CN107032326A - 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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- CN107032326A CN107032326A CN201710257230.XA CN201710257230A CN107032326A CN 107032326 A CN107032326 A CN 107032326A CN 201710257230 A CN201710257230 A CN 201710257230A CN 107032326 A CN107032326 A CN 107032326A
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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
- 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
- C01P2004/62—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, comprises the following steps：A) organic carbon source and transition metal ions are mixed in water, mixed solution is obtained；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, hybrid solid is obtained；C) hybrid solid is calcined, spiral carbon nano pipe is obtained.Method carbon source in the present invention is with low cost with catalyst, is readily available, and early-stage preparations processing method is simple and easy to apply, is advantageously implemented volume production；Nickeliferous and/or manganese catalyst catalytic performance is good, can be up to 45% with the substantial amounts of spiral helicine carbon nanotube product of generation, yield；Involved equipment is simple, and required reaction condition easily reaches；The spiral carbon nano pipe size distribution produced is uniform.
Description
Technical field
The invention belongs to field of nanometer technology, more particularly to a kind of method that solid catalysis prepares spiral carbon nano pipe.
Background technology
The preparation and its utilization of CNT are the focuses of current nanometer technology and material science research.CNT has
Good chemical property, excellent mechanical property and good thermal property.These exclusive outstanding performances cause carbon nanometer
Pipe is widely used in numerous frontier science and technology fields, for example, high-performance conductive composite, super capacitor and electrode material, intelligence
Can robot and biomedicine etc..
Early in 1991, Japanese scientist Iijima was just found that using graphite arc equipment to prepare carbon in accident
Nanotube, and observe with high-resolution-ration transmission electric-lens the clear structure of CNT.Then, the preparation method of CNT is each
State scientific research personnel further studies invention, a series of to come in every shape and the CNT with different physical and chemical properties
Researched and developed.1994, Zhang etc. was found that the carbon nanometer with neat regular helix shape with transmission electron microscope first
Pipe.Spiral carbon nano pipe also has its special helicoidal structure institute while possessing common CNT numerous excellent in performance
The peculiar advantage brought, for example, good energy absorption capability and synthesizing the composite with stronger performance with other materials.
Up to the present, preparing the method for spiral carbon nano pipe has graphite acr method, laser evaporization method and chemical gaseous phase
Deposit (CVD), although but this 3 major class preparation method can realize the synthesis of spiral carbon nano pipe because itself
Limitation can not be produced largely, for example, graphite acr method and laser evaporization method need the output of high-energy and helical form carbon is received
Mitron is generally accessory substance, and preparation amount is less, and CVD also has while needing high energy to export to the catalyst of its central role
Very high requirement.
The content of the invention
It is an object of the invention to provide a kind of method that solid catalysis prepares spiral carbon nano pipe, what the present invention was provided
Equipment needed for method is simple, and reaction condition easily reaches, and yield is higher, easily realizes volume production.
The present invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprises the following steps：
A) organic carbon source and transition metal ions are mixed in water, mixed solution is obtained；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, hybrid solid is obtained；
C) hybrid solid is calcined, spiral carbon nano pipe is obtained.
It is preferred that, the step A) be specially：
Organic carbon source and transition metal salt are mixed in water, mixed solution is obtained；
The transition metal salt includes MnCl2And/or NiCl2。
It is preferred that, the mol ratio of the organic carbon source and transition metal ions is (1~5)：1.
It is preferred that, the step B) in dry temperature be 70~100 DEG C；
The step B) in dry time be 6~12 hours.
It is preferred that, the step C) in calcining temperature be 500~800 DEG C；
The step C) in calcining time be 4~7 hours.
It is preferred that, the temperature of the calcining is realized by heating up, and the speed of the heating is 2~6 DEG C/min.
It is preferred that, the calcining is carried out under protective gas atmosphere, the flow velocity of the protective gas for 50~
200mL/min。
It is preferred that, the step C) it is further comprising the steps of afterwards：
Product after calcining is carried out to pickling, washing and alcohol successively to wash, spiral carbon nano pipe is obtained.
It is preferred that, the pickling uses concentrated nitric acid, and the mass concentration of the concentrated nitric acid is 60~70%.
It is preferred that, the alcohol, which is washed, uses ethanol, and the volumetric concentration of the ethanol is 30~60%.
The present invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprises the following steps：A) will be 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, hybrid solid is obtained；
C) hybrid solid is calcined, spiral carbon nano pipe is obtained.The method that the present invention is provided has advantages below：
(1) carbon source is with low cost with catalyst, is readily available, and early-stage preparations processing method is simple and easy to apply, is advantageously implemented
Volume production.
(2) nickeliferous and/or manganese catalyst catalytic performance is good, and catalyzing urea and/or melamine can be with substantial amounts of generations
Spiral helicine carbon nanotube product, yield is up to 45%.
(3) equipment involved by is simple, and required reaction condition easily reaches.
(4) the spiral carbon nano pipe size distribution produced is uniform.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
Fig. 1 is the SEM figures of spiral carbon nano pipe in the embodiment of the present invention 1；
Fig. 2 is the TEM figures of spiral carbon nano pipe in the embodiment of the present invention 1.
Embodiment
The invention provides a kind of method that solid catalysis prepares spiral carbon nano pipe, comprise the following steps：
A) organic carbon source and transition metal ions are mixed in water, mixed solution is obtained；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, hybrid solid is obtained；
C) hybrid solid is calcined, spiral carbon nano pipe is obtained.
Reaction in the present invention is using melamine and/or urea as carbon source, and transition metal is catalyst, reaction condition letter
It is single, easily reach, and yield is higher, easily realizes volume production.
The present invention mixes organic carbon source and transition metal ions in water, mixed solution is obtained, preferably by organic carbon source
Mixed with transition metal salt in water, obtain 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 includes MnCl2And/or NiCl2；The water is preferably deionized water, described to have
Machine carbon source and the mol ratio of transition metal ions are preferably (1~5)：1, more preferably (2~4)：1, most preferably 3:1.
Mixed solution described in preferred pair of the present invention is stirred, enable it is dispersed in water, the present invention 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 puts the mixed solution
It is dried in vacuum drying chamber, the temperature of the drying is preferably 70~100 DEG C, 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.
Obtain after hybrid solid, the present invention is preferably milled the hybrid solid, obtains mixed-powder, the mixing
The particle diameter of powder is preferably 10~100 μm, more preferably 20~80 μm, most preferably 30~70 μm.
The present invention is preferably calcined mixed-powder, obtains spiral carbon nano pipe, the present invention is preferably by the mixing
Powder is put into tube furnace and calcined, and the temperature of the calcining is preferably 500~800 DEG C, preferably 550~750 DEG C, optimal
Elect 600~700 DEG C as；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 calcining keeps logical protective gas to the calcining production after terminating
Product are cooled 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.
Complete after the calcining, the product after the calcining is preferably carried out pickling, washing and alcohol and washed by the present invention successively, is obtained
To spiral carbon nano pipe, the present invention agitator treating 10~12 hours, Ran Houzai in concentrated nitric acid preferably by the product after calcining
Cleaned repeatedly with deionized water and ethanol.In the present invention, the mass concentration of the concentrated nitric acid is preferably 60~70%, more preferably
For 65%；The volumetric concentration of the ethanol is preferably 30~60%, more preferably 35~55%, most preferably 40~50%.
Complete after cleaning, preferably the product after cleaning is dried again by the present invention, obtains spiral carbon nano pipe institute
It is preferably 70~100 DEG C to state dry temperature, 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 carries out the drying preferably in vacuum drying chamber.
According to spiral carbon nano pipe made from the method in the present invention, size is homogeneous, carbon nanotube diameter be 30~
300nm, pipe range is 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, comprises the following steps：A) will be 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, hybrid solid is obtained；
C) hybrid solid is calcined, spiral carbon nano pipe is obtained.The method that the present invention is provided has advantages below：
(1) carbon source is with low cost with catalyst, is readily available, and early-stage preparations processing method is simple and easy to apply, is advantageously implemented
Volume production.
(2) nickeliferous and/or manganese catalyst catalytic performance is good, and catalyzing urea and/or melamine can be with substantial amounts of generations
Spiral helicine carbon nanotube product, yield is up to 45%.
(3) equipment involved by is simple, and required reaction condition easily reaches.
(4) the spiral carbon nano pipe size distribution produced is uniform.
In order to further illustrate the present invention, prepared by spiral to a kind of solid catalysis that the present invention is provided with reference to embodiments
The method of shape CNT is described in detail, but can not be understood as limiting the scope of the present invention.
In following examples, the yield of CNT is calculated according to below equation：
Wherein, m1 is the quality of CNT, and m2 (reacts the matter of early transition metal salt for the quality of reaction procatalyst
Amount).
Embodiment 1
Take 1g urea and 1gMnCl2It is dissolved in respectively in deionized water, mixture stirring 30min, to cause urea and MnCl2
Uniformly it can disperse in water.Obtained mixed solution is placed in vacuum drying chamber and is vented, temperature is maintained at 70 DEG C, 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 is 4 hours.Treat that calcining terminates, allow medicine to continue to keep logical nitrogen state in tube furnace, naturally cool to
Room temperature.Then use deionized water and alcohol repeatedly clear again within 12 hours with 65% concentrated nitric acid agitator treating the material baked
Wash.Then place in vacuum drying chamber and be vented, temperature is maintained at 70 DEG C, and the time is 8h.At room temperature stone is taken out after natural cooling
Ying Zhou, that is, prepare uniform spiral carbon nano pipe (pipe diameter：100~300nm；Pipe range：10~30 μm；Spiral is straight
1~3 μm of footpath).It is computed, CNT yield is 30%.
The present invention has carried out ESEM 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 figures 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 figures of middle spiral carbon nano pipe.
Embodiment 2
Take 3g melamines and 1gNiCl2Be dissolved in respectively in deionized water, mixture stirring 2h, with cause melamine and
NiCl2Uniformly it can disperse in water.Obtained mixed solution is placed in vacuum drying chamber and is vented, 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.Treat that calcining terminates, allow medicine to continue to keep logical nitrogen state in tube furnace, it is natural
It is cooled to room temperature.The material baked is used into deionized water and alcohol repeatedly with 65% concentrated nitric acid agitator treating 12 hours and then again
Cleaning.Then place in vacuum drying chamber and be vented, temperature is maintained at 80 DEG C, and the time is 16h.Taken out at room temperature after natural cooling
Quartz boat, that is, prepare uniform spiral carbon nano pipe (pipe diameter：50~200nm；Pipe range：5~20 μm；Spiral is straight
0.5~2 μm of footpath).It is computed, CNT yield is 40%.
Embodiment 3
Take 5g melamines and 1gMnCl2Be dissolved in respectively in deionized water, mixture stirring 3h, with cause melamine and
MnCl2Uniformly it can disperse in water.Obtained mixed solution is placed in vacuum drying chamber and is vented, 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.Treat that calcining terminates, allow medicine to continue to keep logical nitrogen state in tube furnace, it is natural
It is cooled to room temperature.The material baked is used into deionized water and alcohol repeatedly with 65% concentrated nitric acid agitator treating 12 hours and then again
Cleaning.Then place in vacuum drying chamber and be vented, temperature is maintained at 100 DEG C, and the time is 24h.Taken at room temperature after natural cooling
Go out quartz boat, that is, prepare uniform spiral carbon nano pipe (pipe diameter：30~100nm；Pipe range：1~10 μm；Spiral
0.2~2 μm of diameter).It is computed, CNT yield is 45%.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method that solid catalysis prepares spiral carbon nano pipe, comprises the following steps：
A) organic carbon source and transition metal ions are mixed in water, mixed solution is obtained；The organic carbon source include urea and/
Or melamine；The transition metal ions includes nickel ion and/or manganese ion；
B) mixed solution is dried, hybrid solid is obtained；
C) hybrid solid is calcined, spiral carbon nano pipe is obtained.
2. it is specially according to the method described in claim 1, it is characterised in that the step A)：
Organic carbon source and transition metal salt are mixed in water, mixed solution is obtained；
The transition metal salt includes MnCl2And/or NiCl2。
3. according to the method described in claim 1, it is characterised in that the mol ratio of the organic carbon source and transition metal ions is
(1~5)：1.
4. the temperature dried according to the method described in claim 1, it is characterised in that the step B) is 70~100 DEG C；
The step B) in dry time be 6~12 hours.
5. the temperature of calcining is 500~800 DEG C according to the method described in claim 1, it is characterised in that the step C)；
The step C) in calcining time be 4~7 hours.
6. method according to claim 4, it is characterised in that the temperature of the calcining passes through the realization, the heating of heating up
Speed be 2~6 DEG C/min.
7. according to the method described in claim 1, it is characterised in that the calcining is carried out under protective gas atmosphere, described
The flow velocity of protective gas is 50~200mL/min.
8. the method according to claim 1~7 any one, it is characterised in that the step C) after also include following step
Suddenly：
Product after calcining is carried out to pickling, washing and alcohol successively to wash, spiral carbon nano pipe is obtained.
9. method according to claim 7, it is characterised in that the pickling uses concentrated nitric acid, the quality of the concentrated nitric acid
Concentration is 60~70%.
10. method according to claim 7, it is characterised in that the alcohol, which is washed, uses ethanol, the volumetric concentration of the ethanol
For 30~60%.
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Cited By (7)
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| CN107570192A (en) * | 2017-08-21 | 2018-01-12 | 东莞理工学院 | A kind of nickel filling nitrogen doped carbon nanotube and its preparation method and application |
| 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 |
| CN112604680A (en) * | 2020-12-14 | 2021-04-06 | 陕西科技大学 | Formaldehyde decomposition material 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 |
| 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 |
| CN114367296A (en) * | 2020-10-15 | 2022-04-19 | 台州学院 | Catalyst for hydrodechlorination of chlorinated aromatic hydrocarbon and preparation method and application thereof |
| CN114630926A (en) * | 2019-10-29 | 2022-06-14 | C2Cnt有限责任公司 | System and method for fabricating carbon nanostructures |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107570192A (en) * | 2017-08-21 | 2018-01-12 | 东莞理工学院 | A kind of nickel filling nitrogen doped carbon nanotube and its preparation method and application |
| 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 |
| CN114630926A (en) * | 2019-10-29 | 2022-06-14 | C2Cnt有限责任公司 | System and method for fabricating carbon nanostructures |
| EP4051627A4 (en) * | 2019-10-29 | 2023-12-20 | C2Cnt Llc | Systems and methods for making carbon nanostructures |
| CN114367296A (en) * | 2020-10-15 | 2022-04-19 | 台州学院 | Catalyst for hydrodechlorination of chlorinated aromatic hydrocarbon and preparation method and application thereof |
| 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 |
| CN112604680A (en) * | 2020-12-14 | 2021-04-06 | 陕西科技大学 | Formaldehyde decomposition material 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 |
| 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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