CN106315560A - Carbon nanotube purification method - Google Patents
Carbon nanotube purification method Download PDFInfo
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- CN106315560A CN106315560A CN201610703554.7A CN201610703554A CN106315560A CN 106315560 A CN106315560 A CN 106315560A CN 201610703554 A CN201610703554 A CN 201610703554A CN 106315560 A CN106315560 A CN 106315560A
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- carbon dioxide
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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 invention discloses a carbon nanotube purification method. The method comprises the following steps: (1) putting carbon nanotubes in a nitrogen atmosphere, and continuously introducing carbon dioxide, wherein the flow rate of the carbon dioxide is 340-370 m<3>/h, the reaction time is 30-40 minutes, and the reaction temperature is 650-680 DEG C; and (2) stopping introducing the carbon dioxide, keeping the carbon nanotubes in the nitrogen atmosphere, and continuously introducing nitrogen to cool the carbon nanotubes until the temperature of the carbon nanotubes is reduced to room temperature, wherein the cooling rate is 13-15 DEG C/min. According to the invention, the carbon nanotube purification method can realize purification of a large batch of carbon nanotubes, and the purity of the carbon nanotubes can reach 99.9%.
Description
Technical field
The present invention relates to the method for purification of a kind of CNT.
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
Close the method for purification of high-volume CNT.
Summary of the invention
The present invention has designed and developed the method for purification of the high CNT of a kind of purification efficiency.
The technical scheme that the present invention provides is:
A kind of method of purification of CNT, 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；
Step (2) stops being passed through carbon dioxide, is maintained in nitrogen atmosphere by CNT, by being continually fed into nitrogen
Lowering the temperature CNT, rate of temperature fall is 13～15 DEG C/min, until the temperature of CNT is reduced to room temperature.
Preferably, in the method for purification of described CNT, in described step (1), the response time is 35min, instead
Answering temperature is 680 DEG C.
Preferably, in the method for purification of described CNT, in described step (1), the flow velocity of carbon dioxide is
365m3/h。
Preferably, in the method for purification of described CNT, in described step (2), rate of temperature fall is 12 DEG C/min.
The method of purification of CNT of the present invention can realize the purification to large batch of CNT, CNT
Purity 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 method for purification of a kind of CNT, 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；
Step (2) stops being passed through carbon dioxide, is maintained in nitrogen atmosphere by CNT, by being continually fed into nitrogen
Lowering the temperature CNT, 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 continually fed into carbon dioxide, and accurately controls the flow velocity of carbon dioxide, response time and reaction
Temperature, thus eliminate impurity contained in CNT, especially can remove the impurity such as amorphous carbon.
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 method for purification of described CNT, in described step (1), the response time is 35min, instead
Answering temperature is 680 DEG C.
Preferably, in the method for purification of described CNT, in described step (1), the flow velocity of carbon dioxide is
365m3/h。
Preferably, in the method for purification 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 method for purification of a CNT, 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；
Step (2) stops being passed through carbon dioxide, 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.
2. the method for purification of CNT as claimed in claim 1, it is characterised in that in described step (1), the response time is
35min, reaction temperature is 680 DEG C.
3. the method for purification of CNT as claimed in claim 1, it is characterised in that in described step (1), carbon dioxide
Flow velocity is 365m3/h。
4. the method for purification of CNT as claimed in claim 1, 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 |
|---|---|---|---|
| CN201610703554.7A CN106315560A (en) | 2016-08-22 | 2016-08-22 | Carbon nanotube purification method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610703554.7A CN106315560A (en) | 2016-08-22 | 2016-08-22 | Carbon nanotube purification method |
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| CN106315560A true CN106315560A (en) | 2017-01-11 |
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| CN201610703554.7A Pending CN106315560A (en) | 2016-08-22 | 2016-08-22 | Carbon nanotube purification method |
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Cited By (3)
| 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 |
| CN115536005A (en) * | 2022-10-31 | 2022-12-30 | 山东大展纳米材料有限公司 | Carbon nano tube purification method |
| CN115536005B (en) * | 2022-10-31 | 2024-04-19 | 山东大展纳米材料有限公司 | Carbon nano tube purification method |
Citations (5)
| 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 |
| CN102020267A (en) * | 2010-12-30 | 2011-04-20 | 上海大学 | Purification method of single-wall carbon nano tube |
| 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 |
| 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 |
| 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 CN201610703554.7A patent/CN106315560A/en active Pending
Patent Citations (5)
| 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 |
| 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 |
| 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 |
| 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 March 2011 * |
Cited By (3)
| 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 |
| CN115536005A (en) * | 2022-10-31 | 2022-12-30 | 山东大展纳米材料有限公司 | Carbon nano tube purification method |
| CN115536005B (en) * | 2022-10-31 | 2024-04-19 | 山东大展纳米材料有限公司 | Carbon nano tube purification method |
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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: 20170111 |
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