CN106335895A - Method for improving purity of carbon nanotubes - Google Patents
Method for improving purity of carbon nanotubes Download PDFInfo
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- CN106335895A CN106335895A CN201610703552.8A CN201610703552A CN106335895A CN 106335895 A CN106335895 A CN 106335895A CN 201610703552 A CN201610703552 A CN 201610703552A CN 106335895 A CN106335895 A CN 106335895A
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- temperature
- carbon nanotubes
- purity
- carbon
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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 a method for improving purity of carbon nanotubes, and the method comprises the following steps: (1) putting the carbon nanotubes under a nitrogen atmosphere, continuously introducing carbon dioxide, wherein carbon dioxide flow rate is 340-370m<3>/h, reaction time is 30-40min, and reaction temperature is 650 to 680 DEG C, then continuously introducing hydrogen, wherein hydrogen flow rate is 200m<3>/h, reaction time is 10min, and reaction temperature is 440 DEG C; and (2) stopping the introducing of the hydrogen, keeping the carbon nanotubes in the nitrogen atmosphere, cooling the carbon nanotubes by constant introducing of the nitrogen until carbon nanotube temperature is reduced to room temperature, wherein cooling rate is 13 to 15 DEG C/min. The method for improving the purity of the carbon nanotubes can realize the purification of a large number of carbon nanotubes, and the purity of the carbon nanotubes can reach 99.9%.
Description
Technical field
The present invention relates to a kind of method improving carbon nano pipe purity.
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 method that high-volume improves carbon nano pipe purity.
Content of the invention
The method that the present invention has designed and developed a kind of high raising carbon nano pipe purity of purification efficiency.
The technical scheme that the present invention provides is:
A kind of method improving carbon nano pipe purity, 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 continually fed into hydrogen, hydrogen afterwards again
Flow velocity be 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；
Step (2) stops being passed through hydrogen, CNT is maintained in nitrogen atmosphere, by being continually fed into nitrogen come to carbon
Nanotube is lowered the temperature, and rate of temperature fall is 13～15 DEG C/min, until the temperature of CNT is reduced to room temperature.
Preferably, in the described method of raising carbon nano pipe purity, in described step (1), the response time is
35min, reaction temperature is 680 DEG C.
Preferably, in the described method of raising carbon nano pipe purity, in described step (1), the flow velocity of carbon dioxide
For 365m3/h.
Preferably, in the method for described raising carbon nano pipe purity, in described step (2), rate of temperature fall is 12 DEG C/
min.
The method improving carbon nano pipe purity of the present invention can achieve the purification to large batch of CNT, and carbon is received
The purity of mitron 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 method improving carbon nano pipe purity, 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 continually fed into hydrogen, hydrogen afterwards again
Flow velocity be 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；
Step (2) stops being passed through hydrogen, CNT is maintained in nitrogen atmosphere, by being continually fed into nitrogen come to carbon
Nanotube is lowered the temperature, and 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.
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 described method of raising carbon nano pipe purity, in described step (1), the response time is
35min, reaction temperature is 680 DEG C.
Preferably, in the described method of raising carbon nano pipe purity, in described step (1), the flow velocity of carbon dioxide
For 365m3/h.
Preferably, in the method for described raising carbon nano pipe purity, 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 method improving carbon nano pipe purity 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 continually fed into hydrogen, the stream of hydrogen afterwards again
Speed is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；
Step (2) stops being passed through hydrogen, CNT is maintained in nitrogen atmosphere, by being continually fed into nitrogen come to carbon nanometer
Pipe is lowered the temperature, and rate of temperature fall is 13～15 DEG C/min, until the temperature of CNT is reduced to room temperature.
2. the method improving carbon nano pipe purity as claimed in claim 1 is it is characterised in that in described step (1), during reaction
Between be 35min, reaction temperature be 680 DEG C.
3. the method improving carbon nano pipe purity as claimed in claim 1 is it is characterised in that in described step (1), titanium dioxide
The flow velocity of carbon is 365m3/h.
4. the method improving carbon nano pipe purity as claimed in claim 1 is it is characterised in that in described step (2), cooling is fast
Rate is 12 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610703552.8A CN106335895A (en) | 2016-08-22 | 2016-08-22 | Method for improving purity of carbon nanotubes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610703552.8A CN106335895A (en) | 2016-08-22 | 2016-08-22 | Method for improving purity of carbon nanotubes |
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| CN106335895A true CN106335895A (en) | 2017-01-18 |
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| CN201610703552.8A Pending CN106335895A (en) | 2016-08-22 | 2016-08-22 | Method for improving purity of carbon nanotubes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174117A (en) * | 2020-09-01 | 2021-01-05 | 深圳市德方纳米科技股份有限公司 | Method for purifying carbon nanotubes |
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 |
-
2016
- 2016-08-22 CN CN201610703552.8A patent/CN106335895A/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, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174117A (en) * | 2020-09-01 | 2021-01-05 | 深圳市德方纳米科技股份有限公司 | Method for purifying carbon nanotubes |
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Effective date of registration: 20180703 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: 20170118 |