CN107151331A - A kind of method of the quick preparation structure controllable metal organic framework compounds of electrochemical method - Google Patents
A kind of method of the quick preparation structure controllable metal organic framework compounds of electrochemical method Download PDFInfo
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- CN107151331A CN107151331A CN201710414235.9A CN201710414235A CN107151331A CN 107151331 A CN107151331 A CN 107151331A CN 201710414235 A CN201710414235 A CN 201710414235A CN 107151331 A CN107151331 A CN 107151331A
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Abstract
The present invention relates to a kind of method of the quick preparation structure controllable metal organic framework compounds of electrochemical method.Present invention electro synthesis metal organic framework (MOF) material in a variety of both macro and micro conductive substrates by a simple and quick step electro synthesis method.And by regulating and controlling the species of organic ligand and metal ion, concentration, ratio in electrolyte solution, and electro synthesis voltage, time etc., oriented growth of a variety of MOFs materials in different type both macro and micro conductive substrates is realized, and its particle size and pattern can be with artificial adjustments.Electrochemical method for synthesizing generated time is short, and operating process is simple, and can be completed in room temperature condition, is that follow-up extension preparation and industrial applications provide condition.In addition, prepared new MOFs thin-film materials are respectively provided with quite wide application prospect in terms of electrolysis water oxygen evolution reaction (OER), electrode material for super capacitor (SCs), lithium ion battery electrode material, bio-sensing.
Description
Technical field
The invention belongs to metal-organic framework material synthesis field, more particularly to a kind of quick preparation structure of electrochemical method
The method of controllable metal organic framework compounds.
Background technology
Metal organic framework compound (metal-organic frameworks, MOFs), also makes metal organic coordination gather
Compound (metal-organic coordination polymers, MOCP), is to pass through coordination by metal ion and organic ligand
Act on a kind of inorganic-organic hybridization functional material of assembling.The multiple tooth organic ligand of metal ion and nitrogenous, oxygen etc. (is mostly
Fragrant polybase or polyacid) self assembly forms and possesses the material of special pore passage structure, wherein metal ion as skeleton structure section
Point, organic ligand turns into the bridged group for connecting these nodes.This metal-organic framework materials can be by different organic
Part is complexed with a variety of metal ions, so as to design and control the pore structure in skeleton so that such material
The features such as with various, the high specific area in structure-rich, adjustable, duct and easily realizing functionalization, in drier, catalyst, suction
Fufen is from numerous field extensive applications such as, optical material, medical diagnosis, electricity, magnetic material, storage gases.At present
Conventional synthetic method has the hot method of hydrothermal/solvent, diffusion method, microwave synthesis and ultrasound synthesis etc., and these methods are different degrees of
On there are problems that HTHP highly energy-consuming, synthesis technique it is complicated, to consersion unit and environmental requirement.In order to avoid above-mentioned
Problem present in these methods, it is proposed that a kind of clean electrochemistry formated new approaches of normal temperature and pressure, in a variety of macroscopic views and
Electro synthesis metal organic framework in conductive microstructure substrate, realize metal-organic framework materials nanometer aspect oriented growth and
Artificial adjustment.
The content of the invention
The present invention is single for the metal organic framework pattern prepared in the prior art, the problems such as building-up process is uncontrollable,
Using a quick and easy step electro synthesis method, a variety of gold are prepared for by electrochemistry formated in both macro and micro conductive substrates
Belong to organic backbone nano material.
A kind of method that electrochemistry quickly prepares metal organic framework compound, prepares the electricity containing organic ligand and metal salt
Electrolyte solution, using potentiostatic method, synthesizes metal organic framework nano material in conductive substrates.
It is preferred that, the organic ligand is selected from 1,2- methylimidazoles, methylimidazole, terephthalic acid (TPA) or trimesic acid
In one or more.
It is preferred that, the metal salt is selected from Zn (NO3)2、Co(NO3)2、Ni(NO3)2、Fe(NO3)3、Cu(NO3)2、Al
(NO3)3、Mg(NO3)2、In(NO3)2、Tb(NO3)2、Eu(NO3)2、ZnCl2、CoCl2、NiCl2、FeCl2、FeCl3、MgCl2、
ZnSO4、CoSO4、NiSO4、FeSO4、Fe2(SO4)3Or MgSO4In one or more.
It is preferred that, the organic solvent of the electrolyte solution is in methanol, ethanol, acetone or DMF
One or more.
It is preferred that, the conductive substrates include macroscopical conductive substrates, selected from nickel foam, ITO, FTO, nickel sheet, titanium sheet, copper
One or more in net, carbon cloth or electrically conducting transparent cloth.
It is preferred that, the conductive substrates include conductive microstructure substrate, cobalt aluminum hydrotalcite are grown in nickel foam, in nickel sheet
Cobalt aluminum hydrotalcite is grown on developing zinc oxide, electro-conductive glass, grows on copper sheet and grows zinc-aluminum hydrotalcite on cupro-nickel hydrotalcite, zinc metal sheet
In one or more.
It is preferred that, in the electrolyte solution metal salt concentrations are 0.1g/mL-1g/mL, and organic ligand and metal salt rub
You are than being 1:10-10:1.
It is preferred that, the conductive substrates are as working electrode, and saturated calomel electrode is as reference electrode, and platinum filament is as to electricity
Pole；Current potential sets scope to be -0.5 to -5V, and generated time is 5-300s, and synthesis temperature scope is 10-50 DEG C.
It is preferred that, methods described also includes the cleaning treatment step of conductive substrates：By conductive substrates respectively with absolute ethyl alcohol,
Acetone and each ultrasonic 10-20min of deionized water, remove the impurity on surface.
The advantage of the invention is that：The present invention is led using a simple and quick step electro synthesis method in a variety of both macro and micros
Electro synthesis metal organic framework in electric substrate, realizes metal-organic framework materials in the oriented growth of nanometer aspect and artificial tune
Control, by regulating and controlling the ratio and electro synthesis voltage, time of organic ligand in electrolyte solution etc., the life to metal organic framework
Long situation can be regulated and controled well, reach that performance is optimal.The method can be completed in room temperature condition, and generated time is short, synthesizes
Journey is simple.The nano material is in electrolysis water oxygen evolution reaction (OER), electrode material for super capacitor (SCs), lithium ion cell electrode
Quite wide application prospect is respectively provided with terms of material, bio-sensing.
Brief description of the drawings
Fig. 1 is on FTO surfaces to synthesize the schematic flow sheet of ZIF-67 nano materials in embodiment 1.
Fig. 2 is on FTO surfaces to synthesize the scanning electron microscope (SEM) photograph of ZIF-67 nano materials in embodiment 1.
Fig. 3 is the schematic flow sheet for synthesizing ZIF-67 nano materials in embodiment 2 on CoAl-LDH@Ni foam.
Fig. 4 is the scanning electron microscope (SEM) photograph for synthesizing ZIF-67 nano materials in embodiment 2 on CoAl-LDH Ni foam.
Embodiment
Further detailed description will be carried out by embodiment and with reference to accompanying drawing to the present invention below, but embodiment is not
For limiting the scope of the invention.
【Embodiment 1】
ZIF-67 nano materials are synthesized on FTO surfaces：
a:Conductive substrates FTO is used into absolute ethyl alcohol, acetone and each ultrasonic 10min of deionized water respectively, the miscellaneous of surface is removed
Matter；
b:Prepare 1mg/mL cobalt nitrates (Co (NO3)2), 0.5mg/mL1,2- methylimidazoles, the mixed solution 50mL of methanol
It is used as electrolyte solution；
c:In the electrolyte solution that step b is prepared, using FTO as working electrode, saturated calomel electrode is used as reference electricity
Pole, platinum filament be to electrode, using potentiostatic method on FTO direct growth ZIF-67, the current potential of electrochemistry formated is set to -0.9V,
Generated time is 200s, and synthesis temperature is 25 DEG C.
【Embodiment 2】
ZIF-67 nano materials are synthesized on CoAl-LDH@Ni foam：
a:Conductive substrates Ni foam are used into absolute ethyl alcohol, acetone and each ultrasonic 10min of deionized water respectively, surface is removed
Impurity；
b：The Ni foam obtained by a steps 1mg/mL cobalt nitrates (Co (NO have been immersed in3)2) and 1mg/mL nitric acid
Aluminium (Al (NO3)3) and the high-temperature high-pressure reaction kettle of 1mg/mL urea in, reactor is put into baking oven, reacts 24 small at 110 DEG C
When, obtain the CoAl-LDH i.e. CoAl-LDH@Ni foam grown on Ni foam.
c:Prepare 1mg/mL cobalt nitrates (Co (NO3)2), the mixed solution of 0.5mg/mL1,2- methylimidazoles and methanol
50mL is used as electrolyte solution；
d:In the electrolyte solution that step c is prepared, CoAl-LDH@Ni foam are regard as working electrode, saturation calomel electricity
Pole as reference electrode, platinum filament be to electrode, using potentiostatic method on CoAl-LDH@FTO direct growth ZIF-67, electrochemistry
The current potential of synthesis is set to -0.9V, and generated time is 200s, and synthesis temperature is 25 DEG C.
【Embodiment 3】
ZIF-8 nano materials are synthesized on ZnO@Ni foil：
a:Conductive substrates Ni foil are used into absolute ethyl alcohol, acetone and each ultrasonic 10min of deionized water respectively, surface is removed
Impurity；
b：The Ni foil obtained by a steps are immersed in the 100mL absolute ethyl alcohols containing 0.06M zinc acetates, 350
Calcined 30 minutes at DEG C.Ni foil after calcining are put into containing 0.06M zinc nitrates and 0.06M hexas (HMT)
In high-temperature high-pressure reaction kettle, after being reacted 24 hours at 100 DEG C, it is washed with deionized water and ethanol, is dried to obtain at room temperature
The ZnO nano-rod array grown on Ni foil, i.e. ZnO@Nifoil.
c:Prepare 1mg/mL zinc nitrates (Zn (NO3)2), 0.5mg/mL1,2- methylimidazoles, the mixed solution 50mL of methanol
It is used as electrolyte solution；
d:In the electrolyte solution that step c is prepared, using ZnO@Ni foil as working electrode, saturated calomel electrode is made
For reference electrode, platinum filament be to electrode, using potentiostatic method on ZnO@Ni foil direct growth ZIF-67, electrochemistry formated
Current potential be set to -0.9V, generated time is 200s, and synthesis temperature is 25 DEG C.
【Embodiment 4】
Cu is synthesized on copper wire3(BTC)2Nano material：
a:Conductive substrates copper wire is used into absolute ethyl alcohol, acetone and each ultrasonic 10min of deionized water respectively, the miscellaneous of surface is removed
Matter；
b:Prepare 1mg/mL copper nitrates (Cu (NO3)2) and 0.5mg/mL trimesic acid and the mixed solution 50mL of ethanol
It is used as electrolyte solution；
c:In the electrolyte solution that step b is prepared, using copper wire as working electrode, saturated calomel electrode is used as reference electricity
Pole, platinum filament be to electrode, using potentiostatic method on copper wire direct growth Cu3(BTC)2, the current potential of electrochemistry formated is set to-
0.9V, generated time is 200s, and synthesis temperature is 25 DEG C.
【Embodiment 5】
Zn is synthesized on zinc metal sheet3(BTC)2Nano material：
a:Conductive substrates zinc metal sheet is used into absolute ethyl alcohol, acetone and each ultrasonic 10min of deionized water respectively, the miscellaneous of surface is removed
Matter；
b:Prepare 1mg/mL zinc nitrates (Zn (NO3)2) and 0.5mg/mL trimesic acid and the mixed solution 50mL of ethanol
It is used as electrolyte solution；
c:In the electrolyte solution that step b is prepared, using zinc metal sheet as working electrode, saturated calomel electrode is used as reference electricity
Pole, platinum filament be to electrode, using potentiostatic method on zinc metal sheet direct growth Zn3(BTC)2, the current potential of electrochemistry formated is set to-
0.9V, generated time is 200s, and synthesis temperature is 25 DEG C.
Present invention electro synthesis in a variety of both macro and micro conductive substrates by a simple and quick step electro synthesis method
Metal organic framework (MOF) material.And by regulate and control the species of organic ligand and metal ion in electrolyte solution, concentration,
Ratio, and electro synthesis voltage, time etc., a variety of MOFs materials are realized in different type both macro and micro conductive substrates
Oriented growth, and its particle size and pattern can be with artificial adjustments.Electrochemical method for synthesizing generated time is short, operating process letter
It is single, and can be completed in room temperature condition, it is that follow-up extension preparation and industrial applications provide condition.In addition, prepared
New MOFs thin-film materials are in electrolysis water oxygen evolution reaction (OER), electrode material for super capacitor (SCs), lithium ion cell electrode
Quite wide application prospect is respectively provided with terms of material, bio-sensing.
It is understood that above is in order to illustrate the principle of the present invention and the example of exploitativeness, not office of the invention
It is limited to this.For those skilled in the art, without departing from the spirit and substance in the present invention, can be with
All variations and modifications are made, these variations and modifications are also considered as protection scope of the present invention.
Claims (9)
1. a kind of method that electrochemistry quickly prepares metal organic framework compound, it is characterised in that prepare containing organic ligand and
The electrolyte solution of metal salt, using potentiostatic method, synthesizes metal organic framework nano material in conductive substrates.
2. the method that electrochemistry according to claim 1 quickly prepares metal organic framework compound, it is characterised in that institute
State the one or more that organic ligand is selected from 1,2- methylimidazoles, methylimidazole, terephthalic acid (TPA) or trimesic acid.
3. the method that electrochemistry according to claim 2 quickly prepares metal organic framework compound, it is characterised in that institute
State metal salt and be selected from Zn (NO3)2、Co(NO3)2、Ni(NO3)2、Fe(NO3)3、Cu(NO3)2、Al(NO3)3、Mg(NO3)2、In
(NO3)2、Tb(NO3)2、Eu(NO3)2、ZnCl2、CoCl2、NiCl2、FeCl2、FeCl3、MgCl2、ZnSO4、CoSO4、NiSO4、
FeSO4、Fe2(SO4)3Or MgSO4In one or more.
4. the method that electrochemistry according to claim 3 quickly prepares metal organic framework compound, it is characterised in that institute
The organic solvent for stating electrolyte solution selection is the one or more in methanol, ethanol, acetone or N,N-dimethylformamide.
5. the method that electrochemistry according to claim 4 quickly prepares metal organic framework compound, it is characterised in that institute
Stating conductive substrates includes macroscopical conductive substrates, selected from nickel foam, ITO, FTO, nickel sheet, titanium sheet, copper mesh, carbon cloth or transparent leads
One or more in electric cloth.
6. the method that electrochemistry according to claim 5 quickly prepares metal organic framework compound, it is characterised in that institute
Conductive substrates are stated including conductive microstructure substrate, cobalt aluminum hydrotalcite are grown in nickel foam, developing zinc oxide, conductive glass in nickel sheet
Cobalt aluminum hydrotalcite is grown on glass, one or more on cupro-nickel hydrotalcite, zinc metal sheet in growth zinc-aluminum hydrotalcite are grown on copper sheet.
7. the method that electrochemistry according to claim 6 quickly prepares metal organic framework compound, it is characterised in that institute
It is 0.1g/mL-1g/mL to state in electrolyte solution metal salt concentrations, and the mol ratio of organic ligand and metal salt is 1:10-10:1.
8. the method that the electrochemistry according to any one in claim 1 to 7 quickly prepares metal organic framework compound,
Characterized in that, the conductive substrates are as working electrode, saturated calomel electrode as reference electrode, platinum filament as to electrode,
Current potential sets scope to be -0.5 to -5V, and generated time is 5-300s, and synthesis temperature scope is 10-50 DEG C.
9. the method that electrochemistry according to claim 8 quickly prepares metal organic framework compound, it is characterised in that institute
Stating method also includes the cleaning treatment step of conductive substrates：Conductive substrates are each with absolute ethyl alcohol, acetone and deionized water respectively
Ultrasonic 10-20min, removes the impurity on surface.
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| CN108531938A (en) * | 2018-05-02 | 2018-09-14 | 北京化工大学 | A kind of three-dimensional multistage structure cobalt nickel aluminium ternary metal elctro-catalyst and its preparation and application for oxygen evolution reaction |
| CN108752368A (en) * | 2018-07-11 | 2018-11-06 | 郑州工程技术学院 | A kind of zinc-containing metal organic framework materials and its synthetic method and application with fluorescence identifying performance |
| CN109036875A (en) * | 2018-04-10 | 2018-12-18 | 新乡学院 | Zn adulterates Ni-MOF self-supporting combination electrode and its preparation method and application |
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