
It is miscellaneous, be not easy the problem of industrialization, provide and a kind of prepare metal oxide multistage knot using the derivative bimetallic oxide template of MOF
The method of structure, preparation process is simple, mild, pervasive, does not use surfactant, is suitable for large-scale industrialized production.
To achieve the goals above, the invention adopts the following technical scheme:
A method of metal oxide multilevel structure being prepared using the derivative bimetallic oxide template of MOF, by the derivative double gold of MOF
Belong to oxide template and obtains metal oxide multilevel structure by alkali process；M is set as in the metal oxide multilevel structure
Metal, the derivative bimetallic oxide template of the MOF is MMoO4- MOF derives bimetallic oxide, the metal oxide
Multilevel structure is MxOy。
Metal-organic framework materials (Metal-organic frameworks, MOF) are metal ion and organic ligand knot
With the crystal of porous network structure made of conjunction, the cellular structure with high-sequential, bigger specific surface area is more connect
Touch active site.The metal oxide obtained using MOFs as precursor preparation usually has adjustable porous structure, the present invention
By controlling pattern, the Nomenclature Composition and Structure of Complexes of MOFs presoma, the derivative bimetallic oxide template of MOF is obtained, using from sacrificial mold
Plate method obtains metal oxide multilevel structure after alkali process, realizes effective adjusting of metal oxide component and structure.
Preferably, the MMoO4The preparation method of-MOF material, comprising the following steps:
(1) by MoO3With 2-methylimidazole aqueous dissolution in deionized water, the water-soluble salt solution of M is added, is heated to 80
It~180 DEG C, is stirred to react 10~18h and M/Mo-MOF material is made after cooling, washing, drying；
(2) by M/Mo-MOF material high-temperature calcination under air atmosphere made from step (1), MMoO is obtained4- MOF is derivative double
Metal oxide.
Preferably, the temperature of high-temperature calcination is 300~900 DEG C in step (2)；Calcination time be 1~for 24 hours；Heating speed
Rate is 1~20 DEG C/min.
Preferably, concentration is used to carry out alkali process for the KOH solution of 0.01~10mol/L.
Preferably, concentration is used to carry out alkali process for the KOH solution of 0.1mol/L.
Preferably, the MMoO4The derivative bimetallic oxide of-MOF and OH-The ratio between the amount of substance be 1:(1~100).
Preferably, the MMoO4The derivative bimetallic oxide of-MOF and OH-The ratio between the amount of substance be 1:25.
Preferably, by MMoO4The derivative bimetallic oxide of-MOF stands 0.5~8h in KOH solution, obtains metal
Oxide multilevel structure MxOy。
Preferably, MMoO4The derivative bimetallic oxide of-MOF time of repose in KOH solution is 6h.
Preferably, the M is selected from one kind of Mn, Cu, Zn, Fe, Mg and Al.
Therefore, the invention has the following beneficial effects:
(1) preparation process is simple, mild, pervasive, to equipment without particular/special requirement, does not use surfactant, can extensive industry
Metaplasia produces；
(2) the metal oxide multilevel structure size uniformity prepared using this method, stable structure, composite distribution are uniform.
Detailed description of the invention
Fig. 1 is the appearance structure figure of product prepared by embodiment 1:
Mn/Mo-MOF(a,b,b1,b2)；MnMoO4- MOF (c, d, e)；Mn3O4Multilevel structure (f).
Fig. 2 is the XRD spectra of Mn/Mo-MOF prepared by embodiment 1.
Fig. 3 is MnMoO prepared by embodiment 14The XRD spectra of-MOF.
Fig. 4 is Mn prepared by embodiment 13O4The XRD spectra of multilevel structure.
Specific embodiment
Below by specific embodiment, and in conjunction with attached drawing, the technical solutions of the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed conventional method in that art.
Embodiment 1
(1) clean beaker is taken, 25ml deionized water is added, weighs 0.5g MoO3It pours into deionized water, weighs 0.475g
2-methylimidazole pours into deionized water, ultrasonic dissolution.A clean beaker is separately taken, is added in 25ml deionized water, weighs 0.26g
Mn(NO3)2·4H2O is poured into deionized water, ultrasonic dissolution, and MoO is added in manganese nitrate solution3In solution.Oil bath heating is to 120
DEG C, it is stirred to react 12h, reaction is down to room temperature after stopping naturally.Deionized water centrifuge washing, in triplicate.And it is true at 60 DEG C
The dry 12h of sky.Mn/Mo-MOF is made；
(2) it takes appropriate Mn/Mo-MOF to place in ship type crucible, crucible is placed among quartz ampoule, in air atmosphere in tube furnace
Lower 500 DEG C of high-temperature oxydation 3h are enclosed, heating rate is 10 DEG C/min.MnMoO is made4- MOF crystal powder；
(3) 10mg MnMoO is taken4- MOF is placed in a clean container, and the KOH solution that 10ml concentration is 0.1mol/L is added,
MnMoO4The ratio between amount of substance of-MOF and OH- is 1:25；6h is stood at room temperature, after reaction, product is transferred to centrifugation
Guan Zhong is repeated 3 times with deionized water centrifuge washing, be placed at 60 DEG C of vacuum drying oven dry 12h, Mn is made3O4Multistage knot
Structure.
Mn/Mo-MOF, MnMoO prepared by embodiment 14- MOF and Mn3O4Multilevel structure does following characterization:
(1) morphology analysis:
Sem analysis:
SEM test carries out in HITACHI S-4700 scanning electron microscope, and sample used is the preparation method is as follows: take on a small amount of
State resulting Mn/Mo-MOF crystal powder, MnMoO4Crystal powder, Mn3O4Multilevel structure powder is placed in the support for posting conducting resinl
Platform surface then puts it into SEM chamber and is tested.
High-resolution tem analysis:
TEM test carried out on JEOL 2010F type transmission electron microscope, sample used the preparation method is as follows: taking above-mentioned reality
Apply the preparation gained Mn/Mo-MOF of example 3 crystal powder, MnMoO4Crystal powder, Mn3O4Multilevel structure powder is micro, is added dropwise respectively about
1ml deionized water, ultrasonic disperse 10min take a small amount of dispersion liquid to be added dropwise using drip method in band micro-grid copper mesh table to being uniformly dispersed
Film (is supported containing microporous carbon) in face, is placed in and spontaneously dries at room temperature.
Mn/Mo-MOF crystal powder, MnMoO obtained in embodiment 14- MOF crystal powder, Mn3O4Multilevel structure powder
The SEM figure at end is with TEM figure as shown in Figure 1, the whole pattern that Fig. 1 (a, b) illustrates Mn/Mo-MOF material is the smooth stick in surface
Shape structure.Fig. 1 (b1, b2) shows that Mn/Mo-MOF has good crystallinity, and stable structure, component is uniform.Fig. 1 (c, d) is shown
By MnMoO made from high-temperature oxydation4The whole pattern of material is club shaped structure.Fig. 1 (e) shows MnMoO4- MOF has good
Good crystallinity, stable structure, component are uniform.Fig. 1 (f) illustrates Mn3O4The whole pattern of multilevel structure material is Mn3O4It receives
Rice piece intersects the club shaped structure to be formed.
Fig. 2-Fig. 4 gives Mn/Mo-MOF crystal powder, the MnMoO prepared in embodiment 14- MOF crystal powder, Mn3O4
The wide-angle XRD spectra of multilevel structure powder shows that gained Mn/Mo-MOF crystalline material has good crystallinity in Fig. 2, with figure
1 (b1, b2) shows that result is consistent, illustrates successfully to synthesize Mn/Mo-MOF material, and Fig. 3 is by MnMoO obtained by high-temperature oxydation4Powder
The XRD spectrum at end, diffraction maximum and MnMoO in figure4Standard card (PDF#50-1287) is consistent, it was demonstrated that successfully synthesizes MnMoO4Material
Material.Fig. 4 is by Mn obtained by dipping by lye3O4The XRD spectrum of multilevel structure powder, diffraction maximum and Mn in figure3O4Standard card
(PDF#24-0734) consistent, it was demonstrated that successfully to synthesize Mn3O4Multilevel structure material.
Embodiment 2
(1) clean beaker is taken, 25ml deionized water is added, weighs 0.5g MoO3It pours into deionized water, weighs 0.475g
2-methylimidazole pours into deionized water, ultrasonic dissolution.A clean beaker is separately taken, is added in 25ml deionized water, weighs 0.26g
Mn(NO3)2·4H2O is poured into deionized water, ultrasonic dissolution, and MoO is added in manganese nitrate solution3In solution.Oil bath heating is to 80
DEG C, it is stirred to react 180h, reaction is down to room temperature after stopping naturally.Deionized water centrifuge washing, in triplicate.And it is true at 60 DEG C
The dry 12h of sky.Mn/Mo-MOF is made；
(2) it takes appropriate Mn/Mo-MOF to place in ship type crucible, crucible is placed among quartz ampoule, in air atmosphere in tube furnace
Enclose lower 300 DEG C of high-temperature oxydations for 24 hours, heating rate is 1 DEG C/min.MnMoO is made4- MOF crystal powder；
(3) 10mg MnMoO is taken4- MOF is placed in a clean container, and the KOH solution that 10ml concentration is 0.01mol/L is added,
MnMoO4The ratio between amount of substance of-MOF and OH- is 1:1.6h is stood at room temperature, after reaction, product is transferred to centrifuge tube
In, with deionized water centrifuge washing, be repeated 3 times, be placed at 60 DEG C of vacuum drying oven dry 12h.Mn is made3O4Multilevel structure.
Embodiment 3
(1) clean beaker is taken, 25ml deionized water is added, weighs 0.5g MoO3It pours into deionized water, weighs 0.475g
2-methylimidazole pours into deionized water, ultrasonic dissolution.A clean beaker is separately taken, is added in 25ml deionized water, weighs 0.26g
Mn(NO3)2·4H2O is poured into deionized water, ultrasonic dissolution, and MoO is added in manganese nitrate solution3In solution.Oil bath heating is to 180
DEG C, it is stirred to react 12h, reaction is down to room temperature after stopping naturally.Deionized water centrifuge washing, in triplicate.And it is true at 60 DEG C
The dry 12h of sky.Mn/Mo-MOF is made；
(2) it takes appropriate Mn/Mo-MOF to place in ship type crucible, crucible is placed among quartz ampoule, in air atmosphere in tube furnace
Lower 900 DEG C of high-temperature oxydation 1h are enclosed, heating rate is 20 DEG C/min.MnMoO is made4- MOF crystal powder；
(3) 10mg MnMoO is taken4- MOF is placed in a clean container, and the KOH solution that 10ml concentration is 10mol/L is added,
MMoO4The ratio between the derivative bimetallic oxide of-MOF and the amount of substance of OH- are 1:100；6h is stood at room temperature, after reaction,
Product is transferred in centrifuge tube, with deionized water centrifuge washing, is repeated 3 times, be placed at 60 DEG C of vacuum drying oven it is dry
Mn is made in 12h3O4Multilevel structure.
Embodiment 4
(1) clean beaker is taken, 25ml deionized water is added, weighs 0.5g MoO3It pours into deionized water, weighs 0.475g
2-methylimidazole pours into deionized water, ultrasonic dissolution.A clean beaker is separately taken, is added in 25ml deionized water, weighs
0.306g Zn(NO3)2·6H2O is poured into deionized water, ultrasonic dissolution, and MoO is added in zinc nitrate solution3In solution.Oil bath adds
Heat is stirred to react 12h to 120 DEG C, and reaction is down to room temperature after stopping naturally.Deionized water centrifuge washing, in triplicate, and in 60
It is dried in vacuo 12h at DEG C, Zn/Mo-MOF is made；
(2) it takes appropriate Zn/Mo-MOF to place in ship type crucible, crucible is placed among quartz ampoule, in air atmosphere in tube furnace
Lower 800 DEG C of high-temperature oxydation 5h are enclosed, heating rate is 5 DEG C/min, and ZnMoO is made4- MOF crystal powder；
(3) 10mg ZnMoO is taken4MOF crystal powder is placed in a clean container, and it is molten that the KOH that 10ml concentration is 0.5mol/L is added
Liquid, ZnMoO4- MOF and OH-The ratio between the amount of substance be 1:25, stand 8h at room temperature, after reaction, by product be transferred to from
In heart pipe, with deionized water centrifuge washing, be repeated 3 times, be placed at 60 DEG C of vacuum drying oven dry 12h, obtain ZnO multistage
Structure.
Embodiment 5
(1) clean beaker is taken, 25ml deionized water is added, weighs 0.5g MoO3It pours into deionized water, weighs 0.475g
2-methylimidazole pours into deionized water, ultrasonic dissolution.A clean beaker is separately taken, is added in 25ml deionized water, weighs
0.386g Al(NO3)2·9H2O is poured into deionized water, ultrasonic dissolution, and MoO is added in aluminum nitrate solution3In solution.Oil bath adds
Heat is stirred to react 12h to 100 DEG C, and reaction is down to room temperature after stopping naturally.Deionized water centrifuge washing, in triplicate, and in 60
It is dried in vacuo 12h at DEG C, Al/Mo-MOF is made；
(2) it takes appropriate Al/Mo-MOF to place in ship type crucible, crucible is placed among quartz ampoule, in air atmosphere in tube furnace
Lower 350 DEG C of high-temperature oxydation 3h are enclosed, heating rate is 10 DEG C/min, and Al is made2(MoO4)3- MOF crystal powder；
(3) 10mg Al is taken2(MoO4)3- MOF crystal powder is placed in a clean container, and it is 0.1mol/L's that 10ml concentration, which is added,
KOH solution, Al2(MoO4)3- MOF and OH-The ratio between the amount of substance be 1:45, stand 10h at room temperature, after reaction, will produce
Object is transferred in centrifuge tube, with deionized water centrifuge washing, is repeated 3 times, be placed at 60 DEG C of vacuum drying oven dry 12h, i.e.,
Al is made2O3Multilevel structure.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, and is not surpassing
There are also other variations and modifications under the premise of technical solution documented by claim out.
Claims (10)
1. a kind of method for preparing metal oxide multilevel structure using the derivative bimetallic oxide template of MOF, which is characterized in that
The derivative bimetallic oxide template of MOF is obtained into metal oxide multilevel structure by alkali process；M is set to aoxidize as the metal
Metal in object multilevel structure, the derivative bimetallic oxide template of the MOF is MMoO4- MOF derives bimetallic oxide, institute
Stating metal oxide multilevel structure is MxOy。
2. a kind of derivative bimetallic oxide template of utilization MOF according to claim 1 prepares metal oxide multistage knot
The method of structure, which is characterized in that the MMoO4The preparation method of-MOF material, comprising the following steps:
(1) by MoO3With 2-methylimidazole aqueous dissolution in deionized water, the water-soluble salt solution of M is added, it is heated to 80~
It 180 DEG C, is stirred to react 6h or more and M/Mo-MOF material is made after cooling, washing, drying；
(2) by M/Mo-MOF material high-temperature calcination under air atmosphere made from step (1), MMoO is obtained4The derivative double gold of-MOF
Belong to oxide.
3. a kind of derivative bimetallic oxide template of utilization MOF according to claim 3 prepares metal oxide multistage knot
The method of structure, which is characterized in that it is characterized in that, the temperature of high-temperature calcination is 300~900 DEG C in step (2)；Calcination time
For 1~for 24 hours；Heating rate is 1~20 DEG C/min.
4. a kind of derivative bimetallic oxide template of utilization MOF according to claim 1 or 2 or 3 prepares metal oxide
The method of multilevel structure, which is characterized in that concentration is used to carry out alkali process for the KOH solution of 0.01~10mol/L.
5. a kind of derivative bimetallic oxide template of utilization MOF according to claim 4 prepares metal oxide multistage knot
The method of structure, which is characterized in that concentration is used to carry out alkali process for the KOH solution of 0.1mol/L.
6. a kind of derivative bimetallic oxide template of utilization MOF according to claim 4 prepares metal oxide multistage knot
The method of structure, which is characterized in that the MMoO4OH in the derivative bimetallic oxide of-MOF and KOH solution-The ratio between the amount of substance
For 1:(1~100).
7. a kind of derivative bimetallic oxide template of utilization MOF according to claim 4 prepares metal oxide multistage knot
The method of structure, which is characterized in that the MMoO4The derivative bimetallic oxide of-MOF and OH-The ratio between the amount of substance be 1:25.
8. a kind of described according to claim 1 or 5 or 6 or 7 prepare metal oxidation using the derivative bimetallic oxide template of MOF
The method of object multilevel structure, which is characterized in that by MMoO4- the derivative bimetallic oxide of MOF stands 0.5 in KOH solution~
8h obtains metal oxide multilevel structure MxOy。
9. a kind of derivative bimetallic oxide template of utilization MOF according to claim 8 prepares metal oxide multistage knot
The method of structure, which is characterized in that MMoO4The derivative bimetallic oxide of-MOF time of repose in KOH solution is 6h.
10. a kind of according to claim 1 or described in 9, using the derivative bimetallic oxide template of MOF to prepare metal oxide more
The method of level structure, which is characterized in that the M is selected from one kind of Mn, Cu, Zn, Fe, Mg and Al.
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