CN110289424A - A kind of preparation method of MOF derived carbon and cellular porous carbon composite - Google Patents
A kind of preparation method of MOF derived carbon and cellular porous carbon composite Download PDFInfo
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- CN110289424A CN110289424A CN201910612380.7A CN201910612380A CN110289424A CN 110289424 A CN110289424 A CN 110289424A CN 201910612380 A CN201910612380 A CN 201910612380A CN 110289424 A CN110289424 A CN 110289424A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention provides the preparation method of a kind of MOF derived carbon and cellular porous carbon composite, three-dimensional honeycomb shape porous carbon materials are prepared first, then in situ on it to load MOF, the cellular porous carbon composite of MOF derived carbon has been loaded finally by high temperature pyrolysis carbonization MOF.This method has advantage at low cost using cheap glucose, dicyandiamide, base metal salt, methylimidazole as raw material；The composite material of this method preparation can utilize the space structure advantage of cellular porous carbon material, in conjunction with the MOF derived carbon loaded on hole wall, pass through the regulation of the type of metal ion and organic ligand in MOF, various metals and nonmetal doping site are introduced into porous material, help to improve the reactivity and mass transfer advantage in electrochemical reaction of composite material.
Description
Technical field
The invention belongs to carbon material fields, and in particular to load MOF derived carbon in a kind of cellular porous carbon material surface
The composite material of layer.The material can be applied to the neck such as fuel cell, metal-air battery, lithium ion battery, solid state lithium battery
In domain.
Background technique
Carbon material is widely used in lithium ion battery, fuel cell, metal-air battery, solid state lithium battery, lithium-sulfur cell
And adsorbing separation field.Cellular porous carbon material be a kind of carbon plate/graphene wall in three dimensions relatively orderly connection,
The carbon material for forming class honeycomb-patterned ordered porous structure, is a kind of excellent bionical carbon material of structure.As catalyst material or
When electrode base material, the micropore in cellular porous carbon material can significantly improve the specific surface area of material, and macropore and
Meso-hole structure is conducive to provide internal quick mass transfer channel.This very good solution traditional active carbon, a wiener
When stacking and using the problem of mass transfer channel blocks easily occurs for rice carbon nanotube, two-dimensional graphene, non-ordered three-dimensional carbon material.Mesh
Before, cellular porous carbon material can be by with SiO2Ball, molecular sieve, surfactant and sodium chloride crystal etc. are template,
Cladding/absorption organic matter, is then carbonized-washes away template and obtain.However in many application fields, since carbon material itself is catalyzed
Activity or chemical reaction capacity limit, it would be desirable to element doping modification is carried out in the duct carbon wall of cellular porous carbon material
Deng improving the activity and selectivity to goal response with this.Patent CN109244489A uses surfactant aid dispersion
Method grown one layer of MOFs material on one-dimensional carbon nanotube surface.It increases the utilization efficiency of material surface and introduces activity
Site, but due to the limitation of one-dimensional base material so that the space efficiency of material entirety is not high.Document Advanced
Materials 2018,30 (30), 1802011 to report a kind of ultra-fine cobalt nanometer particle-carbon nanotube loaded in two-dimentional stone
The composite material of black alkene, but due to the plane property of two-dimensional material, so that space utilization rate is not also high.Patent
CN201811045264.3 reports a kind of preparation of three-dimensional grapheme load C oCu-MOF composite electrocatalyst, but electric from scanning
From the point of view of mirror figure, three-dimensional grapheme is not ordered porous structural, thus without the intrinsic excellent of the 3-D ordered multiporous carbon material of honeycomb
Gesture, while the unordered stacking of two-dimentional MOFs grown is also unfavorable for the exposure and mass transfer of active site.
To sum up, the document and patent of existing report, existing MOF derived carbon and one-dimensional or two-dimentional, three-dimensional carbon composite wood
There is no the advantages for playing MOF derived carbon and honeycomb-patterned ordered porous carbon materials for material.
Summary of the invention
The purpose of the present invention is to provide a kind of honeycomb-patterned ordered porous carbon composite (MOF for having loaded MOF derived carbon
Derived carbon/cellular porous carbon composite) and preparation method thereof, which utilizes honeycomb-patterned ordered porous carbon materials
Space structure advantage passes through the kind of metal ion and organic ligand in MOF in conjunction with the derivative carbon-coating of MOF loaded on hole wall
The regulation of class introduces a variety of nonmetallic and metal-doped carbon potential point into porous material, and the material helped to improve is in electrochemistry
Reactivity and reaction capacity in reaction.
The core technology feature that MOF derived carbon of the present invention/cellular porous carbon composite is different from current material is,
The derivative carbon-coating of MOF is loaded in situ on the carbon wall of cellular porous carbon material.The method for preparing the material is: first with carbon containing
The organic matter of nitrogen, using metal salt as carbided catalyst, passes through freeze-drying using NaCl template as template for carbon source and nitrogen source
Obtain the presoma of Coated with Organic Matter sodium chloride superfine crystal；Then being prepared for honeycomb by the method that high temperature pyrolysis is carbonized has
Sequence porous carbon material；Again by solvent-thermal method on the carbon wall of porous carbon materials one layer of MOF of homoepitaxial.Finally honeycomb is had
Sequence porous carbon materials MOF composite material, by obtaining a kind of the orderly of the uniform load derivative carbon-coating of MOF after secondary pyrolysis
Porous carbon materials material.Specifically, MOF derived carbon of the invention/cellular porous carbon composite is by following technology
Scheme is realized.
(1) by glucose, dicyandiamide and iron chloride (or cobalt chloride, nickel chloride) with quality than range be 100 ~ 1000:100
~ 1000:1 ~ 10 are added in saturated sodium chloride solution, after pouring into liquid nitrogen fast freezing after mixing evenly, are put into freeze drier
Middle freeze-drying obtains carbon materials material precursor.
(2) will in the tube furnace under resulting presoma argon atmosphere carry out high temperature pyrolysis carbonization, first with 2 ~ 10 DEG C/
Min is warming up to a certain temperature within the scope of 450 ~ 600 DEG C, is warming up to after constant temperature 30min ~ 3h a certain within the scope of 800 ~ 1000 DEG C
Temperature continues 2 h of constant temperature.After carbon material after pyrolysis is cooled to room temperature, impregnated using deionized water or 0.5 M H2SO4 solution
Template sodium chloride is removed, then obtains cellular porous carbon material by suction filtration process.
(3) cellular porous carbon material is added dissolved with Cu (NO3)2•3H2O、Zn(NO3)2•6H2O、Co(NO3)2•6H2O or
Ni(NO3)2•6H2In the methanol solution of one or both of O metal salt, 2-methylimidazole is added (or to benzene after impregnating 1 ~ 6 h
Dioctyl phthalate) methanol solution, by this mixed solution be added reaction kettle in by 90 ~ 150 DEG C reactions 3 ~ for 24 hours after, be cooled to room temperature
Afterwards, by filtering, methanol washing, the cellular porous carbon composite that MOF is loaded on drying to obtain carbon wall.
(4) above-mentioned 2 ~ 10 DEG C/min of porous carbon composite for having loaded MOF is warming up within the scope of 600 ~ 1100 DEG C
After a certain temperature, constant temperature is heat-treated 1 ~ 6 h, then cools to room temperature and has been loaded MOF derived carbon/honeycomb-patterned ordered porous carbon
Composite material.
Various specific chemical names in above-mentioned bracket are intended merely to provide specific example, it is not limited to this.
The positive effect of the present invention is as follows: (1) reagent used in entire preparation section be base metal salt, it is glucose, double
The cheap reagent such as cyanamide, non precious metal, without other surfaces activating agent etc adjuvant addition, material entirety synthesis cost and
Cost of material is lower；(2) honeycomb-patterned ordered porous carbon materials can promote the transfer of reactant, product in composite material, and
Provide the electron transmission carrier of high conductivity；(3) metal ion of load MOF can easily be regulated and controled using this method, had
The type and content of machine object ligand, it is thus possible to different active sites is introduced in composite system.(4) MOF is derivative
Carbon/honeycomb derived carbon and preparation method thereof also can be generalized to the composite material of other three-dimensional porous substrates and MOF derived carbon
Preparation.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of cellular porous carbon material employed in example 1 in the present invention.
Fig. 2 is gained MOF derived carbon/cellular porous carbon composite scanning electron microscope (SEM) photograph in example 1 in the present invention
(SEM).
Specific embodiment
Technical characteristic in order to better illustrate the present invention is illustrated below by specific embodiment
Embodiment 1
90 ml saturated sodium chloride solutions are added into beaker, then are separately added into 4 g glucose, 4 g dicyandiamides and 80 mg
FeCl3•6H2O forms uniform orange solution after being sufficiently stirred.After the liquid nitrogen instantaneous cooling solution is added, place it in cold
It is freeze-dried 24 h in lyophilizer, obtains solid powdery presoma.By presoma be added porcelain boat in, under argon atmosphere into
Row pyrolysis, 5 DEG C/min rise to 550 DEG C, and 5 DEG C/min is warming up to 900 DEG C again after 1 h of constant temperature, after 900 DEG C of 2 h of constant temperature
Natural cooling.By resulting black solid in 0.5 M H2SO4It after 6 h of middle immersion, filters, 80 DEG C of vacuum after deionized water washing
Cellular porous carbon material can be obtained in dry 12 h, and SEM figure is as shown in Figure 1.Then by the cellular porous carbon materials of 100 mg
Material and 50 mg Cu (NO3)2•3H2O, 300 mg Zn(NO3)2•6H2O is mixed in 100 ml methanol and is slowly stirred 7 h, later
100 ml are poured into carbon substrate metallic solution dissolved with the methanol solution of 530 mg 2-methylimidazoles, after 5 min are mixed
4 h are reacted under the conditions of 120 DEG C, after being cooled to room temperature, can be obtained after methanol suction filtration and 80 DEG C of 12 h of vacuum drying
The cellular porous carbon composite of CuZn-MOF/.200 mg CuZn-MOF/ honeycomb-patterned ordered porous carbon composites are poured into
After porcelain boat, 900 DEG C of progress high temperature pyrolysis are warming up to 5 DEG C/min under argon atmosphere, after 3 h of constant temperature after natural cooling to obtain the final product
To CuZn-MOF derived carbon/honeycomb-patterned ordered porous carbon composite.Fig. 2 is that there is gained MOF derived carbon/honeycomb in the present invention
The scanning electron microscope (SEM) photograph (SEM) of sequence porous carbon composite (Cu-ZIF-8@C).It is porous with CuZn-MOF derived carbon/honeycomb-patterned ordered
For carbon composite as fuel cell, the elctro-catalyst of metal-air battery anode oxygen reduction reaction, half wave potential reference can
Inverse hydrogen electrode (vs. RHE) is 0.86 V, is higher than business Pt/C catalyst.
Embodiment 2
Cellular porous carbon preparation process is same as Example 1, by the cellular porous carbon material of 200 mg and 100 mg Co
(NO3)2•6H2O, 500 mg Zn(NO3)2•6H2O is mixed in 100 ml methanol and is slowly stirred 7 h, backward carbon substrate metal
100 ml are poured into solution dissolved with the methanol solution of 670 mg 2-methylimidazoles, are mixed after 5 min in 110 DEG C of conditions
After being cooled to room temperature, CoZn-MOF/ honeycomb is can be obtained after methanol suction filtration and 80 DEG C of 12 h of vacuum drying in 6 h of lower reaction
Shape porous carbon composite.After 300 mg CuZn-MOF/ honeycomb-patterned ordered porous carbon composites are poured into porcelain boat, in argon gas
900 DEG C of progress high temperature pyrolysis are warming up to 5 DEG C/min under atmosphere, CoZn-MOF is obtained after natural cooling after 3 h of constant temperature and spreads out
Raw carbon/honeycomb-patterned ordered porous carbon composite.Using this CoZn-MOF derived carbon/honeycomb-patterned ordered porous carbon composite as
The elctro-catalyst of fuel cell, metal-air battery anode oxygen reduction reaction, half wave potential reference reversible hydrogen electrode (vs.
RHE) it is 0.86 V, is higher than business Pt/C catalyst.
Embodiment 3
Cellular porous carbon preparation process is same as Example 1, by the cellular porous carbon material of 200 mg and 100 mg Co
(NO3)2•6H2O, 500 mg Zn(NO3)2•6H2O is mixed in 100 ml methanol and is slowly stirred 7 h, backward carbon substrate metal
100 ml are poured into solution dissolved with the methanol solution of 670 mg 2-methylimidazoles, are mixed after 5 min in 110 DEG C of conditions
After being cooled to room temperature, CoZn-MOF/ honeycomb is can be obtained after methanol suction filtration and 80 DEG C of 12 h of vacuum drying in 6 h of lower reaction
Shape porous carbon composite.After 300 mg CuZn-MOF/ honeycomb-patterned ordered porous carbon composites are poured into porcelain boat, in argon gas
1000 DEG C of progress high temperature pyrolysis are warming up to 5 DEG C/min under atmosphere, CoZn-MOF is obtained after natural cooling after 3 h of constant temperature and spreads out
Raw carbon/honeycomb-patterned ordered porous carbon composite.Using this CoZn-MOF derived carbon/honeycomb-patterned ordered porous carbon composite as
The elctro-catalyst of fuel cell, metal-air battery anode oxygen reduction reaction, half wave potential reference reversible hydrogen electrode (vs.
RHE) it is 0.88 V, is higher than business Pt/C catalyst.
Claims (4)
1. a kind of preparation method of MOF derived carbon and cellular porous carbon composite, it is characterised in that: more in three-dimensional honeycomb shape
MOF is loaded on the carbon material of hole in situ, the three-dimensional honeycomb of MOF derived carbon has then been loaded by high temperature pyrolysis carbonization MOF
Shape porous carbon composite, the material it is specific the preparation method is as follows:
(1) glucose, dicyandiamide and Iron trichloride hexahydrate are added in saturated sodium chloride solution by a certain percentage, after mixing evenly
Liquid nitrogen fast freezing is poured into, is then placed in freeze drier and is lyophilized, obtain carbon materials material precursor；
(2) high temperature pyrolysis carbonization will be carried out in the tube furnace under resulting presoma argon atmosphere, be warming up to 450 ~ 600 first
Constant temperature 30 min ~ 3 h within the scope of DEG C is warming up to continuation 2 h of constant temperature, the carbon material after pyrolysis within the scope of 800 ~ 1000 DEG C later
After being cooled to room temperature, deionized water or 0.5 M H are used2SO4Solution, which impregnates, removes template sodium chloride, then by filtering
Journey obtains three-dimensional porous carbon material；
(3) three-dimensional honeycomb shape porous carbon materials are added dissolved in the methanol solution of transition metal salt, 2- methyl miaow is then added
This mixed solution is added in reaction kettle after 90 ~ 150 DEG C of reactions, is cooled to by the methanol solution of azoles (or terephthalic acid (TPA))
After room temperature, by suction filtration, the three-dimensional porous carbon composite for washing, being dried to obtain load MOF on carbon wall；
(4) constant temperature is heat-treated 1 ~ 6 h after being warming up to 600 ~ 1100 DEG C to the above-mentioned porous carbon composite for having loaded MOF, then
It is cooled to room temperature and has been loaded MOF derived carbon/3-D ordered multiporous carbon composite.
2. a kind of preparation method of MOF derived carbon and three-dimensional porous carbon composite as described in claim 1, it is characterised in that
The composite material can utilize the space structure advantage of three-dimensional honeycomb shape porous carbon materials, derivative in conjunction with the MOF loaded on hole wall
Carbon introduces various metals and non-gold into porous material by the regulation of the type of metal ion and organic ligand in MOF
Belong to doping site, helps to improve the reactivity and mass transfer advantage in electrochemical reaction of composite material.
3. a kind of preparation method of MOF derived carbon and three-dimensional porous carbon composite as described in claim 1, it is characterised in that
Iron chloride can be replaced with cobalt chloride or nickel chloride in step (1).
4. a kind of preparation method of MOF derived carbon and three-dimensional porous carbon composite as described in claim 1, it is characterised in that
Transition metal salt is Cu (NO3)2•3H2O、Zn(NO3)2•6H2O、Co(NO3)2•6H2O or Ni (NO3)2•6H2One of O or two
Kind.
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| CN111545208A (en) * | 2020-05-26 | 2020-08-18 | 福州大学 | Cobalt-nickel bimetallic catalyst and preparation method thereof |
| CN111558391A (en) * | 2020-05-26 | 2020-08-21 | 福州大学 | Heteroatom-doped cobalt metal catalyst and preparation method thereof |
| CN113943158A (en) * | 2021-12-20 | 2022-01-18 | 杭州德海艾科能源科技有限公司 | Preparation method of graphite felt for flow battery |
| CN114068195A (en) * | 2021-11-18 | 2022-02-18 | 四川金汇能新材料股份有限公司 | Metal-compounded carbon negative electrode material and preparation method thereof |
| CN114229825A (en) * | 2021-12-24 | 2022-03-25 | 北京航空航天大学 | Metal monoatomic-doped three-dimensional porous carbon material and preparation method and application thereof |
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| CN115084483A (en) * | 2022-07-21 | 2022-09-20 | 清创人和生态工程技术有限公司 | Walnut shell derived porous carbon/nickel/sulfur composite material and battery anode material prepared from same |
| CN115784228A (en) * | 2022-12-21 | 2023-03-14 | 陕西科技大学 | Bimetal modified nitrogen-doped porous carbon nanosheet and preparation method and application thereof |
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| CN111558391A (en) * | 2020-05-26 | 2020-08-21 | 福州大学 | Heteroatom-doped cobalt metal catalyst and preparation method thereof |
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| CN114068195A (en) * | 2021-11-18 | 2022-02-18 | 四川金汇能新材料股份有限公司 | Metal-compounded carbon negative electrode material and preparation method thereof |
| CN113943158A (en) * | 2021-12-20 | 2022-01-18 | 杭州德海艾科能源科技有限公司 | Preparation method of graphite felt for flow battery |
| CN114229825A (en) * | 2021-12-24 | 2022-03-25 | 北京航空航天大学 | Metal monoatomic-doped three-dimensional porous carbon material and preparation method and application thereof |
| CN115084483A (en) * | 2022-07-21 | 2022-09-20 | 清创人和生态工程技术有限公司 | Walnut shell derived porous carbon/nickel/sulfur composite material and battery anode material prepared from same |
| CN115784228A (en) * | 2022-12-21 | 2023-03-14 | 陕西科技大学 | Bimetal modified nitrogen-doped porous carbon nanosheet and preparation method and application thereof |
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