CN105776181B - A kind of preparation method of flake nano porous carbon and carbon nano tube compound material - Google Patents
A kind of preparation method of flake nano porous carbon and carbon nano tube compound material Download PDFInfo
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- CN105776181B CN105776181B CN201610281333.5A CN201610281333A CN105776181B CN 105776181 B CN105776181 B CN 105776181B CN 201610281333 A CN201610281333 A CN 201610281333A CN 105776181 B CN105776181 B CN 105776181B
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- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
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Abstract
A kind of synthetic method of flake nano porous carbon and carbon nano tube compound material, belongs to new material technology field.Intercalation growth, confinement carbonization and acid corrosion based on metal organic framework compound inside layered inorganic template two-dimensional nano duct remove template procedure, obtain the composite material of flake nano porous carbon and carbon nanotube.This method is simple and reliable, it is easy to accomplish the large-scale production of two-dimensional nano porous carbon sheet material and one-dimensional carbon nanotube composite material.Gained nanoporous carbon plate and carbon nano tube compound material chemical composition and pore structure are highly controllable, have wide application prospect in fields such as catalysis, energy storage and conversions.
Description
Technical field
The present invention relates to the preparation methods of a kind of flake nano porous carbon and carbon nano tube compound material, belong to new material skill
Art field.
Background technique
Flake nano porous carbon refers to the porous nano carbon material with quasi- two-dimensional structure.Compared with granular nano material,
Sheet two-dimensional nano porous material has microstructure, the bigger specific surface area, shorter lotus matter diffusion/transmission of high opening
Electron-transport effect in length and unique two-dimensional surface is one of the hot fields of function nano investigation of materials in recent years, is storing up
The great application prospect in the fields such as energy, catalysis, photoelectric material.And carbon nanotube has 1-dimention nano tubular structure, has good
Mechanical performance and electric conductivity.
Carbon material has good physical and chemical stability, electric conductivity and Structural flexibility, is widely used in the energy, urges
The fields such as change, biologic medical.Carbon material and two-dimensional nano knot have been organically combined by the two-dimensional nano-carbon material of representative of graphene
The advantage of structure is the function nano material of a kind of structure novel, unique properties.The traditional preparation methods master of two-dimensional nano-carbon material
Will be based on the methods of chemical vapor deposition, micromechanics stripping method, solvent removing, such method preparation process is cumbersome, it is difficult to realize
To the synchronization modulation of two-dimensional nano-carbon material chemical composition and microstructure, thus it is difficult to be used widely.
Metal organic framework compound is formed by the multiple tooth organic ligand and transition metal ions self assembly of oxygen-containing, nitrogen etc.
Coordination polymer, generally using metal ion as tie point, organic ligand position support constitute hole ordered 3 D structure abundant,
There is application potential in multiple fields.The general carbon content of metal organic framework compound is higher, internal naturally enriched a large amount of
Hetero atom (such as nitrogen) and metallic atom can realize conversion and group to nano-carbon material by being simply pyrolyzed carbonisation
At structure regulating.In the process, metal organic framework compound pore structure abundant can be saved largely, thus by
Its derivative nano-carbon material, which is often not necessarily to activation, can possess high-specific surface area.In addition, metal organic framework compound structure
High-sequential, pattern, size, crystal plane structure are controllable, are easily implemented using it as structured forerunner to derivative nano carbon material
Expect the finely regulating of microstructure, moreover, can retain after the nitrogen and metallic atom carbonization in metal organic framework compound
Among prepared carbon materials, the good reactivity of carbon materials and catalytic activity are assigned.Therefore, metal organic framework
Compound is considered as constructing the ideal forerunner with high-specific surface area, the adjustable nano-carbon material of Heteroatom doping and duct
Body.Conventional method is only capable of obtaining micro-nano granules derived from metal organic framework compound at present, with metal organic framework chemical combination
Object is that presoma constructs two-dimensional nano-carbon material, especially constructs the composite construction of two-dimensional nano porous carbon and one-dimensional carbon nanotube
It is still the huge challenge of functional material research field.
Summary of the invention
The purpose of the present invention is to provide the preparation methods of a kind of flake nano porous carbon and carbon nano tube compound material, should
Preparation method is proposed using metal organic framework compound as structured forerunner, with the commercialization with two-dimensional nano duct structure
Inorganic layered compounds are as stay in place form, based on different metal organic framework compounds in layered inorganic template two-dimensional nanopore
Intercalation growth, confinement carbonization and acid corrosion inside road remove template procedure, obtain highly controllable flake porous of composed structure
The composite construction of nano-sized carbon and carbon nanotube.Present invention process is simple, can be substantially reduced using commercialization presoma with template
Production cost, it is easy to accomplish large-scale production.
The technical solution adopted by the present invention is that: a kind of preparation method of flake nano porous carbon and carbon nano tube compound material
Include the following steps:
A, layered inorganic template is added in the solution of transition metal salt and lower immersion 30 minutes is stirred by ultrasonic, make layered inorganic
Ion exchange occurs for template interlayer cation, obtains metal ion-modified layered inorganic template, reaction temperature is room temperature；It is used
Solvent is one of water, methanol or ethyl alcohol；
B, layered inorganic template metal ion-modified obtained in step a is mixed with transition metal salt, organic ligand,
It is reacted 24 hours under room temperature, obtains the composite construction of organic framework compounds intercalated inorganic template；
C, by the composite construction of organic framework compounds intercalated inorganic template obtained in step b, under normal pressure, in setting
The composite construction of nano-sized carbon intercalation is obtained under calcination atmosphere；
D, the composite construction of nano-sized carbon intercalation obtained in step c is reacted to removal inorganic template with hydrofluoric acid solution, is used
Deionized water and ethyl alcohol washed product repeatedly, obtain the flake nano porous carbon and carbon nano tube compound material, acid after drying
Washing reaction temperature is room temperature, and the reaction time is 6-24 hours.
The metal ion-modified layered inorganic template includes bentonite, montmorillonite or layered double hydroxide.
The transition metal salt includes the nitrate of nickel, cobalt, iron, zinc, nickel, cobalt, iron, zinc chloride, nickel, cobalt, iron, zinc
Acetate, metal salt concentrations 0.01-1M.
The organic ligand includes at least one in phenylimidazole, 2-methylimidazole, 2- nitroimidazole or 2- imidazole formaldehyde
Kind, organic ligand solution concentration is 0.01-0.5M, and the molar ratio of organic ligand and transition metal salt is 0.01-4.0.
The calcination atmosphere includes one of nitrogen, argon gas, helium, hydrogen or carbon dioxide, calcination temperature 300-
1100 DEG C, calcination time is 0.2-6 hours.
The flake nano porous carbon and carbon nano tube compound material, flake nano porous carbon size is 1-100 microns, thick
Degree is 1-50 nanometers, and for carbon nanotube Parallel Growth on the face of flake nano porous carbon, composite construction contains N doping and not
With transient metal doped, there is micropore, meso-hole structure, specific surface area 100-1000m2g-1。
The beneficial effects of the present invention are: it the use of metal organic framework compound is presoma, layered inorganic compound is
Two-dimensional nanostructure template, the confinement for realizing the metal organic framework compound in the confinement space in stratiform template duct are raw
Long, confinement carbonization and carbon nanotube catalytic growth process, obtains the nanoporous carbon of sheet and the composite construction of carbon nanotube,
Similar to the leaf structure of nature tree, flake nano porous carbon is equivalent to leaf, and the carbon nanotube wherein inlayed is equivalent to
The vein of leaf.The present invention provides prepare flake porous carbon and composite structure of carbon nano tube by metal organic framework compound
Method, by selecting different transition metal salt and organic ligand, the flake nano of available a variety of the Nomenclature Composition and Structure of Complexes is more
The composite material of hole carbon and carbon nanotube.Products obtained therefrom has flourishing pore structure, and flaky nanometer structure can significantly contract
The presence of the diffusion length of the substances such as short ion, gas, electrolyte, vein shape carbon nanotube further enhances the conductive energy of material
Power, and the composition of composite material is led rich in uniform N doping and metal-doped, therefore in catalysis, energy storage and conversion etc.
Domain is with a wide range of applications.
Detailed description of the invention
Fig. 1 be the derivative cobalt/N doping flake nano porous carbon of ZIF-67 metal organic framework compound prepared by example 1 with
The transmission electron microscope photo of carbon nano tube compound material.
Fig. 2 is that the derivative cobalt/nickel/N doping flake nano of CoNi-ZIF metal organic framework compound prepared by example 2 is more
The transmission electron microscope photo of hole carbon and carbon nano tube compound material.
Fig. 3 is the derivative nickel/N doping flake nano porous carbon of ZnNi-ZIF metal organic framework compound prepared by example 3
With the transmission electron microscope photo of carbon nano tube compound material.
Fig. 4 is the transmission electricity of the derivative porous carbon nanosheet of N doping of ZIF-8 metal organic framework compound prepared by example 4
Mirror photo.
Specific embodiment
Embodiment 1
A, by 0.5g montmorillonite ultrasonic disperse in 50mL cobalt nitrate aqueous solution (0.07M), ultrasound centrifugation point after 30 minutes
From and with ethanol washing 2 times, the montmorillonite of cobalt ions modification is obtained；By the montmorillonite ultrasonic disperse of cobalt ions modification in 80mL nitre
In sour cobalt ethanol solution (0.125M), ultrasound is added in 80mL methylimidazole methanol solution (0.5M) after 30 minutes, stirs 5 points
By mixed dispersion liquid in standing 24 hours under room temperature after clock；After reaction, product is centrifugated and uses ethanol washing 2
Secondary, 80 DEG C of drying obtain the montmorillonite powder of ZIF-67 intercalation.
B, the montmorillonite powder of the ZIF-67 intercalation prepared in step a is heated to 900 DEG C in nitrogen stream, control heating
Rate is 5 DEG C of min-1, calcination time is 2 hours.After reaction, black solid powder is obtained.
C, the black solid powder prepared in step b is soaked in hydrofluoric acid, reaction is separated by filtration after 12 hours, is spent
Ion water washing 3 times, the derivative cobalt/N doping porous carbon nanometer of ZIF-67 metal organic framework compound is obtained after 80 DEG C of drying
Piece.Its specific surface area is up to 423m2g-1, thickness is in 50nm hereinafter, cobalt nano-particle average-size about 15nm, cobalt content are about
22wt.% has carbon nanotube generation on flake nano porous carbon.
Embodiment 2
A, by 0.5g montmorillonite ultrasonic disperse in 50mL cobalt nitrate (0.035M) and nickel nitrate (0.035M) mixed aqueous solution
In, ultrasound is centrifugated after 30 minutes and with ethanol washing 2 time, obtains cobalt/nickel ion modification montmorillonite；Cobalt ions is modified
Montmorillonite ultrasonic disperse in 80mL cobalt nitrate (0.0625M) and nickel nitrate (0.0625M) mixed ethanol solution, 30 points of ultrasound
It is added in 80mL methylimidazole methanol solution (0.5M), is stirred after five minutes by mixed dispersion liquid in quiet under room temperature after clock
It sets 24 hours；After reaction, product is centrifugated and is used ethanol washing 2 times, 80 DEG C of drying obtain CoNi-ZIF intercalation
Montmorillonite powder.
B, with step b in embodiment 1；
C, the black solid powder prepared in step b is soaked in hydrofluoric acid, reaction is separated by filtration after 12 hours, is spent
Ion water washing 3 times, the derivative cobalt/nickel/N doping porous carbon of CoNi-ZIF metal organic framework compound is obtained after 80 DEG C of drying
Nanometer sheet.Wherein metal nanoparticle size is in 25nm hereinafter, there is carbon nanotube generation on flake nano porous carbon.
Embodiment 3
A, by 0.5g montmorillonite ultrasonic disperse in 50mL zinc nitrate (0.035M) and nickel nitrate (0.035M) mixed aqueous solution
In, ultrasound is centrifugated after 30 minutes and with ethanol washing 2 time, obtains zinc/nickel ion modification montmorillonite；Cobalt ions is modified
Montmorillonite ultrasonic disperse in 80mL zinc nitrate (0.0625M) and nickel nitrate (0.0625M) mixed ethanol solution, 30 points of ultrasound
It is added in 80mL methylimidazole methanol solution (0.5M), is stirred after five minutes by mixed dispersion liquid in quiet under room temperature after clock
It sets 24 hours；After reaction, product is centrifugated and is used ethanol washing 2 times, 80 DEG C of drying obtain ZnNi-ZIF intercalation
Montmorillonite powder.
B, with step b in embodiment 1；
C, the black solid powder prepared in step b is soaked in hydrofluoric acid, reaction is separated by filtration after 12 hours, is spent
Ion water washing 3 times, the derivative nickel/N doping porous carbon nanometer of ZnNi-ZIF metal organic framework compound is obtained after 80 DEG C of drying
Piece has carbon nanotube generation on flake nano porous carbon.
Embodiment 4
A, by 0.5g montmorillonite ultrasonic disperse in 50mL zinc nitrate (0.07M) aqueous solution, ultrasound centrifugation point after 30 minutes
From and with ethanol washing 2 times, the montmorillonite of zinc ion modification is obtained；By the montmorillonite ultrasonic disperse of zinc ion modification in 80mL nitre
In sour zinc (0.125M) ethanol solution, ultrasound is added in 80mL methylimidazole methanol solution (0.5M) after 30 minutes, stirs 5 points
By mixed dispersion liquid in standing 24 hours under room temperature after clock；After reaction, product is centrifugated and uses ethanol washing 2
Secondary, 80 DEG C of drying obtain the montmorillonite powder of ZIF-8 intercalation.
B, with step b in embodiment 1；
C, the black solid powder prepared in step b is soaked in excessive hydrofluoric acid, filtering point after reaction 12 hours
From being washed with deionized 3 times, the derivative N doping porous carbon of ZIF-8 metal organic framework compound obtained after 80 DEG C of drying and is received
Rice piece, specific surface area are up to 436m2g-1。
Claims (5)
1. a kind of preparation method of flake nano porous carbon and carbon nano tube compound material, it is characterised in that include the following steps:
A, montmorillonite or bentonite stratiform inorganic template are added to ultrasound in the aqueous solution of transition metal salt to impregnate 30 minutes, make to cover
Ion exchange occurs for de- soil or bentonite stratiform inorganic template interlayer cation, obtains metal ion-modified montmorillonite or swelling
Soil layer shape inorganic template, reaction temperature are room temperature；
B, by montmorillonite metal ion-modified obtained in step a or bentonite stratiform inorganic template and transition metal salt, have
The mixing of machine ligand, react 24 hours under room temperature, and acquisition organic framework compounds intercalated montmorillonite or bentonite inorganic template are answered
Close structure；
C, by organic framework compounds intercalated montmorillonite obtained in step b or the composite construction of bentonite inorganic template, normal
Pressure, obtains the composite construction of nano-sized carbon intercalation under calcination atmosphere in setting；
D, the composite construction of nano-sized carbon intercalation obtained in step c is reacted with hydrofluoric acid solution to removal inorganic template, spend from
Sub- water and ethyl alcohol washed product repeatedly, obtain the flake nano porous carbon and carbon nano tube compound material, pickling are anti-after drying
Answering temperature is room temperature, and the reaction time is 6-24 hours.
2. the preparation method of a kind of flake nano porous carbon and carbon nano tube compound material according to claim 1, special
Sign is, the transition metal salt includes the nitrate of nickel, cobalt, iron, zinc, nickel, cobalt, iron, zinc chlorate, nickel, cobalt, iron,
The acetate of zinc, metal salt concentrations 0.01-1M.
3. the preparation method of a kind of flake nano porous carbon and carbon nano tube compound material according to claim 1, special
Sign is that the organic ligand includes at least one in phenylimidazole, 2-methylimidazole, 2- nitroimidazole or 2- imidazole formaldehyde
Kind, organic ligand solution concentration is 0.01-0.5 M, and the molar ratio of organic ligand and transition metal salt is 0.01-4.0.
4. the preparation method of a kind of flake nano porous carbon and carbon nano tube compound material according to claim 1, special
Sign is that the calcination atmosphere includes one of nitrogen, argon gas, helium, calcination temperature 300-1100oC, when calcining
Between be 0.2-6 hours.
5. the preparation method of a kind of flake nano porous carbon and carbon nano tube compound material according to claim 1, special
Sign is that the flake nano porous carbon and carbon nano tube compound material, flake nano porous carbon size are 1-100 microns, thick
Degree is 1-50 nanometers, and for carbon nanotube Parallel Growth on the face of flake nano porous carbon, composite construction contains N doping and not
With transient metal doped, there is micropore, meso-hole structure, specific surface area is 100-1000 m2 g-1。
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