CN106365146A - Impurity removal method of carbon nanotubes - Google Patents
Impurity removal method of carbon nanotubes Download PDFInfo
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- CN106365146A CN106365146A CN201610705090.3A CN201610705090A CN106365146A CN 106365146 A CN106365146 A CN 106365146A CN 201610705090 A CN201610705090 A CN 201610705090A CN 106365146 A CN106365146 A CN 106365146A
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- impurity
- carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
Abstract
The invention discloses an impurity removal method of carbon nanotubes. The method comprises the following steps: 1, placing the carbon nanotubes in nitrogen atmosphere, continuously introducing carbon dioxide at a flow velocity of 340-370 m<3>/h, carrying out a reaction at 650-680 DEG C for 30-40 min, introducing nitrogen to cool the carbon nanotubes at a controlled cooling rate of 30-40 DEG C/min, continuously introducing nitrogen for 10 min when the temperature decreases to 440 DEG C, continuously introducing hydrogen at a flow velocity of 200 m<3>/h, carrying out a reaction at 440 DEG C for 10 min, continuously introducing for 20 min, and keeping the temperature of nitrogen at 440 DEG C; and 2, keeping the carbon nanotubes in nitrogen atmosphere, and continuously introducing nitrogen to cool the carbon nanotubes. The method realizes purification of a large batch of the carbon nanotubes, and makes the purity of the carbon nanotubes reach 99.9%.
Description
Technical field
The present invention relates to a kind of impurity-removing method of CNT.
Background technology
1991 end of the year Japanese scholars lijimat are found that the CNT being made up of carbon atom, because its structure is special, such as
Typical one-dimensional nano structure, the body of hollow, it has high axial strength l00 times of steel (about) and very high elasticity
Modulus, draw ratio big (as be 100～l000), superelevation surface atom than, high-temperature stable, anti-friction wear-resistant be good, heat conductivity
The property such as good, CNT shows the many and diverse property of other carbonaceous materials, therefore is applied to Novel electric
The field such as sub- device or new function material.At present CNT be prepared as in a large number study its physics and chemical characteristic and reality
Application provides possibility, but is frequently accompanied by quite counting using the CNT that the methods such as arc process and Floating catalyst method are prepared
The impurity of amount, such as carbon nano-particle, amorphous carbon, Nano carbon balls and catalyst particle etc..The very big ground resistance of presence of these impurity
Hinder physical property research and the practical application of CNT, therefore the purifying research of CNT has more and more been weighed
Depending on.Current purification route is mainly used CNT and is come with the minute differences of the aspects such as the reason of impurity, chemistry such as amorphous carbon
Reach the purpose of purification, method of purification mainly has: chemical oxidization method, vapour phase oxidation process, liquid phase oxidation, intercalation oxidizing process etc.,
But these methods are only suitable for a small amount of CNT purification, and obtain is low-purity CNT.It would therefore be highly desirable to invention is a kind of suitable
Close the impurity-removing method of high-volume CNT.
Content of the invention
The present invention has designed and developed a kind of impurity-removing method of the high CNT of purification efficiency.
The technical scheme that the present invention provides is:
A kind of impurity-removing method of CNT, comprising:
CNT is first placed in nitrogen atmosphere step (1), is continually fed into carbon dioxide, and the flow velocity of carbon dioxide is
340～370m3/ h, the response time is 30～40min, and reaction temperature is 650～680 DEG C, is passed through nitrogen that CNT is entered
Row cooling, and control rate of temperature fall to be 30～40 DEG C/min, when cooling to 440 DEG C, then it is continually fed into nitrogen 10min, afterwards again
It is continually fed into hydrogen, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C, persistently leads to afterwards again
Enter nitrogen 20min, the temperature of nitrogen is maintained at 440 DEG C；
CNT is maintained in nitrogen atmosphere step (2), by being continually fed into nitrogen, CNT is dropped
Temperature, rate of temperature fall is 13～15 DEG C/min, until the temperature of CNT is reduced to room temperature.
Preferably, in the impurity-removing method of described CNT, in described step (1), the response time is 35min, instead
Temperature is answered to be 680 DEG C.
Preferably, in the impurity-removing method of described CNT, in described step (1), the flow velocity of carbon dioxide is
365m3/h.
Preferably, in the impurity-removing method of described CNT, in described step (2), rate of temperature fall is 12 DEG C/min.
The impurity-removing method of CNT of the present invention can achieve the purification to large batch of CNT, CNT
Purity can reach 99.9%.
Specific embodiment
The present invention is described in further detail below, with make those skilled in the art with reference to specification word being capable of evidence
To implement.
The present invention provides a kind of impurity-removing method of CNT, comprising:
CNT is first placed in nitrogen atmosphere step (1), is continually fed into carbon dioxide, and the flow velocity of carbon dioxide is
340～370m3/ h, the response time is 30～40min, and reaction temperature is 650～680 DEG C, is passed through nitrogen that CNT is entered
Row cooling, and control rate of temperature fall to be 30～40 DEG C/min, when cooling to 440 DEG C, then it is continually fed into nitrogen 10min, afterwards again
It is continually fed into hydrogen, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C, persistently leads to afterwards again
Enter nitrogen 20min, the temperature of nitrogen is maintained at 440 DEG C；
CNT is maintained in nitrogen atmosphere step (2), by being continually fed into nitrogen, CNT is dropped
Temperature, rate of temperature fall is 13～15 DEG C/min, until the temperature of CNT is reduced to room temperature.
The present invention passes through first to be continually fed into carbon dioxide, and the precise control flow velocity of carbon dioxide, response time and anti-
Answering temperature, thus eliminating contained impurity in CNT, especially can remove the impurity such as amorphous carbon.Through one
After the reaction of section time, then it is passed through the higher hydrogen of reproducibility, thus further being reacted to the impurity of more difficult reaction, this
Impurity both can be removed by sample as much as possible, can also reduce the consumption to hydrogen simultaneously, thus reducing the cost of production, makes this
The method of invention is more suitable for processing to large batch of CNT.The reaction temperature of hydrogen is than the reaction temperature of carbon dioxide
Degree is much lower, therefore, between two stages, first CNT is lowered the temperature, and controls rate of temperature fall, waits to cool to suitable
During the reaction temperature of suitable hydrogen, it is continually fed into nitrogen for a period of time, so that CNT is tended towards stability, thus being favorably improved hydrogen
The reaction efficiency of impurity.
Last in step (1), treat that hydrogen completes to the process of CNT, then be continually fed into nitrogen 20min, and this
When do not lower the temperature, and be to maintain the temperature of nitrogen under the reaction temperature of hydrogen, this is because, after the completion of hydrogen treat, impurity
With the portion of product of hydrogen still can adsorb on the carbon nanotubes, when with nitrogen above-mentioned condition persistently purge a period of time, nitrogen
Portion of product all can be taken away, thus ensureing the refining effect to CNT.
And, find through research, rate of temperature fall also has impact to the quality of CNT, therefore, the present invention also essence
Really control rate of temperature fall.
The purity of the CNT that the present invention finally gives can reach 99.9%.
Preferably, in the impurity-removing method of described CNT, in described step (1), the response time is 35min, instead
Temperature is answered to be 680 DEG C.
Preferably, in the impurity-removing method of described CNT, in described step (1), the flow velocity of carbon dioxide is
365m3/h.
Preferably, in the impurity-removing method of described CNT, in described step (2), rate of temperature fall is 12 DEG C/min.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment
With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily
Realize other modification, therefore under the general concept being limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details.
Claims (4)
1. a kind of impurity-removing method of CNT is it is characterised in that include:
CNT is first placed in nitrogen atmosphere step (1), is continually fed into carbon dioxide, and the flow velocity of carbon dioxide is 340～
370m3/ h, the response time is 30～40min, and reaction temperature is 650～680 DEG C, is passed through nitrogen that CNT is dropped
Temperature, and control rate of temperature fall to be 30～40 DEG C/min, when cooling to 440 DEG C, then it is continually fed into nitrogen 10min, continue afterwards again
It is passed through hydrogen, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C, is continually fed into nitrogen afterwards again
Gas 20min, the temperature of nitrogen is maintained at 440 DEG C；
CNT is maintained in nitrogen atmosphere step (2), by being continually fed into nitrogen, CNT is lowered the temperature, fall
Warm speed is 13～15 DEG C/min, until the temperature of CNT is reduced to room temperature.
2. the impurity-removing method of CNT as claimed in claim 1 is it is characterised in that in described step (1), and the response time is
35min, reaction temperature is 680 DEG C.
3. the impurity-removing method of CNT as claimed in claim 1 is it is characterised in that in described step (1), carbon dioxide
Flow velocity is 365m3/h.
4. the impurity-removing method of CNT as claimed in claim 1 is it is characterised in that in described step (2), rate of temperature fall is
12℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610705090.3A CN106365146A (en) | 2016-08-22 | 2016-08-22 | Impurity removal method of carbon nanotubes |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610705090.3A CN106365146A (en) | 2016-08-22 | 2016-08-22 | Impurity removal method of carbon nanotubes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
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|---|---|---|---|---|
| WO2002064868A1 (en) * | 2001-02-12 | 2002-08-22 | William Marsh Rice University | Gas-phase process for purifying single-wall carbon nanotubes and compositions thereof |
| CN101712469A (en) * | 2008-09-30 | 2010-05-26 | 韩华石油化学株式会社 | Continuous method and apparatus of purifying carbon nanotube |
| CN102020267A (en) * | 2010-12-30 | 2011-04-20 | 上海大学 | Purification method of single-wall carbon nano tube |
| CN103930603A (en) * | 2011-09-06 | 2014-07-16 | 西南纳米技术公司 | Single wall carbon nanotube purification process and improved single wall carbon nanotubes |
-
2016
- 2016-08-22 CN CN201610705090.3A patent/CN106365146A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002064868A1 (en) * | 2001-02-12 | 2002-08-22 | William Marsh Rice University | Gas-phase process for purifying single-wall carbon nanotubes and compositions thereof |
| CN101712469A (en) * | 2008-09-30 | 2010-05-26 | 韩华石油化学株式会社 | Continuous method and apparatus of purifying carbon nanotube |
| CN102020267A (en) * | 2010-12-30 | 2011-04-20 | 上海大学 | Purification method of single-wall carbon nano tube |
| CN103930603A (en) * | 2011-09-06 | 2014-07-16 | 西南纳米技术公司 | Single wall carbon nanotube purification process and improved single wall carbon nanotubes |
Non-Patent Citations (1)
| Title |
|---|
| 梁大明等: "《煤基炭材料》", 31 March 2011 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Effective date of registration: 20180629 Address after: 518000 Guangdong Shenzhen Longhua New District big wave street Longsheng community Tenglong road gold rush e-commerce incubation base exhibition hall E commercial block 706 Applicant after: Shenzhen step Technology Transfer Center Co., Ltd. Address before: 536000 the Guangxi Zhuang Autonomous Region Beihai Hepu County West Town Baisha village committee 15 village team 23 Applicant before: Lai Shiquan |
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Application publication date: 20170201 |