CN105776181A - Preparation method of flaky nanoholes carbon and carbon nanotube composite - Google Patents
Preparation method of flaky nanoholes carbon and carbon nanotube composite Download PDFInfo
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- CN105776181A CN105776181A CN201610281333.5A CN201610281333A CN105776181A CN 105776181 A CN105776181 A CN 105776181A CN 201610281333 A CN201610281333 A CN 201610281333A CN 105776181 A CN105776181 A CN 105776181A
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- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
A preparation method of a flaky nanoholes carbon and carbon nanotube composite belongs to the technical field of new materials. The flaky nanoholes carbon and carbon nanotube composite is obtained based on intercalation growth of a metal-organic framework compound in two-dimensional nanoholes of a lamellar inorganic template, confinement carbonization and template removal by acid corrosion. The method is simple and reliable, the large-scale production of two-dimensional nanoholes carbon flake material and one-dimensional carbon nanotube composite is easy to implement. The obtained nanoholes carbon flake and carbon nanotube composite has highly controllable chemical composition and pore structure height and has a promising application prospect in the catalysis field, the energy storage and conversion field and other fields.
Description
Technical field
The preparation method that the present invention relates to a kind of flake nano porous carbon and carbon nano tube compound material, belongs to new material technology field.
Background technology
Flake nano porous carbon refers to the porous nano material with carbon element with quasi-two-dimensional structure.Compared with granular nano material, lamellar two-dimensional nano porous material has electric transmission effect in the two-dimensional surface of the microstructure of high opening, bigger specific surface area, shorter lotus matter diffusion/conveying length and uniqueness, it is one of the hot fields of function nano investigation of materials in recent years, in great application prospects in field such as energy storage, catalysis, photoelectric materials.And CNT has 1-dimention nano tubular structure, there is good mechanical performance and electric conductivity.
Material with carbon element has good physical and chemical stability, electric conductivity and Structural flexibility, is widely used in the fields such as the energy, catalysis, biologic medical.Organically combine the advantage of material with carbon element and two-dimensional nanostructure with the two-dimensional nano material with carbon element that Graphene is representative, be that a class formation is novel, the function nano material of unique properties.The traditional preparation methods of two-dimensional nano material with carbon element is based primarily upon the methods such as chemical vapour deposition (CVD), micromechanics stripping method, solvent stripping, this type of method preparation process is loaded down with trivial details, it is difficult to the synchronization modulation to two-dimensional nano material with carbon element chemical composition Yu microstructure, thus is difficult to be used widely.
Metal organic framework compound is the coordination polymer of the multiple tooth organic ligand by oxygen-containing, nitrogen etc. and transition metal ions self assembly, general with metal ion for junction point, organic ligand position supports and constitutes the ordered 3 D structure that hole is abundant, has application potential in multiple fields.The general carbon content of metal organic framework compound is higher, internal naturally enriched substantial amounts of hetero atom (such as nitrogen etc.) and metallic atom, it is possible to realized to the conversion of nano-carbon material and composition structure regulating by simple pyrolysis carbonisation.In the process, the pore structure that metal organic framework compound is abundant can major part be preserved, thus often can be had high-specific surface area without activation by its derivative nano-carbon material.In addition, metal organic framework compound structure height is orderly, pattern, size, crystal plane structure are controlled, using be easily achieved the finely regulating to derivative nano-carbon material microstructure as structured forerunner, moreover, nitrogen in metal organic framework compound and can be retained among prepared carbon materials after metallic atom carbonization, gives the good reactivity of carbon materials and catalysis activity.Therefore, metal organic framework compound is considered as the desirable presoma constructed and have the adjustable nano-carbon material in high-specific surface area, Heteroatom doping and duct.Current conventional method is only capable of obtaining the micro-nano granules that metal organic framework compound is derivative, constructing two-dimensional nano material with carbon element with metal organic framework compound for presoma, the composite construction particularly constructing two-dimensional nano porous carbon and one-dimensional CNT is still the huge challenge of functional material research field.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of flake nano porous carbon and carbon nano tube compound material, this preparation method proposes using metal organic framework compound as structured forerunner, there is the commercialization inorganic layered compounds of two-dimensional nano duct structure as stay in place form, template procedure is removed in intercalation growth, confinement carbonization and the acid corrosion within layered inorganic template two-dimensional nano duct, it is thus achieved that form the composite construction of the controlled flake porous nano-sized carbon of structure height and CNT based on different metal organic framework compounds.Present invention process is simple, uses commercialization presoma and template can be substantially reduced production cost, it is easy to accomplish large-scale production.
The technical solution used in the present invention is: the preparation method of a kind of flake nano porous carbon and carbon nano tube compound material comprises the steps:
A, layered inorganic template is added in the solution of transition metal salt under ultrasonic agitation soak 30 minutes, make layered inorganic template interlayer cation generation ion exchange, it is thus achieved that metal ion-modified layered inorganic template, reaction temperature is room temperature；Solvent for use is the one in water, methanol or ethanol；
B, the metal ion-modified layered inorganic template obtained in step a is mixed with transition metal salt, organic ligand, react 24 hours under room temperature, it is thus achieved that the composite construction of organic framework compounds intercalated inorganic template；
C, the composite construction of organic framework compounds intercalated inorganic template that will obtain in step b, at ambient pressure, in setting the composite construction obtaining nano-sized carbon intercalation under calcination atmosphere；
D, composite construction and the hydrofluoric acid solution of the nano-sized carbon intercalation obtained in step c are reacted removal inorganic template, with deionized water and ethanol cyclic washing product, described flake nano porous carbon and carbon nano tube compound material is obtained after drying, pickling reaction temperature is room temperature, and the response time is 6-24 hour.
Described metal ion-modified layered inorganic template includes bentonite, montmorillonite or layered double hydroxide.
Described transition metal salt includes the nitrate of nickel, cobalt, ferrum, zinc, nickel, cobalt, ferrum, zinc chloride, nickel, cobalt, ferrum, zinc acetate, metal salt concentrations is 0.01-1M.
Described organic ligand includes at least one in phenylimidazole, 2-methylimidazole, 2-nitroimidazole or 2-imidazole formaldehyde, and organic ligand solution concentration is 0.01-0.5M, and the mol ratio of organic ligand and transition metal salt is 0.01-4.0.
Described calcination atmosphere includes the one in nitrogen, argon, helium, hydrogen or carbon dioxide, and calcining heat is 300-1100 DEG C, and calcination time is 0.2-6 hour.
Described flake nano porous carbon and carbon nano tube compound material, flake nano porous carbon is sized to 1-100 micron, thickness is 1-50 nanometer, CNT Parallel Growth is on the face of flake nano porous carbon, composite construction contains N doping and different transient metal doped, having micropore, meso-hole structure, specific surface area is 100-1000m2g-1。
The beneficial effects of the present invention is: use metal organic framework compound is presoma, layered inorganic compound is two-dimensional nanostructure template, achieve the catalytic growth process of the confinement growth of metal organic framework compound in the confinement space in stratiform template duct, confinement carbonization and CNT, obtain the nanoporous carbon of lamellar and the composite construction of CNT, it is similar to the leaf structure of nature tree, flake nano porous carbon is equivalent to leaf, and the CNT wherein inlayed is equivalent to the vein of leaf.The invention provides the method being prepared flake porous carbon and composite structure of carbon nano tube by metal organic framework compound, by selecting different transition metal salts and organic ligand, it is possible to obtain the flake nano porous carbon of multiple the Nomenclature Composition and Structure of Complexes and the composite of CNT.Products obtained therefrom has the pore structure of prosperity, flaky nanometer structure can be greatly shortened the diffusion length of the materials such as ion, gas, electrolyte, the existence of vein shape CNT further enhances the conductive capability of material, and the composition of composite is rich in uniform N doping and metal-doped, is therefore with a wide range of applications in fields such as catalysis, energy storage and conversions.
Accompanying drawing explanation
Fig. 1 is the ZIF-67 metal organic framework compound derivative cobalt/N doping flake nano porous carbon transmission electron microscope photo with carbon nano tube compound material of example 1 preparation.
Fig. 2 is the CoNi-ZIF metal organic framework compound derivative cobalt/nickel/N doping flake nano porous carbon transmission electron microscope photo with carbon nano tube compound material of example 2 preparation.
Fig. 3 is the ZnNi-ZIF metal organic framework compound derivative nickel/N doping flake nano porous carbon transmission electron microscope photo with carbon nano tube compound material of example 3 preparation.
Fig. 4 is the transmission electron microscope photo of the derivative N doping porous carbon nanometer sheet of ZIF-8 metal organic framework compound of example 4 preparation.
Detailed description of the invention
Embodiment 1
A, by 0.5g montmorillonite ultrasonic disperse in 50mL cobalt nitrate aqueous solution (0.07M), centrifugation by washing with alcohol 2 times after ultrasonic 30 minutes, it is thus achieved that the montmorillonite that cobalt ion is modified；The montmorillonite ultrasonic disperse modified by cobalt ion is in 80mL cobalt nitrate alcoholic solution (0.125M), add in 80mL methylimidazole methanol solution (0.5M) after ultrasonic 30 minutes, after stirring 5 minutes, mixed dispersion liquid is stood 24 hours under room temperature condition；After reaction terminates, by product centrifugation and with washing with alcohol 2 times, the montmorillonite powder body of 80 DEG C of drying acquisition ZIF-67 intercalations.
B, heating the montmorillonite powder body of ZIF-67 intercalation of preparation in step a to 900 DEG C in nitrogen stream, controlling heating rate is 5 DEG C of min-1, calcination time is 2 hours.Reaction obtains black solid powder after terminating.
C, the black solid powder of preparation in step b is soaked in Fluohydric acid., isolated by filtration after react 12 hours, with deionized water wash 3 times, 80 DEG C dry after obtain ZIF-67 metal organic framework compound and derive cobalt/N doping porous carbon nanometer sheet.Its specific surface area is up to 423m2g-1, thickness is at below 50nm, and cobalt nano-particle average-size is about 15nm, and cobalt content is about 22wt.%, and flake nano porous carbon has CNT to generate.
Embodiment 2
A, by 0.5g montmorillonite ultrasonic disperse in 50mL cobalt nitrate (0.035M) and nickel nitrate (0.035M) mixed aqueous solution, centrifugation by washing with alcohol 2 times after ultrasonic 30 minutes, it is thus achieved that the montmorillonite of cobalt/nickel ion modification；The montmorillonite ultrasonic disperse modified by cobalt ion is in 80mL cobalt nitrate (0.0625M) with nickel nitrate (0.0625M) mixed ethanol solution, add in 80mL methylimidazole methanol solution (0.5M) after ultrasonic 30 minutes, after stirring 5 minutes, mixed dispersion liquid is stood 24 hours under room temperature condition；After reaction terminates, by product centrifugation and with washing with alcohol 2 times, the montmorillonite powder body of 80 DEG C of drying acquisition CoNi-ZIF intercalations.
B, with step b in embodiment 1；
C, the black solid powder of preparation in step b is soaked in Fluohydric acid., isolated by filtration after react 12 hours, with deionized water wash 3 times, 80 DEG C dry after obtain CoNi-ZIF metal organic framework compound and derive cobalt/nickel/N doping porous carbon nanometer sheet.Wherein metal nanoparticle size has CNT to generate on below 25nm, 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, centrifugation by washing with alcohol 2 times after ultrasonic 30 minutes, it is thus achieved that the montmorillonite of zinc/nickel ion modification；The montmorillonite ultrasonic disperse modified by cobalt ion is in 80mL zinc nitrate (0.0625M) with nickel nitrate (0.0625M) mixed ethanol solution, add in 80mL methylimidazole methanol solution (0.5M) after ultrasonic 30 minutes, after stirring 5 minutes, mixed dispersion liquid is stood 24 hours under room temperature condition；After reaction terminates, by product centrifugation and with washing with alcohol 2 times, the montmorillonite powder body of 80 DEG C of drying acquisition ZnNi-ZIF intercalations.
B, with step b in embodiment 1；
C, by step b preparation black solid powder be soaked in Fluohydric acid., isolated by filtration after reacting 12 hours, with deionized water wash 3 times, obtain the derivative nickel/N doping porous carbon nanometer sheet of ZnNi-ZIF metal organic framework compound after 80 DEG C of drying, flake nano porous carbon has CNT to generate.
Embodiment 4
A, by 0.5g montmorillonite ultrasonic disperse in 50mL zinc nitrate (0.07M) aqueous solution, centrifugation by washing with alcohol 2 times after ultrasonic 30 minutes, it is thus achieved that the montmorillonite that zinc ion is modified；The montmorillonite ultrasonic disperse modified by zinc ion is in 80mL zinc nitrate (0.125M) alcoholic solution, add in 80mL methylimidazole methanol solution (0.5M) after ultrasonic 30 minutes, after stirring 5 minutes, mixed dispersion liquid is stood 24 hours under room temperature condition；After reaction terminates, by product centrifugation and with washing with alcohol 2 times, the montmorillonite powder body of 80 DEG C of drying acquisition ZIF-8 intercalations.
B, with step b in embodiment 1；
C, by step b preparation black solid powder be soaked in excessive Fluohydric acid., isolated by filtration after reacting 12 hours, with deionized water wash 3 times, 80 DEG C dry after obtain the derivative N doping porous carbon nanometer sheet of ZIF-8 metal organic framework compound, its specific surface area is up to 436m2g-1。
Claims (6)
1. the preparation method of a flake nano porous carbon and carbon nano tube compound material, it is characterised in that comprise the steps:
A, layered inorganic template is added in the solution of transition metal salt under ultrasonic agitation soak 30 minutes, make layered inorganic template interlayer cation generation ion exchange, it is thus achieved that metal ion-modified layered inorganic template, reaction temperature is room temperature；Solvent for use is the one in water, methanol or ethanol；
B, the metal ion-modified layered inorganic template obtained in step a is mixed with transition metal salt, organic ligand, react 24 hours under room temperature, it is thus achieved that the composite construction of organic framework compounds intercalated inorganic template；
C, the composite construction of organic framework compounds intercalated inorganic template that will obtain in step b, at ambient pressure, in setting the composite construction obtaining nano-sized carbon intercalation under calcination atmosphere；
D, composite construction and the hydrofluoric acid solution of the nano-sized carbon intercalation obtained in step c are reacted removal inorganic template, with deionized water and ethanol cyclic washing product, described flake nano porous carbon and carbon nano tube compound material is obtained after drying, pickling reaction temperature is room temperature, and the response time is 6-24 hour.
2. the preparation method of a kind of flake nano porous carbon according to claim 1 and carbon nano tube compound material, it is characterised in that described metal ion-modified layered inorganic template includes bentonite, montmorillonite or layered double hydroxide.
3. the preparation method of a kind of flake nano porous carbon according to claim 1 and carbon nano tube compound material, it is characterized in that, described transition metal salt includes the nitrate of nickel, cobalt, ferrum, zinc, nickel, cobalt, ferrum, zinc chloride, nickel, cobalt, ferrum, zinc acetate, metal salt concentrations is 0.01-1M.
4. the preparation method of a kind of flake nano porous carbon according to claim 1 and carbon nano tube compound material, it is characterized in that, described organic ligand includes at least one in phenylimidazole, 2-methylimidazole, 2-nitroimidazole or 2-imidazole formaldehyde, organic ligand solution concentration is 0.01-0.5M, and the mol ratio of organic ligand and transition metal salt is 0.01-4.0.
5. the preparation method of a kind of flake nano porous carbon according to claim 1 and carbon nano tube compound material, it is characterized in that, described calcination atmosphere includes the one in nitrogen, argon, helium, hydrogen or carbon dioxide, and calcining heat is 300-1100 DEG C, and calcination time is 0.2-6 hour.
6. the preparation method of a kind of flake nano porous carbon according to claim 1 and carbon nano tube compound material, it is characterized in that, described flake nano porous carbon and carbon nano tube compound material, flake nano porous carbon is sized to 1-100 micron, thickness is 1-50 nanometer, and CNT Parallel Growth is on the face of flake nano porous carbon, and composite construction contains N doping and different transient metal doped, having micropore, meso-hole structure, specific surface area is 100-1000m2g-1。
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| CN112331482A (en) * | 2020-08-04 | 2021-02-05 | 盐城工学院 | Porous carbon composite material and preparation method and application thereof |
| CN112599771A (en) * | 2020-12-15 | 2021-04-02 | 南京工业大学 | Metal-doped carbon tube/carbon sheet composite material and preparation method and application thereof |
| CN113173582A (en) * | 2021-04-30 | 2021-07-27 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Flexible self-supporting activated carbon microchip/carbon nanotube composite material, preparation method and application |
| CN113173582B (en) * | 2021-04-30 | 2022-08-30 | 江西省纳米技术研究院 | Flexible self-supporting active carbon microchip/carbon nano tube composite material, preparation method and application |
| CN114671427A (en) * | 2022-03-21 | 2022-06-28 | 中国人民解放军国防科技大学 | Composite nanomaterial of carbon nano sheet in-situ loaded carbon nano tube and preparation method and application thereof |
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| CN115106061B (en) * | 2022-07-27 | 2023-06-20 | 常州大学 | Preparation method of attapulgite/flaky activated carbon honeycomb adsorbent |
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