CN106185867A - The purity of CNT improves method - Google Patents
The purity of CNT improves method Download PDFInfo
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- CN106185867A CN106185867A CN201610704031.4A CN201610704031A CN106185867A CN 106185867 A CN106185867 A CN 106185867A CN 201610704031 A CN201610704031 A CN 201610704031A CN 106185867 A CN106185867 A CN 106185867A
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- nitrogen
- hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The purity that the invention discloses a kind of CNT improves method, including: CNT is first placed in nitrogen atmosphere by 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, it is passed through nitrogen CNT is lowered the temperature, and to control rate of temperature fall be 30～40 DEG C/min, when cooling to 440 DEG C, being continually fed into nitrogen 10min again, be continually fed into hydrogen the most again, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；Step (2) stops being passed through hydrogen, is maintained in nitrogen atmosphere by CNT, lowers the temperature CNT by being continually fed into nitrogen.The present invention can realize the purification to large batch of CNT, and the purity of CNT can reach 99.9%.
Description
Technical field
The purity that the present invention relates to a kind of CNT improves method.
Background technology
1991 the end of the year Japanese scholars Lijimat be found that the CNT being made up of carbon atom, owing to its structure is special, as
Typical one-dimensional nano structure, the body of hollow, it has high axial strength (about l00 times of steel) and the highest 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 character such as good, CNT shows many with the diverse property of other carbonaceous materials, therefore is applied to Novel electric
The fields 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 the CNT utilizing the method such as arc process and Floating catalyst method to prepare is frequently accompanied by quite counting
The impurity of amount, such as carbon nano-particle, amorphous carbon, Nano carbon balls and catalyst particle etc..The very big ground resistance of existence of these impurity
Having hindered the physical property research of CNT and actual application, therefore the purification to CNT is studied and is the most more and more weighed
Depending on.Purification route is come mainly by the minute differences of the aspects such as the reason of impurity, chemistry such as CNT and amorphous carbon at present
Reaching the purpose purified, 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 to be purified, and obtain is low-purity CNT.It would therefore be highly desirable to invention one is suitable
The purity closing high-volume CNT improves method.
Summary of the invention
The present invention has designed and developed the purity of the high CNT of a kind of purification efficiency and has improved method.
The technical scheme that the present invention provides is:
The purity of a kind of CNT improves method, including:
CNT is first placed in nitrogen atmosphere by 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 and enters CNT
Row cooling, and to control rate of temperature fall be 30～40 DEG C/min, when cooling to 440 DEG C, then is continually fed into nitrogen 10min, the most again
Being continually fed into hydrogen, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；
Step (2) stops being passed through hydrogen, is maintained in nitrogen atmosphere by CNT, comes carbon by being continually fed into nitrogen
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 purity raising method of described CNT, in described step (1), the response time is
35min, reaction temperature is 680 DEG C.
Preferably, in the purity raising method of described CNT, in described step (1), the flow velocity of carbon dioxide
For 365m3/h。
Preferably, in the purity raising method of described CNT, in described step (2), rate of temperature fall is 12 DEG C/
min。
The purity of CNT of the present invention improves method can realize the purification to large batch of CNT, and carbon is received
The purity of mitron can reach 99.9%.
Detailed description of the invention
The present invention is described in further detail below, with make those skilled in the art with reference to description word can evidence
To implement.
The present invention provides the purity of a kind of CNT to improve method, including:
CNT is first placed in nitrogen atmosphere by 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 and enters CNT
Row cooling, and to control rate of temperature fall be 30～40 DEG C/min, when cooling to 440 DEG C, then is continually fed into nitrogen 10min, the most again
Being continually fed into hydrogen, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；
Step (2) stops being passed through hydrogen, is maintained in nitrogen atmosphere by CNT, comes carbon by being continually fed into nitrogen
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 is by being first continually fed into carbon dioxide, and accurately controls the flow velocity of carbon dioxide, and the response time is with anti-
Answer temperature, thus eliminate impurity contained 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 hydrogen that reproducibility is higher, thus the impurity of more difficult reaction is reacted further, this
Impurity both can be removed by sample as much as possible, can also reduce the consumption to hydrogen simultaneously, thus reduce the cost of production, makes this
The method of invention is more suitable for processing large batch of CNT.The reaction temperature of hydrogen is than the reaction temperature of carbon dioxide
Spend much lower, therefore, between two stages, first CNT is lowered the temperature, and control rate of temperature fall, wait to cool to fit
During the reaction temperature of suitable hydrogen, it is continually fed into nitrogen a period of time, makes CNT tend towards stability, thus be favorably improved hydrogen
The reaction efficiency of impurity.
Further, find through research, also there is impact, therefore, the present invention also essence in rate of temperature fall to the quality of CNT
Really control rate of temperature fall.
The purity of the CNT that the present invention finally gives can reach 99.9%.
Preferably, in the purity raising method of described CNT, in described step (1), the response time is
35min, reaction temperature is 680 DEG C.
Preferably, in the purity raising method of described CNT, in described step (1), the flow velocity of carbon dioxide
For 365m3/h。
Preferably, in the purity raising method of described CNT, in described step (2), rate of temperature fall is 12 DEG C/
min。
Although embodiment of the present invention are disclosed as above, but it is not restricted in description and embodiment listed
Using, it can be applied to various applicable the field of the invention completely, for those skilled in the art, and can be easily
Realizing other amendment, therefore under the general concept limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details.
Claims (4)
1. the purity of a CNT improves method, it is characterised in that including:
CNT is first placed in nitrogen atmosphere by step (1), is continually fed into carbon dioxide, the flow velocity of carbon dioxide be 340～
370m3/ h, the response time is 30～40min, and reaction temperature is 650～680 DEG C, is passed through nitrogen and drops CNT
Temperature, and to control rate of temperature fall be 30～40 DEG C/min, when cooling to 440 DEG C, then is continually fed into nitrogen 10min, continues the most again
Being passed through hydrogen, the flow velocity of hydrogen is 200m3/ h, the response time is 10min, and reaction temperature is 440 DEG C；
Step (2) stops being passed through hydrogen, is maintained in nitrogen atmosphere by CNT, comes carbon nanometer by being continually fed into nitrogen
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 purity of CNT as claimed in claim 1 improves method, it is characterised in that in described step (1), during reaction
Between be 35min, reaction temperature is 680 DEG C.
3. the purity of CNT as claimed in claim 1 improves method, it is characterised in that in described step (1), titanium dioxide
The flow velocity of carbon is 365m3/h。
4. the purity of CNT as claimed in claim 1 improves method, it is characterised in that in described step (2), cooling speed
Rate is 12 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610704031.4A CN106185867A (en) | 2016-08-22 | 2016-08-22 | The purity of CNT improves method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610704031.4A CN106185867A (en) | 2016-08-22 | 2016-08-22 | The purity of CNT improves method |
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| CN201610704031.4A Pending CN106185867A (en) | 2016-08-22 | 2016-08-22 | The purity of CNT improves method |
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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 |
| CN103407984A (en) * | 2013-07-16 | 2013-11-27 | 清华大学 | Carbon nano-tube purification method based on weak oxidizing atmosphere oxidation assisted acid treatment |
| CN104310375A (en) * | 2014-10-09 | 2015-01-28 | 清华大学 | Method for removing carbon impurities in single-walled carbon nanotube |
| CN105060271A (en) * | 2015-07-30 | 2015-11-18 | 惠州集越纳米材料技术有限责任公司 | Carbon nano-tube purification method |
-
2016
- 2016-08-22 CN CN201610704031.4A patent/CN106185867A/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 |
| CN103407984A (en) * | 2013-07-16 | 2013-11-27 | 清华大学 | Carbon nano-tube purification method based on weak oxidizing atmosphere oxidation assisted acid treatment |
| CN104310375A (en) * | 2014-10-09 | 2015-01-28 | 清华大学 | Method for removing carbon impurities in single-walled carbon nanotube |
| CN105060271A (en) * | 2015-07-30 | 2015-11-18 | 惠州集越纳米材料技术有限责任公司 | Carbon nano-tube purification method |
Non-Patent Citations (1)
| Title |
|---|
| 梁大明等: "《煤基炭材料》", 31 December 2010, 化学工业出版社 * |
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Effective date of registration: 20180626 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: 20161207 |