CN107032326B - A kind of method that solid catalysis prepares spiral carbon nano pipe - Google Patents
A kind of method that solid catalysis prepares spiral carbon nano pipe Download PDFInfo
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- CN107032326B CN107032326B CN201710257230.XA CN201710257230A CN107032326B CN 107032326 B CN107032326 B CN 107032326B CN 201710257230 A CN201710257230 A CN 201710257230A CN 107032326 B CN107032326 B CN 107032326B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprising the following steps: A) organic carbon source and transition metal ions are mixed in water, obtain mixed solution；The organic carbon source includes urea and/or melamine；The transition metal ions includes nickel ion and/or manganese ion；B) mixed solution is dried, obtains hybrid solid；C) hybrid solid is calcined, obtains spiral carbon nano pipe.Method carbon source in the present invention is low in cost with catalyst, is easy to get, and early-stage preparations processing method is simple and easy, is advantageously implemented volume production；Nickeliferous and/or manganese catalyst catalytic performance is good, can largely generate spiral helicine carbon nanotube product, and yield is up to 45%；Related equipment is simple, and required reaction condition is easy to reach；The spiral carbon nano pipe size distribution produced is uniform.
Description
Technical field
The invention belongs to a kind of methods that field of nanometer technology more particularly to solid catalysis prepare spiral carbon nano pipe.
Background technique
The preparation and its utilization of carbon nanotube are the hot spots of current nanotechnology and material science research.Carbon nanotube has
Good chemical property, excellent mechanical property and good thermal property.These exclusive outstanding performances make carbon nanometer
Pipe is widely used in numerous frontier science and technology fields, for example, high-performance conductive composite material, super capacitor and electrode material, intelligence
It can robot and biomedicine etc..
Early in 1991, Japanese scientist Iijima, which was just had found in accident using graphite arc equipment, prepares carbon
Nanotube, and observe with high-resolution-ration transmission electric-lens the clear structure of carbon nanotube.Then, the preparation method of carbon nanotube is each
State scientific research personnel further studies invention, a series of carbon nanotubes to come in every shape and have different physical and chemical properties
It is researched and developed.1994, Zhang etc. had found the carbon nanometer with neat regular helix shape with transmission electron microscope for the first time
Pipe.Spiral carbon nano pipe also has its special helicoidal structure institute while having common carbon nanotube numerous excellent in performance
Bring peculiar advantage, for example, good energy absorption capability and synthesizing the composite material with stronger performance with other materials.
Up to the present, the method for preparing spiral carbon nano pipe has graphite acr method, laser evaporization method and chemical gaseous phase
It deposits (CVD), however although this 3 major class preparation method may be implemented the synthesis of spiral carbon nano pipe, but because itself
Limitation is unable to mass production, for example, graphite acr method and laser evaporization method need the output of high-energy and helical form carbon is received
Mitron is mostly by-product, and preparation amount is less, and CVD also has the catalyst of its central role while needing high energy to export
Very high requirement.
Summary of the invention
It is provided by the invention the purpose of the present invention is to provide a kind of method that solid catalysis prepares spiral carbon nano pipe
Equipment needed for method is simple, and reaction condition is easy to reach, and yield is higher, volume production easy to accomplish.
The present invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprising the following steps:
A organic carbon source and transition metal ions are mixed in water), obtain mixed solution；The organic carbon source includes urine
Element and/or melamine；The transition metal ions includes nickel ion and/or manganese ion；
B) mixed solution is dried, obtains hybrid solid；
C) hybrid solid is calcined, obtains spiral carbon nano pipe.
Preferably, the step A) specifically:
Organic carbon source and transition metal salt are mixed in water, obtain mixed solution；
The transition metal salt includes MnCl2And/or NiCl2。
Preferably, the molar ratio of the organic carbon source and transition metal ions is (1~5): 1.
Preferably, the step B) in dry temperature be 70~100 DEG C；
The step B) in dry time be 6~12 hours.
Preferably, the step C) in calcine temperature be 500~800 DEG C；
The step C) in calcine time be 4~7 hours.
Preferably, the temperature of the calcining is realized by heating, and the rate of the heating is 2~6 DEG C/min.
Preferably, the calcining carries out under protective gas atmosphere, and the flow velocity of the protective gas is 50~
200mL/min。
Preferably, the step C) further comprising the steps of afterwards:
Calcined product is successively carried out to pickling, washing and alcohol to wash, obtains spiral carbon nano pipe.
Preferably, the pickling uses concentrated nitric acid, and the mass concentration of the concentrated nitric acid is 60~70%.
Preferably, the alcohol is washed using ethyl alcohol, and the volumetric concentration of the ethyl alcohol is 30~60%.
The present invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprising the following steps: A) it will be organic
Carbon source and transition metal ions mix in water, obtain mixed solution；The organic carbon source includes urea and/or melamine；
The transition metal ions includes nickel ion and/or manganese ion；B) mixed solution is dried, obtains hybrid solid；
C) hybrid solid is calcined, obtains spiral carbon nano pipe.Method provided by the invention has the advantage that
(1) carbon source is low in cost with catalyst, is easy to get, and early-stage preparations processing method is simple and easy, is advantageously implemented
Volume production.
(2) nickeliferous and/or manganese catalyst catalytic performance is good, and catalyzing urea and/or melamine can be generated largely
Spiral helicine carbon nanotube product, yield are up to 45%.
(3) equipment involved in is simple, and required reaction condition is easy to reach.
(4) the spiral carbon nano pipe size distribution produced is uniform.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the SEM figure of spiral carbon nano pipe in the embodiment of the present invention 1；
Fig. 2 is the TEM figure of spiral carbon nano pipe in the embodiment of the present invention 1.
Specific embodiment
The present invention provides a kind of methods that solid catalysis prepares spiral carbon nano pipe, comprising the following steps:
A organic carbon source and transition metal ions are mixed in water), obtain mixed solution；The organic carbon source includes urine
Element and/or melamine；The transition metal ions includes nickel ion and/or manganese ion；
B) mixed solution is dried, obtains hybrid solid；
C) hybrid solid is calcined, obtains spiral carbon nano pipe.
Using melamine and/or urea as carbon source, transition metal is catalyst, reaction condition letter for reaction in the present invention
It is single, it is easy to reach, and yield is higher, volume production easy to accomplish.
The present invention mixes organic carbon source and transition metal ions in water, obtains mixed solution, preferably by organic carbon source
It is mixed in water with transition metal salt, obtains mixed solution.
In the present invention, the organic carbon source is urea and/or melamine, and the transition metal ions is nickel ion
And/or manganese ion, the transition metal salt preferably include MnCl2And/or NiCl2；The water is preferably deionized water, described to have
Machine carbon source and the molar ratio of transition metal ions are preferably (1~5): 1, more preferably (2~4): 1, most preferably 3:1.
The present invention is preferably stirred the mixed solution, enables evenly dispersed in water, and the present invention is to described
The time of stirring does not have special limitation, specifically, in an embodiment of the present invention, can stir 0.5~3 hour.
The mixed solution is dried the present invention, obtains hybrid solid, and the present invention preferably sets the mixed solution
It being dried in a vacuum drying oven, the temperature of the drying is preferably 70~100 DEG C, and more preferably 80~90 DEG C；It is described dry
The dry time is preferably 6~12 hours, more preferably 7~11 hours, most preferably 8~10 hours.
After obtaining hybrid solid, the present invention preferably mills the hybrid solid, obtains mixed-powder, the mixing
The partial size of powder is preferably 10~100 μm, more preferably 20~80 μm, most preferably 30~70 μm.
The present invention preferably calcines mixed-powder, obtains spiral carbon nano pipe, the present invention is preferably by the mixing
Powder is put into tube furnace and is calcined, and the temperature of the calcining is preferably 500~800 DEG C, preferably 550~750 DEG C, optimal
It is selected as 600~700 DEG C；The time of the calcining is preferably 4~8 hours, more preferably 5~7 hours, most preferably 6 hours.This
Invention preferably carries out the calcining under protective gas atmosphere, and logical protective gas to the calcining is kept to produce after calcining
Product cool down at room temperature, and the protective gas is preferably nitrogen, helium or argon gas；The flow velocity of the protective gas is preferably
50~200mL/min, more preferably 100~150mL/min.
After completing the calcining, the calcined product is preferably successively carried out pickling, washing and alcohol and washed by the present invention, is obtained
To spiral carbon nano pipe, the present invention preferably by calcined product in concentrated nitric acid agitator treating 10~12 hours, then again
It is cleaned repeatedly with deionized water and ethyl alcohol.In the present invention, the mass concentration of the concentrated nitric acid is preferably 60~70%, more preferably
It is 65%；The volumetric concentration of the ethyl alcohol is preferably 30~60%, and more preferably 35~55%, most preferably 40~50%.
After completing cleaning, preferably the product after cleaning is dried again by the present invention, obtains spiral carbon nano pipe institute
Stating dry temperature is preferably 70~100 DEG C, and more preferably 80~90 DEG C；The time of the drying is preferably 8~24 hours, more
Preferably 10~20 hours, most preferably 12~18 hours.The present invention preferably carries out the drying in a vacuum drying oven.
According to spiral carbon nano pipe made from the method in the present invention, size is uniform, carbon nanotube diameter be 30~
300nm, pipe range are 1~30 μm, and screw diameter is 0.2~3 μm.
The present invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprising the following steps: A) it will be organic
Carbon source and transition metal ions mix in water, obtain mixed solution；The organic carbon source includes urea and/or melamine；
The transition metal ions includes nickel ion and/or manganese ion；B) mixed solution is dried, obtains hybrid solid；
C) hybrid solid is calcined, obtains spiral carbon nano pipe.Method provided by the invention has the advantage that
(1) carbon source is low in cost with catalyst, is easy to get, and early-stage preparations processing method is simple and easy, is advantageously implemented
Volume production.
(2) nickeliferous and/or manganese catalyst catalytic performance is good, and catalyzing urea and/or melamine can be generated largely
Spiral helicine carbon nanotube product, yield are up to 45%.
(3) equipment involved in is simple, and required reaction condition is easy to reach.
(4) the spiral carbon nano pipe size distribution produced is uniform.
In order to further illustrate the present invention, with reference to embodiments to a kind of solid catalysis preparation spiral provided by the invention
The method of shape carbon nanotube is described in detail, but cannot be understood as limiting the scope of the present invention.
In following embodiment, the yield of carbon nanotube is calculated according to following formula:
Wherein, m1 is the quality of carbon nanotube, and m2 is quality (the i.e. matter of reaction early transition metal salt for reacting procatalyst
Amount).
Embodiment 1
Take 1g urea and 1gMnCl2It is dissolved in deionized water respectively, mixture stirs 30min, so that urea and MnCl2
Can uniformly it disperse in water.Obtained mixed solution is placed in a vacuum drying oven exhaust, temperature is maintained at 70 DEG C, and the time is
6h.Powder after obtained hybrid solid is milled is put into tube furnace, in the environment of nitrogen, is burnt at 500 DEG C
System, molding time are 4 hours.To the end of calcining, allows drug to continue to keep logical nitrogen state in tube furnace, naturally cool to
Room temperature.Then use deionized water and alcohol repeatedly clear again concentrated nitric acid agitator treating 12 hours of 65% of the material baked
It washes.Then it places and is vented in vacuum oven, temperature is maintained at 70 DEG C, time 8h.Stone is taken out after natural cooling at room temperature
Ying Zhou prepares uniform spiral carbon nano pipe (pipe diameter: 100~300nm；Pipe range: 10~30 μm；Spiral is straight
1~3 μm of diameter).It is computed, carbon nanotube yield is 30%.
The present invention has carried out scanning electron microscope and transmission electron microscope detection to spiral carbon nano pipe made from the present embodiment respectively,
As a result as shown in Fig. 1~2, Fig. 1 is the SEM figure of spiral carbon nano pipe in the embodiment of the present invention 1, and Fig. 2 is the embodiment of the present invention 1
The TEM of middle spiral carbon nano pipe schemes.
Embodiment 2
Take 3g melamine and 1gNiCl2Be dissolved in deionized water respectively, mixture stir 2h so that melamine and
NiCl2Can uniformly it disperse in water.Obtained mixed solution is placed in a vacuum drying oven exhaust, temperature is maintained at 80 DEG C,
Time is 10h.Powder after obtained hybrid solid is milled is put into tube furnace, in the environment of nitrogen, at 700 DEG C
It is fired, molding time is 6 hours.To the end of calcining, drug is allowed to continue to keep logical nitrogen state in tube furnace, it is natural
It is cooled to room temperature.Then the material baked was used into deionized water and alcohol repeatedly again with 65% concentrated nitric acid agitator treating 12 hours
Cleaning.Then it places and is vented in vacuum oven, temperature is maintained at 80 DEG C, time 16h.It is taken out after natural cooling at room temperature
Quartz boat prepares uniform spiral carbon nano pipe (pipe diameter: 50~200nm；Pipe range: 5~20 μm；Spiral is straight
0.5~2 μm of diameter).It is computed, carbon nanotube yield is 40%.
Embodiment 3
Take 5g melamine and 1gMnCl2Be dissolved in deionized water respectively, mixture stir 3h so that melamine and
MnCl2Can uniformly it disperse in water.Obtained mixed solution is placed in a vacuum drying oven exhaust, temperature is maintained at 100 DEG C,
Time is 12h.Powder after obtained hybrid solid is milled is put into tube furnace, in the environment of nitrogen, at 800 DEG C
It is fired, molding time is 8 hours.To the end of calcining, drug is allowed to continue to keep logical nitrogen state in tube furnace, it is natural
It is cooled to room temperature.Then the material baked was used into deionized water and alcohol repeatedly again with 65% concentrated nitric acid agitator treating 12 hours
Cleaning.Then it places and is vented in vacuum oven, temperature is maintained at 100 DEG C, and the time is for 24 hours.It is taken after natural cooling at room temperature
Quartz boat out prepares uniform spiral carbon nano pipe (pipe diameter: 30~100nm；Pipe range: 1~10 μm；Spiral
0.2~2 μm of diameter).It is computed, carbon nanotube yield is 45%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of method that solid catalysis prepares spiral carbon nano pipe, comprising the following steps:
A organic carbon source and transition metal salt are mixed in water), obtain mixed solution；The organic carbon source include urea and/or
Melamine；The transition metal salt includes MnCl2And/or NiCl2；
The molar ratio of the organic carbon source and transition metal ions is (1~5): 1；
B) mixed solution is dried, obtains hybrid solid；
The temperature of the drying is 70~100 DEG C；The time of the drying is 6~12 hours；
C) hybrid solid is calcined, obtains spiral carbon nano pipe.
2. the method according to claim 1, wherein the step C) in the temperature calcined be 500~800 DEG C；
The step C) in calcine time be 4~7 hours.
3. according to the method described in claim 2, it is characterized in that, the temperature of the calcining passes through heating realization, the heating
Rate be 2~6 DEG C/min.
4. the method according to claim 1, wherein it is described calcining carried out under protective gas atmosphere, it is described
The flow velocity of protective gas is 50~200mL/min.
5. method described in any one according to claim 1~4, which is characterized in that the step C) after further include following step
It is rapid:
Calcined product is successively carried out to pickling, washing and alcohol to wash, obtains spiral carbon nano pipe.
6. according to the method described in claim 5, it is characterized in that, the pickling uses concentrated nitric acid, the quality of the concentrated nitric acid
Concentration is 60~70%.
7. according to the method described in claim 5, it is characterized in that, the alcohol is washed using ethyl alcohol, the volumetric concentration of the ethyl alcohol
It is 30~60%.
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| CN107570192B (en) * | 2017-08-21 | 2021-01-15 | 东莞理工学院 | Nickel-filled nitrogen-doped carbon nanotube and preparation method and application thereof |
| CN109879274A (en) * | 2019-04-26 | 2019-06-14 | 青岛科技大学 | Molte-salt synthesis prepares spiral carbon nano pipe and its preparation method and application |
| EP4051627A4 (en) * | 2019-10-29 | 2023-12-20 | C2Cnt Llc | Systems and methods for making carbon nanostructures |
| CN114367296B (en) * | 2020-10-15 | 2023-07-25 | 台州学院 | Catalyst for hydrodechlorination of chlorinated aromatic hydrocarbon and preparation method and application thereof |
| CN112604681A (en) * | 2020-12-14 | 2021-04-06 | 陕西科技大学 | Formaldehyde degradation material and preparation method and application thereof |
| CN112604680A (en) * | 2020-12-14 | 2021-04-06 | 陕西科技大学 | Formaldehyde decomposition material and preparation method and application thereof |
| CN113509951A (en) * | 2021-07-12 | 2021-10-19 | 深圳市康弘环保技术有限公司 | Preparation method and application of visible light catalytic nano material |
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