CN104192823A - Vapor purification method of carbon nanotubes - Google Patents
Vapor purification method of carbon nanotubes Download PDFInfo
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- CN104192823A CN104192823A CN201410391035.2A CN201410391035A CN104192823A CN 104192823 A CN104192823 A CN 104192823A CN 201410391035 A CN201410391035 A CN 201410391035A CN 104192823 A CN104192823 A CN 104192823A
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Abstract
The invention discloses a vapor purification method of carbon nanotubes. The vapor purification method of the carbon nanotubes comprises the following steps: filling the carbon nanotubes into a crucible, and pushing the crucible into a tubular furnace, under the protective atmosphere of a protective gas, raising the temperature of the tubular furnace to 600 DEG C-1100 DEG C, after the temperature of the tubular furnace reaches a set temperature, starting introducing a reactant gas and a diluted gas for reacting, after the reaction time is finished, stopping introducing the reactant gas and cooling the carbon nanotubes to room temperature in the presence of the diluted gas to obtain high-purity carbon nanotubes. The vapor purification method of the carbon nanotubes disclosed by the invention has the advantages of short reaction time, high production efficiency, no pollutant emission, small loss, high recovery rate and wide range of application. The carbon nanotubes have the characteristics of high purity, no need of secondary purification treatment and complete structure.
Description
Technical field
The present invention relates to carbon nanotube manufacturing technology field, relate in particular to a kind of vapor phase purification method of carbon nanotube.
Background technology
Existing liquid phase method of purification technical process complexity, processing speed is slow, and efficiency is low; In liquid phase purge process, use in a large number acid solutions and purify waste water, spent acid processing cost is high, contaminate environment; Carbon nanotube is washed middle sexual needs and is repeatedly washed, and water loss is very big, waste resource; Carbon nanotube is repeatedly washed and is produced many losses, affects the rate of recovery.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of vapor phase purification method of carbon nanotube, shortened process on the one hand, improve processing speed and production efficiency, solve on the other hand the problem of three wastes processing, reduce pollutant emission as far as possible, the purifying flow process of optimizing carbon nanotube, reduces production loss, improves the rate of recovery.
For solving the problems of the technologies described above, the invention provides a kind of vapor phase purification method of carbon nanotube, comprise the following steps:
(1) carbon nanotube is inserted in crucible, pushed in tube furnace;
(2), under the protective atmosphere of shielding gas, described tube furnace is warming up to 600 DEG C-1100 DEG C;
(3) described tube furnace furnace temperature arrives after design temperature, starts to pass into reactant gases and diluent gas reaction;
(4) reaction times stops passing into reactant gases after finishing, make described carbon nanotube at the protection borehole cooling of diluent gas to room temperature, obtain high-purity carbon nano tube.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, described in step (1), carbon nanotube is prepared with catalyzer, and described catalyzer is any one in Fe-Al component catalyst, Fe-Al-Mg component catalyst, La-Ni component catalyst and La-Ni-Co component catalyst.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, described in step (2), shielding gas is rare gas element or nitrogen.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, tube furnace described in step (2) is warming up to 600 DEG C-1100 DEG C with the speed of 10 DEG C/min.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, described in step (3), reactant gases is chlorine.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, described in diluent gas described in step (3) and step (2), shielding gas is gas of the same race.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, described in step (3), the volumetric concentration of reactant gases is 5%-10%, and surplus is described diluent gas.
As a kind of preferred version of the vapor phase purification method of a kind of carbon nanotube of the present invention, the reaction times described in step (4) is 120min.
The vapor phase purification method of carbon nanotube of the present invention, the carbon component that utilizes carbon nanotube not with the feature of chlorine reaction, use chlorine at a certain temperature with carbon nanotube in catalyst reaction, the muriate gasification that reaction generates, along with air-flow leaves carbon nanotube, thereby obtain highly purified carbon nanotube.Be characterized in: 1, utilize vapor phase process, single step reaction can reach the object of purifying, and the reaction times is short, and production efficiency is high; 2, purge process produces waste gas and impurity can be by lowered temperature reclamation processing, non-pollutant discharges; 3, the product after gas-phase reaction is carbon nanotube, does not need to carry out product separation, and loss is little, and the rate of recovery is high; 4, the carbon nano pipe purity that uses the method to obtain is high, does not need to carry out secondarily purified processing; 5, the carbon nanotube structure obtaining after purifying is complete, and inherent structure and the performance of purge process on carbon nanotube do not affect; 6, this purification process is applied widely, can be used for the purifying of carbon nanotube prepared by most metals catalyzer.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with embodiment, the present invention is further detailed explanation.
The vapor phase purification method of a kind of carbon nanotube that the present invention proposes, it comprises the steps or operates.
Step 1, inserts carbon nanotube in crucible, pushes in tube furnace.
In one embodiment, this step can specific as followsly be carried out: the carbon nanotube of preparing with catalyzer is inserted in crucible, push in tube furnace, wherein, described catalyzer is any one in Fe-Al component catalyst, Fe-Al-Mg component catalyst, La-Ni component catalyst and La-Ni-Co component catalyst.
Step 2, under the protective atmosphere of shielding gas, is warming up to 600 DEG C-1100 DEG C by described tube furnace.
In one embodiment, this step can specific as followsly be carried out: under the protective atmosphere of shielding gas, described tube furnace is warming up to 600 DEG C-1100 DEG C with the speed of 10 DEG C/min, wherein said shielding gas is rare gas element or nitrogen.
Step 3, described tube furnace furnace temperature arrives after design temperature, starts to pass into reactant gases and diluent gas reaction.
In one embodiment; this step can specific as followsly be carried out: described tube furnace furnace temperature arrives after design temperature; start to pass into chlorine and diluent gas reaction; the volumetric concentration of wherein said reactant gases is 5%-10%; surplus is described diluent gas, and shielding gas described in described diluent gas and step 2 is gas of the same race.
Step 4, stops passing into reactant gases after the reaction times finishes, make described carbon nanotube at the protection borehole cooling of diluent gas to room temperature, obtain high-purity carbon nano tube.
In one embodiment, this step can specific as followsly be carried out: reaction stops passing into reactant gases after 120min, make described carbon nanotube at the protection borehole cooling of diluent gas to room temperature, obtain high-purity carbon nano tube.
It is elaborated to production method of the present invention below in conjunction with specific embodiment.
Embodiment mono-
The carbon nanotube of preparing with Fe-Al component catalyst is inserted in crucible, pushed in tube furnace.Under the protection of nitrogen, be warming up to 600 DEG C with the speed of 10 DEG C/min.Furnace temperature arrives after design temperature, starts to pass into reaction gas.Chlorine gas concentration is 5%, and nitrogen gas concn is 95%, reaction 120min.After reaction times finishes, stop logical chlorine, make carbon nanotube at the protection borehole cooling of nitrogen to room temperature.
Product is purity higher than 99.9% carbon nanotube.
Embodiment bis-
The carbon nanotube of preparing with Fe-Al-Mg component catalyst is inserted in crucible, pushed in tube furnace.Under argon gas atmosphere, be warming up to 600 DEG C with the speed of 10 DEG C/min.Furnace temperature arrives after design temperature, starts to pass into reaction gas.Chlorine gas concentration is 5%, and argon concentration is 95%, reaction 120min.After reaction times finishes, stop logical chlorine, make carbon nanotube at the protection borehole cooling of argon gas to room temperature.
Product is purity higher than 99% carbon nanotube.
Embodiment tri-
The carbon nanotube of preparing with La-Ni component catalyst is inserted in crucible, pushed in tube furnace.Under argon gas atmosphere, be warming up to 1100 DEG C with the speed of 10 DEG C/min.Furnace temperature arrives after design temperature, starts to pass into reaction gas.Chlorine gas concentration is 10%, and argon concentration is 90%, reaction 120min.After reaction times finishes, stop logical chlorine, make carbon nanotube at the protection borehole cooling of argon gas to room temperature.
Product is purity higher than 99.9% carbon nanotube.
Embodiment tetra-
The carbon nanotube of preparing with La-Ni-Co component catalyst is inserted in crucible, pushed in tube furnace.Under helium atmosphere, be warming up to 1100 DEG C with the speed of 10 DEG C/min.Furnace temperature arrives after design temperature, starts to pass into reaction gas.Chlorine gas concentration is 10%, and concentrations of helium is 90%, reaction 120min.After reaction times finishes, stop logical chlorine, make carbon nanotube at the protection borehole cooling of helium to room temperature.
Product is purity higher than 99.9% carbon nanotube.
In sum, the vapor phase purification method of a kind of carbon nanotube of the present invention, the carbon component that utilizes carbon nanotube not with the feature of chlorine reaction, use chlorine at a certain temperature with carbon nanotube in catalyst reaction, the muriate gasification that reaction generates, along with air-flow leaves carbon nanotube, thereby obtain highly purified carbon nanotube.Be characterized in: 1, utilize vapor phase process, single step reaction can reach the object of purifying, and the reaction times is short, and production efficiency is high; 2, purge process produces waste gas and impurity can be by lowered temperature reclamation processing, non-pollutant discharges; 3, the product after gas-phase reaction is carbon nanotube, does not need to carry out product separation, and loss is little, and the rate of recovery is high; 4, the carbon nano pipe purity that uses the method to obtain is high, does not need to carry out secondarily purified processing; 5, the carbon nanotube structure obtaining after purifying is complete, and inherent structure and the performance of purge process on carbon nanotube do not affect; 6, this purification process is applied widely, can be used for the purifying of carbon nanotube prepared by most metals catalyzer.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (8)
1. a vapor phase purification method for carbon nanotube, it comprises:
(1) carbon nanotube is inserted in crucible, pushed in tube furnace;
(2), under the protective atmosphere of shielding gas, described tube furnace is warming up to 600 DEG C-1100 DEG C;
(3) described tube furnace furnace temperature arrives after design temperature, starts to pass into reactant gases and diluent gas reaction;
(4) reaction times stops passing into reactant gases after finishing, make described carbon nanotube at the protection borehole cooling of diluent gas to room temperature, obtain high-purity carbon nano tube.
2. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, it is characterized in that: described in step (1) prepared by carbon nanotube catalyzer, described catalyzer is any one in Fe-Al component catalyst, Fe-Al-Mg component catalyst, La-Ni component catalyst and La-Ni-Co component catalyst.
3. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, is characterized in that: described in step (2), shielding gas is rare gas element or nitrogen.
4. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, is characterized in that: tube furnace described in step (2) is warming up to 600 DEG C-1100 DEG C with the speed of 10 DEG C/min.
5. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, is characterized in that: described in step (3), reactant gases is chlorine.
6. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, is characterized in that: described in diluent gas described in step (3) and step (2), shielding gas is gas of the same race.
7. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, is characterized in that: described in step (3), the volumetric concentration of reactant gases is 5%-10%, and surplus is described diluent gas.
8. the vapor phase purification method of a kind of carbon nanotube as claimed in claim 1, is characterized in that: the reaction times described in step (4) is 120min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107074548A (en) * | 2015-09-15 | 2017-08-18 | Lg化学株式会社 | With the crystalline CNT of improvement |
| CN109502572A (en) * | 2018-12-29 | 2019-03-22 | 苏州第元素纳米技术有限公司 | Carbon nanotube method of purification |
| CN109809394A (en) * | 2019-03-25 | 2019-05-28 | 青岛超瑞纳米新材料科技有限公司 | A kind of iodine purifying plant and its method of purification based on carbon nanotube |
| CN115535997A (en) * | 2022-09-28 | 2022-12-30 | 上海岚玥新材料科技有限公司 | Efficient purification system device and process for carbon material |
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| US20100143234A1 (en) * | 2008-12-04 | 2010-06-10 | Sony Corporation | Methods of preparing and purifying carbon nanotubes, carbon nanotubes, and an element using the same |
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| CN1475438A (en) * | 2003-07-18 | 2004-02-18 | 清华大学 | Purification method of carbon nano pipe and its device |
| CN101041427A (en) * | 2006-03-22 | 2007-09-26 | 索尼株式会社 | Manufacturing method of carbon material, carbon material and manufacturing method of electronic components |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107074548A (en) * | 2015-09-15 | 2017-08-18 | Lg化学株式会社 | With the crystalline CNT of improvement |
| CN109502572A (en) * | 2018-12-29 | 2019-03-22 | 苏州第元素纳米技术有限公司 | Carbon nanotube method of purification |
| CN109809394A (en) * | 2019-03-25 | 2019-05-28 | 青岛超瑞纳米新材料科技有限公司 | A kind of iodine purifying plant and its method of purification based on carbon nanotube |
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| CN115535997B (en) * | 2022-09-28 | 2023-09-29 | 上海岚玥新材料科技有限公司 | High-efficiency purifying system device and process for carbon materials |
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