CN105060271A - Carbon nano-tube purification method - Google Patents
Carbon nano-tube purification method Download PDFInfo
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- CN105060271A CN105060271A CN201510466039.7A CN201510466039A CN105060271A CN 105060271 A CN105060271 A CN 105060271A CN 201510466039 A CN201510466039 A CN 201510466039A CN 105060271 A CN105060271 A CN 105060271A
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Abstract
The invention provides a carbon nano-tube purification method, which mainly comprises: a, during or completing a carbon nano-tube preparation process through fixed bed or fluidized bed equipment, introducing a reducing gas and/or an inert gas, wherein specifically the gas is hydrogen and/or carbon dioxide, the reaction temperature is 100-800 DEG C, the reaction time is 3-60 min, and the gas flow rate is 0.06-1000 m<3>/h; and b, stopping the introducing of the reducing gas, cooling to a room temperature in the protection of an inert gas so as to obtain the carbon nano-tubes with the purity of more than or equal to 99.5%, wherein the inert gas is nitrogen and/or argon. With the method of the present invention, the impurity can be removed under the premise of no damage on the carbon tubes, the advantages of simple process, easy operation, high purification efficiency, low cost and the like are provided, and the method is suitable for industrial large-batch purification of the carbon nano-tubes.
Description
Technical field
The present invention relates to carbon nanotube preparation technology field, particularly a kind of method of purification of carbon nanotube in enormous quantities.
Background technology
1991 the end of the year Japanese scholars Lijimat found the carbon nanotube that is made up of carbon atom, because its structure is special, as the body of typical one dimension Nano structure, hollow, it has high axial strength (being about the l00 of steel doubly) and very high Young's modulus, the surface atom of length-to-diameter ratio large (-as be 100 ~ l000), superelevation is than, the character such as high-temperature stable, anti-friction wear-resistant are good, thermal conductivity is good, carbon nanotube shows many properties diverse with other carbonaceous materials, therefore is applied to the field such as Novel electronic devices or new function material.Current carbon nanotube be prepared as in a large number research its physics and chemistry characteristic and practical application provide possibility, but the carbon nanotube utilizing the method such as arc process and Floating catalyst method to prepare is usually with a considerable amount of impurity, as carbon nano-particle, amorphous carbon, Nano carbon balls and catalyst particle etc.The existence of these impurity greatly hinders physical property research and the practical application of carbon nanotube, is therefore more and more paid attention to the purifying research of carbon nanotube.Current purification route mainly utilizes the minute differences of the aspect such as reason, chemistry of the impurity such as carbon nanotube and amorphous carbon to reach the object of purification; method of purification mainly contains: chemical oxidization method, vapour phase oxidation process, liquid phase oxidation, intercalation oxidation style etc.; but these methods are only suitable for a small amount of carbon nanotube purifies; such as (see figure 1): carbon nanotube prepared by fixed bed unit; temperature of reaction is 500 DEG C; do not pass into reducing gas, pass into nitrogen protection, gas flow rate is 150m
3/ h, drops to room temperature, and take out, what obtain is low-purity carbon nanotube.But the effective ways being industrially applicable to preparation purification carbon nanotube in enormous quantities still lack, and therefore, urgently invent a kind of method of purification being applicable to carbon nanotube in enormous quantities.
Summary of the invention
The object of this invention is to provide a kind of carbon nanotube method of purification, it is suitable for the purification of carbon nanotube in enormous quantities, solves in prior art and is only that a small amount of carbon nanotube is purified and the problem such as the carbon nano pipe purity obtained is not high.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of carbon nanotube method of purification, and the method comprises:
A, prepare after carbon nanotube completes at fixed bed or fluidized bed plant, temperature of reaction is risen to 100 DEG C-800 DEG C, passing into gas flow rate is 0.06m
3/ h-1000m
3the reducing gas of/h and/or rare gas element, the reaction times is 3-60 minute; Described reducing gas is hydrogen and/or carbonic acid gas; Described rare gas element is nitrogen.
B, stopping pass into described reducing gas, drop to room temperature, namely obtain described carbon nanotube in the protection of rare gas element; Described rare gas element is nitrogen or argon gas.
Further, described temperature of reaction is 100 DEG C, and described reducing gas is hydrogen, and the gas flow rate of described hydrogen is 100m
3/ h, the described reaction times is 20 minutes; Described rare gas element is nitrogen.
Further, described temperature of reaction is upgraded to 600 DEG C, and described reducing gas is hydrogen, and the gas flow rate of described hydrogen is 500m
3/ h, the described reaction times is 20 minutes; Described rare gas element is nitrogen.
Further, described temperature of reaction is 700 DEG C, and described reducing gas and rare gas element are hydrogen and nitrogen mixed gas, and the gas flow rate of described hydrogen is 80m
3/ h, the gas overall flow rate of described hydrogen and nitrogen mixed gas is 300m
3/ h, the described reaction times is 60 minutes; Described rare gas element is nitrogen.
Further, described temperature of reaction is 800 DEG C, and described reducing gas and rare gas element are carbonic acid gas and nitrogen mixed gas, and the gas flow rate of described carbonic acid gas is 0.06m
3/ h, the gas overall flow rate of described carbonic acid gas and nitrogen mixed gas is 500m
3/ h, the described reaction times is 3 minutes; Described rare gas element is nitrogen.
Further, described temperature of reaction is 300 DEG C, and described reducing gas is carbon dioxide, and the gas flow rate of described carbonic acid gas is 1000m
3/ h, the described reaction times is 20 minutes; Described rare gas element is argon gas.
Further, described carbon nanotube is Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
As shown from the above technical solution, advantage of the present invention and positively effect are: the present invention can Impurity removal under the prerequisite not injuring carbon pipe, there is technique simple, the advantages such as convenient to operation and cost is lower, be applicable to large batch of carbon nanotube to purify, and the carbon nano pipe purity obtained all reaches more than 99.5%.
Accompanying drawing explanation
Fig. 1 is the SEM scintigram of low-purity carbon nanotube in prior art.
Fig. 2 is the SEM scintigram of high-purity carbon nano tube in the present embodiment.
Embodiment
The exemplary embodiment embodying feature & benefits of the present invention will describe in detail in the following description.Be understood that the present invention can have various changes on different embodiments, it neither departs from the scope of the present invention, and explanation wherein and to be shown in be use when explain in essence, and be not used to limit the present invention.
The present invention proposes a kind of carbon nanotube method of purification, and this carbon nanotube is Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.Now the specific embodiment of carbon nanotube method of purification of the present invention is described below:
embodiment one
Prepare after carbon nanotube completes at fixed bed unit, temperature of reaction is risen to 100 DEG C, passing into gas flow rate is 100m
3the hydrogen of/h, the reaction times is 20 minutes.
Stop passing into hydrogen, pass into nitrogen, under the protection of nitrogen, temperature drops to room temperature gradually, and namely obtain the carbon nanotube of purity more than 99.5%, purification process completes, see the SEM scintigram of Fig. 2 high-purity carbon nano tube.
embodiment two
Prepare after carbon nanotube completes at fluidized bed plant, temperature of reaction is upgraded to 600 DEG C, passing into gas flow rate is 500m
3the hydrogen of/h, the reaction times is 20 minutes.
Stop passing into hydrogen, pass into nitrogen, under the protection of nitrogen, temperature drops to room temperature gradually, and namely obtain the carbon nanotube of purity more than 99.5%, purification process completes.
embodiment three
Prepare after carbon nanotube completes at fluidized bed plant, temperature of reaction is upgraded to 700 DEG C, passes into hydrogen and nitrogen mixed gas, the gas flow rate of hydrogen is 80m
3/ h, the gas overall flow rate of hydrogen and nitrogen mixed gas is 300m
3/ h, the reaction times is 60 minutes.
Stop passing into hydrogen, temperature drops to room temperature gradually under nitrogen protection, and namely obtain the carbon nanotube of purity more than 99.5%, purification process completes.
embodiment four
Prepare after carbon nanotube completes at fluidized bed plant, temperature of reaction is upgraded to 800 DEG C, passes into carbonic acid gas and nitrogen mixed gas, the gas flow rate of carbonic acid gas is 0.06m
3/ h, the gas overall flow rate of carbonic acid gas and nitrogen mixed gas is 500m
3/ h, the reaction times is 3 minutes.
Stop passing into carbonic acid gas, under the protection of nitrogen, temperature drops to room temperature gradually, and namely obtain the carbon nanotube of purity more than 99.5%, purification process completes.
embodiment five
Prepare after carbon nanotube completes at fluidized bed plant, temperature of reaction is upgraded to 300 DEG C, passes into the carbon dioxide that gas flow rate is 1000m3/h, the reaction times is 20 minutes.
Stop passing into carbonic acid gas, pass into argon gas, under the protection of argon gas, temperature drops to room temperature gradually, and namely obtain the carbon nanotube of purity more than 99.5%, purification process completes.
It is Powdered, particulate state or the two mixing that the various embodiments described above are applicable to carbon nanotube form; Be applicable to the purification of carbon nanotube prepared by the different activities component catalysts such as iron, cobalt, nickel simultaneously, effectively can remove iron, cobalt, nickel metallic impurity.Reducing gas in the embodiment of the present invention and non-carbonic nanotube material (as impurity such as decolorizing carbon) react, and can not damage carbon nanotube, and the removal of impurity of getting on the basis of guarantee carbon nanotube performance, reaches high-purity carbon nano tube.The method of purification technique of carbon nanotube of the present invention is simple, and easy to operate, cost is low, is adapted at industrial large batch of carbon nanotube and purifies.
In addition, in the embodiment of the present invention analytical pure of reducing gas and rare gas element all more than 99.9%.
Although describe the present invention with reference to exemplary embodiment, should be appreciated that term used illustrates and exemplary and nonrestrictive term.Spirit or the essence of invention is not departed from because the present invention can specifically implement in a variety of forms, so be to be understood that, above-mentioned embodiment is not limited to any aforesaid details, and explain widely in the spirit and scope that should limit in claim of enclosing, therefore fall into whole change in claim or its equivalent scope and remodeling and all should be claim of enclosing and contained.
Claims (7)
1. a carbon nanotube method of purification, is characterized in that, the method comprises:
A, prepare after carbon nanotube completes at fixed bed or fluidized bed plant, temperature of reaction is risen to 100 DEG C-800 DEG C, passing into gas flow rate is 0.06m
3/ h-1000m
3the reducing gas of/h and/or rare gas element, the reaction times is 3-60 minute; Described reducing gas is hydrogen and/or carbonic acid gas; Described rare gas element is nitrogen;
B, stopping pass into described reducing gas, drop to room temperature, namely obtain described carbon nanotube in the protection of rare gas element; Described rare gas element is nitrogen or argon gas.
2. carbon nanotube method of purification as claimed in claim 1, it is characterized in that, described temperature of reaction is 100 DEG C, and described reducing gas is hydrogen, and the gas flow rate of described hydrogen is 100m
3/ h, the described reaction times is 20 minutes; Described rare gas element is nitrogen.
3. carbon nanotube method of purification as claimed in claim 1, it is characterized in that, described temperature of reaction is upgraded to 600 DEG C, and described reducing gas is hydrogen, and the gas flow rate of described hydrogen is 500m
3/ h, the described reaction times is 20 minutes; Described rare gas element is nitrogen.
4. carbon nanotube method of purification as claimed in claim 1, it is characterized in that, described temperature of reaction is 700 DEG C, and described reducing gas and rare gas element are hydrogen and nitrogen mixed gas, and the gas flow rate of described hydrogen is 80m
3/ h, the gas overall flow rate of described hydrogen and nitrogen mixed gas is 300m
3/ h, the described reaction times is 60 minutes; Described rare gas element is nitrogen.
5. carbon nanotube method of purification as claimed in claim 1, it is characterized in that, described temperature of reaction is 800 DEG C, and described reducing gas and rare gas element are carbonic acid gas and nitrogen mixed gas, and the gas flow rate of described carbonic acid gas is 0.06m
3/ h, the gas overall flow rate of described carbonic acid gas and nitrogen mixed gas is 500m
3/ h, the described reaction times is 3 minutes; Described rare gas element is nitrogen.
6. carbon nanotube method of purification as claimed in claim 1, it is characterized in that, described temperature of reaction is 300 DEG C, and described reducing gas is carbon dioxide, and the gas flow rate of described carbonic acid gas is 1000m
3/ h, the described reaction times is 20 minutes; Described rare gas element is argon gas.
7. carbon nanotube method of purification as claimed in claim 1, it is characterized in that, described carbon nanotube is Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
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Cited By (7)
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| CN106185867A (en) * | 2016-08-22 | 2016-12-07 | 赖世权 | The purity of CNT improves method |
| CN106185870A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | The Carbon nanotube purification system of reuse heat energy |
| CN106315560A (en) * | 2016-08-22 | 2017-01-11 | 赖世权 | Carbon nanotube purification method |
| CN108682511A (en) * | 2018-04-03 | 2018-10-19 | 信阳师范学院 | The method for improving carbon nanotube film conductivity |
| CN109273726A (en) * | 2018-02-08 | 2019-01-25 | 成都理工大学 | A kind of carbon coated air electrode material and its preparation method and application |
| CN111498835A (en) * | 2020-04-27 | 2020-08-07 | 内蒙古骏成新能源科技有限公司 | Horizontal fluidizing device for gas-phase purification of carbon nano tube and fluidizing purification method |
| CN115215326A (en) * | 2022-02-23 | 2022-10-21 | 无锡东恒新能源科技有限公司 | Pre-oxidation device for carbon nano tube purification |
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Cited By (7)
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| CN109273726A (en) * | 2018-02-08 | 2019-01-25 | 成都理工大学 | A kind of carbon coated air electrode material and its preparation method and application |
| CN108682511A (en) * | 2018-04-03 | 2018-10-19 | 信阳师范学院 | The method for improving carbon nanotube film conductivity |
| CN111498835A (en) * | 2020-04-27 | 2020-08-07 | 内蒙古骏成新能源科技有限公司 | Horizontal fluidizing device for gas-phase purification of carbon nano tube and fluidizing purification method |
| CN115215326A (en) * | 2022-02-23 | 2022-10-21 | 无锡东恒新能源科技有限公司 | Pre-oxidation device for carbon nano tube purification |
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