CN105668548B - The method that core shell structure customizes high dispersive codope porous carbon - Google Patents
The method that core shell structure customizes high dispersive codope porous carbon Download PDFInfo
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Abstract
The method that core shell structure customizes high dispersive codope porous carbon, belongs to porous carbon materials and technical field of graphene.Metal-organic framework materials of the selection containing specific objective element are shell, using the nano particle of the metal component containing low boiling as core, the presoma for possessing core shell structure is formed, after adding small molecule carbon source or nitrogen source, codope porous carbon materials are prepared by temperature programming tube furnace high temperature cabonization.This method can easily be realized codoping modified to the multiple element of carbon material.The high temperature sublimation energy effective activation target material of low boiling core component so that doped chemical is uniformly dispersed.This method accurately can control codope element by screening parent, so as to realize the customization of high dispersive codope porous carbon.
Description
Technical field
The present invention relates to it is a kind of by core shell structure customize high dispersive codope porous carbon method, belong to porous carbon materials and
Technical field of graphene.
Background technology
Porous carbon materials refer to the carbon material with Different Pore Structures, and its aperture can be according to the requirement of practical application (such as
Institute's binding molecule size etc.) regulated and controled, its size is between the nanometer level microporous macropore to micron order.Porous carbon materials have
Have the property of carbon material, as chemical stability height, good conductivity, it is cheap the advantages that；Meanwhile the introducing of pore structure makes its same
When have the characteristics that specific surface area is big, pore passage structure is controllable, aperture is adjustable.Porous carbon materials are in gas separation, the purification of water, color
Spectrum analysis, catalysis and the field such as photocatalysis and energy stores are widely used.
The preparation method of porous carbon materials is varied, conventional preparation method:
Mainly using silica as template hard template method (Jun S, Joo SH, Ryoo R, Kruk M, Jaroniec M,
Liu Z,Ohsuna T,Terasaki O.Synthesis of New Nanoporous Carbon with Hexagonally
Ordered Mesostructure[J].J.Am.Chem.Soc.,2000,122(43):10712-10713)；Soft template method (Li
Z,Yan W,Dai S.A Novel Vesicular Carbon Synthesized Using Amphiphilic
Carbonaceous Material and Micelle Templating Approach[J].Carbon,2004,42(4):
767-770)；Activation method (Jagtoyen M, Derbyshire F.Activated Carbons from Yellow Poplar
and White Oak by H3PO4Activation[J].Carbon,1998,36(7-8):1085-1097)；Miscellaneous element doping
Modified (Zhao Y, Liu X, Yao KX, Zhao L, Han Y.Superior Capture of CO2Achieved by
Introducing Extra-Framework Cations into N-Doped Microporous Carbon[J]
.Chem.Mater.,2012,24(24):4725-4734) etc..However, go deep into research, for multiple element codope
The demand more and more higher of material.Existing porous carbon materials method of modifying, often adulterated just for single element；It is doped element such as
Precious metals pt or organic element P, N etc., at the defects of can be only present in carbon material mostly, its be distributed and reunite it is unmanageable,
And it is available for the element species of doping limited, partial picture also needs to the auxiliary synthesis of expensive device.Therefore, it is necessary to design one kind
Method, multielement codope can be both realized with easy-to-use, and the element energy high uniformity adulterated is dispersed in target material
In.
The content of the invention
First technical problem to be solved by this invention is provided a kind of with high electricity for the above-mentioned state of the art
The preparation method of chemical property multiple element codope porous carbon materials, it is easy to operate, easily realize, can scale synthesis and environment
It is friendly.
Second technical problem to be solved by this invention is that have that a variety of different parents are available, codope element
Species and ratio are controllable.
3rd technical problem to be solved by this invention is that codope element can be achieved to be uniformly distributed.
4th technical problem to be solved by this invention be available with core shell structure fully activate from inside to outside it is porous
Carbon material.
Technical scheme is used by the present invention solves above-mentioned technical problem：The present invention is with the change of the metallic element containing low boiling
The nano particle of compound is as core, to enter one containing core shell structure of the MOF materials as shell for needing to be adulterated object element, core shell structure
Step and secondary carbon or carbon nitrogen source (carbon, carbon nitrogen source are preferably small molecule) are mixed to get core shell structure presoma, before core shell structure
During driving the high temperature cabonization of body under anaerobic, the core component in composite construction vaporizes at high temperature, realizes to material
Pore-creating and activation, finally give codope porous carbon materials.
The present invention passes through from volatile under different MOF material precursors metallic compound and organic ligand, with high temperature
Metal compound nanoparticles customization core shell structure, using this core shell structure as presoma, in temperature programming tube furnace, height
High dispersive codope porous carbon materials are prepared in temperature carbonization.Pass through ESEM, transmission electron microscope, Raman spectrum, X-ray diffraction etc.
It is high dispersive codope porous carbon materials that a series of signs, which demonstrate prepared material,.
The available MOF materials of the present invention：MOF-1, MOF-5, MOF-74, ZIF-7, ZIF-8, ZIF-9, ZIF-64,
ZIF-67, MIL-53 (Al), MIL-53 (Cr), MIL-53 (Fe), Cr-MIL-101, NH2The number such as-MIL101 (Al), HKUST-1
Ten even hundreds of material.Prepared by the present invention contains when needing to be adulterated the MOF material shells of object element using preparation MOF
The metal ligand and organic ligand of material precursor.
The volatile metal of the present invention refers to that boiling point is less than 1000 DEG C of metal；Volatile metallic compound nano
Grain optional metal oxide nanoparticles such as ZnO, CdO, other kinds of metallic compound such as potassium carbonate nano particle, carbonic acid
Sodium nano particle, or MOF (such as ZIF-7, ZIF-8) material of the metallic element containing low boiling.
The method that the present invention prepares core shell structure presoma, comprises the following steps：
The metal ligand used for preparing MOF materials is mixed by a certain percentage with volatile metal compound nanoparticles
Together in absolute methanol, solution 1 is obtained, the organic ligand used for preparing MOF materials is dissolved in other absolute methanol, obtained
Solution 2；Solution 2 is added into solution 1, stirred, filtering；Vacuum drying treatment is carried out to obtained mixing material, is then carbon
Source and nitrogen source are mixed in absolute methanol, are stirred, and are filtered, and washing, after drying process, obtain core shell structure presoma.
Washing solid portion is washed with absolute methanol.
If the volatile metal compound nanoparticles of the present invention select metal oxide nanoparticles, metal oxide
The mol ratio of nano particle/metal ligand/absolute methanol is (0.01-1):(1-9.99)：(10-999), metal ligand with it is organic
Part ratio is (0.01-1):(1-9.99).The molar ratio range of metal ligand/carbon source/nitrogen source is 0.1:1:1 to 1:1:1:
10。
The method that high temperature cabonization presoma prepares high dispersive codope porous carbon materials, comprises the following steps：
Obtained core shell structure presoma is placed in tube furnace, before being heated up to tube furnace, first vacuumized, with
Just the gas and other impurities adsorbed in removal system, is passed through inert gas；Then it is raised to from room temperature with 1-20 DEG C/min speed
A certain value in 100-500 DEG C, is incubated 1-5h at such a temperature, then heats to carbonization final temperature with 1-20 DEG C/min speed
A certain value between 300-1500 DEG C of degree, it is incubated 30min-5h, natural cooling room temperature, you can obtain high dispersive codope porous carbon
Material.The final temperature temperature of any technical scheme is above the holding temperature of centre.
Inert gas includes nitrogen, argon gas, helium, neon, Krypton, xenon or radon gas.
Compared with prior art, this method preparation process is simple, easy to operate, can customize multielement codope substantially
Porous carbon materials, doped chemical content and the regulation and control of decentralization of product material can be realized according to the application field of material, also may be used
Regulate and control the degree of graphitization of char-forming material according to preparation process.
Brief description of the drawings
Fig. 1 is codope porous carbon materials synthetic method schematic diagram in embodiment 1.
Fig. 2 is presoma X-ray diffractogram in embodiment 1.
Fig. 3 is the electron scanning micrograph of presoma in embodiment 1.
Fig. 4 is the transmission electron microscope photo of presoma in embodiment 1.
Fig. 5 is porous carbon materials Raman spectrogram in embodiment 1.
Fig. 6 is the distribution diagram of element of porous carbon materials in embodiment 1.
Fig. 7 is the electron scanning micrograph of porous carbon materials in embodiment 1.
Fig. 8 is the transmission electron microscope photo of porous carbon materials in embodiment 1.
Fig. 9 is the nitrogen adsorption curve of porous carbon materials in embodiment 1.
Figure 10 is the pore-size distribution of porous carbon materials in embodiment 1.
Figure 11 is the electron scanning micrograph of porous carbon materials in embodiment 2.
Figure 12 is the electron scanning micrograph of presoma in embodiment 2.
Figure 13 is the electron scanning micrograph of porous carbon materials in embodiment 2.
Specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.Experimental drug derives from commercial channel (Ark
Pharm, Inc., Mai Kelin, An Naiji, Chinese medicines group), do not purify further unless otherwise indicated；
Embodiment 1：Prepare the porous carbon materials of cation doping and nitrogen
The first step：By 0.25g ZnO nanos particle and 1g cabaltous nitrate hexahydrates (Co (NO3)·6H2O) it is mixed in 200ml first
In alcohol, 30min is stirred, obtains solution 1；2.23g 2-methylimidazoles are dissolved in 200ml absolute methanols, it is ultrasonic to completely molten
Solution, obtains solution 2.Solution 2 is slowly added into solution 1, stirs 10h.Products therefrom 1 filters, and is washed with 3*5ml absolute methanols
Wash, be dried overnight at 130 DEG C.Take the 0.14g of product 1 to be dissolved in 0.7g melamines and 0.7g urea in absolute methanol, stir
20h, filtering solution, precipitation is washed with 3*5ml absolute methanols, and under vacuum condition, temperature 60 C dries 3h, obtains product 2, i.e.,
The presoma of core shell structure.
Second step：The presoma that quality is 0.5g is placed in tube furnace, before being heated up to tube furnace, first taken out true
Sky, then pass to inert gas.Then 300 DEG C are raised to from room temperature with 6 DEG C/min, are incubated 3h at such a temperature, then with 3 DEG C/
Min is heated to 950 DEG C, is incubated 120min.It is cooled to room temperature, you can obtain high dispersive Co, the N codope porous carbon materials of black
Carbon-Z1。
Embodiment 2：The porous carbon materials of cation doping and nitrogen are prepared using CdO as core
The first step：By 0.40g CdO nano particles and 1g cabaltous nitrate hexahydrates (Co (NO3)·6H2O) it is mixed in 200ml first
In alcohol, 30min is stirred, obtains solution 1；2.23g 2-methylimidazoles are dissolved in 200ml absolute methanols, it is ultrasonic to completely molten
Solution, obtains solution 2.Solution 2 is slowly added into solution 1, stirs 10h.Products therefrom 1 filters, and is washed with 3*5ml absolute methanols
Wash, be dried overnight at 130 DEG C.Take the 0.14g of product 1 to be dissolved in 0.7g melamines and 0.7g urea in absolute methanol, stir
20h, filtering solution, precipitation is washed with 3*5ml absolute methanols, and under vacuum condition, temperature 60 C dries 3h, obtains product 2, i.e.,
The presoma of core shell structure.
Second step：The presoma that quality is 0.5g is placed in tube furnace, before being heated up to tube furnace, first taken out true
Sky, then pass to inert gas.Then 300 DEG C are raised to from room temperature with 6 DEG C/min, are incubated 3h at such a temperature, then with 3 DEG C/
Min is heated to 850 DEG C, is incubated 120min.It is cooled to room temperature, you can obtain high dispersive Co, the N codope porous carbon materials of black
Carbon-Z2。
Embodiment 3：The porous carbon materials of cation doping and nitrogen are prepared using ZIF-8 as core
The first step：By 1g zinc nitrate hexahydrates (Zn (NO3)·6H2O) it is dissolved in 200ml methanol, stirs 30min, obtain
Solution 1；2.23g 2-methylimidazoles are dissolved in 200ml absolute methanols, ultrasound obtains solution 2 to being completely dissolved.By solution 2
It is slowly added into solution 1, stirs 0.5h.Centrifuged 10 minutes under 10000R/min rotating speeds and obtain ZIF-8 nano particles, use 3*5ml
Absolute methanol washs, and is dried overnight at 60 DEG C.
Second step：By the 0.40g ZIF-8 nano particles in the first step and 1g cabaltous nitrate hexahydrates (Co (NO3)·H2O) mix
Together in 200ml methanol, 30min is stirred, obtains solution 3；2.23g 2-methylimidazoles are dissolved in 200ml absolute methanols, surpassed
Sound obtains solution 4 to being completely dissolved.Solution 4 is slowly added into solution 3, stirs 10h.Products therefrom 1 filters, with 3*5ml without
Water methanol washs, and is dried overnight at 130 DEG C.The 0.14g of product 1 is taken to be dissolved in absolute methanol with 0.7g melamines and 0.7g urea
In, 20h is stirred, filtering solution, precipitation is washed with 3*5ml absolute methanols, and under vacuum condition, temperature 60 C dries 3h, obtains
The presoma of product 2, i.e. core shell structure.
3rd step：The presoma that quality is 0.5g is placed in tube furnace, before being heated up to tube furnace, first taken out true
Sky, then pass to inert gas.Then 300 DEG C are raised to from room temperature with 6 DEG C/min, are incubated 3h at such a temperature, then with 3 DEG C/
Min is heated to 850 DEG C, is incubated 120min.It is cooled to room temperature, you can obtain high dispersive Co, the N codope porous carbon materials of black
Carbon-Z3。
The x-ray diffractogram of powder of presoma is as shown in Figure 2.In PXRD figures, presoma can be significantly observed
Diffraction maximum is substantially almost completely overlapped with the peak of ZIF-67 and ZnO nano particle.Transmission electron microscope picture such as Fig. 3 institutes of presoma
Show, can substantially observe ZnO lattice diffraction fringe.Fig. 2 forms ZIF-67 bags to Fig. 4 union declarations, presoma really
Wrap up in ZnO core shell structure.
Typically there is three peaks, D peaks (1360cm in the Raman spectrum of graphene-1), G peaks (1580cm-1) and 2D peaks
(2720cm-1Left and right).G peaks are by all sp in carbocyclic ring or long-chain2Caused by the extensional motion of atom pair, defect and unordered lure
Lead the generation at D peaks, the peak intensity at D peaks characterize non-graphitized boundary number in material number, that is, the non-graphitized knot of random layer
Structure.The double resonance Raman Process that 2D peaks participate in originating from two opposite phonons of momentum.In all sp by chemical preparation2Carbon
It is found in material.As shown in Fig. 5 Raman spectrograms, G peak intensities are slightly below D peaks, because the doping of miscellaneous element makes carbon
Caused by the lattice of atom is destroyed.800cm in Fig. 5-1Metal cobalt/cobalt oxide in the peak respective material of left and right.
Fig. 6 shows the C of porous carbon materials, N, Co, O Elemental redistribution, can substantially observe, Co, and N element is uniform
It is distributed in porous carbon materials.
Fig. 8 is the transmission electron microscope photo of porous carbon materials, it can be seen that the lattice fringe of Co elements, Co do not reunite.
Fig. 9 is porous carbon materials nitrogen adsorption curve, and its BET specific surface area is about 226m2/g。
Figure 10 is the pore-size distribution of porous carbon materials, it can be seen that is micropore and structure that is mesoporous and depositing.
Claims (6)
1. the method that core shell structure customizes high dispersive codope porous carbon, it is characterised in that with the change of the metallic element containing low boiling
The nano particle of compound is as core, to enter one containing core shell structure of the MOF materials as shell for needing to be adulterated object element, core shell structure
Step is mixed to get core shell structure presoma, the high temperature cabonization of core shell structure presoma under anaerobic with secondary carbon or carbon nitrogen source
During, the core component in composite construction vaporizes at high temperature, realizes pore-creating and activation to material, it is more to finally give codope
Hole carbon material；
The method for wherein preparing core shell structure presoma, comprises the following steps：
The metal ligand used for preparing MOF materials is mixed in by a certain percentage with volatile metal compound nanoparticles
Absolute methanol, solution 1 is obtained, the organic ligand used for preparing MOF materials is dissolved in other absolute methanol, obtains solution
2；Solution 2 is added into solution 1, stirred, filtering；Vacuum drying treatment is carried out to obtained mixing material, then again with carbon source and
Nitrogen source is mixed in absolute methanol, is stirred, and is filtered, and washing, after drying process, obtains core shell structure presoma；
Volatile metal refers to that boiling point is less than 1000 DEG C of metal.
2. the method that the core shell structure according to claim 1 customizes high dispersive codope porous carbon, it is characterised in that MOF materials
Selected from MOF-1, MOF-5, MOF-74, ZIF-7, ZIF-8, ZIF-9, ZIF-64, ZIF-67, MIL-53 (Al), MIL-53 (Cr),
MIL-53 (Fe), Cr-MIL-101, NH2- MIL101 (Al) or HKUST-1.
3. the method that the core shell structure according to claim 1 customizes high dispersive codope porous carbon, it is characterised in that volatile
Metal compound nanoparticles select metal oxide nanoparticles, then metal oxide nanoparticles：Metal ligand：Without water beetle
The mol ratio of alcohol is (0.01-1):(1-9.99)：(10-999), metal ligand and organic ligand mol ratio are (0.01-1):(1-
9.99)。
4. the method that the core shell structure according to claim 1 customizes high dispersive codope porous carbon, it is characterised in that volatile
Metal compound nanoparticles select metal oxide nanoparticles, potassium carbonate nano particle, sodium carbonate nano particle, or containing low
The MOF materials of boiling point metallic element.
5. the method that the core shell structure according to claim 1 customizes high dispersive codope porous carbon, it is characterised in that high temperature cabonization
The method that presoma prepares high dispersive codope porous carbon materials, comprises the following steps：Obtained core shell structure presoma is put
In tube furnace, before being heated up to tube furnace, first vacuumize, so that the gas and other that are adsorbed in removal system are miscellaneous
Matter, it is passed through inert gas；Then from room temperature with 1-20 DEG C/min speed be raised to 100-500 DEG C insulation 1-5h, then with 1-20 DEG C/
Min speed heats to 300-1500 DEG C of insulation 30min-5h of carbonization finishing temperature, natural cooling room temperature, you can obtain high dispersive
Codope porous carbon materials.
6. the method that the core shell structure according to claim 5 customizes high dispersive codope porous carbon, it is characterised in that inert gas
Selected from nitrogen, argon gas, helium, neon, Krypton, xenon or radon gas.
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| CN108374179B (en) * | 2018-02-07 | 2019-05-14 | 浙江大学 | A kind of preparation method and application of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping |
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