CN109502572A - Carbon nanotube method of purification - Google Patents
Carbon nanotube method of purification Download PDFInfo
- Publication number
- CN109502572A CN109502572A CN201811633818.1A CN201811633818A CN109502572A CN 109502572 A CN109502572 A CN 109502572A CN 201811633818 A CN201811633818 A CN 201811633818A CN 109502572 A CN109502572 A CN 109502572A
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- China
- Prior art keywords
- carbon nanotube
- heating element
- nano tube
- purification
- carbon nano
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/17—Purification
-
- 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
A kind of carbon nanotube method of purification in material purification technique field, comprising: heating element is made in carbon nanotube to be purified and is connected in impulse circuit；Heating element is placed in electrified regulation and logical chlorine under vacuum condition, until carbon nano tube surface metal, metal oxide and chlorine reaction gasification generate high-purity carbon nano tube in heating element；It is passed through mixed gas to the high-purity carbon nano tube that inert gas excludes including metal chloride gas to be under inert gas shielding state, cooling high-purity carbon nano tube completes carbon nanotube purification.The present invention can be improved carbon nanotube purification efficiency, reduce energy consumption and pollution.
Description
Technical field
The present invention relates to a kind of technology in material purification field, specifically a kind of carbon nanotube method of purification.
Background technique
In carbon nanotube synthesis process, metallic catalysts and magnesia, aluminium oxide, the silica such as iron, cobalt, nickel are used
Etc. catalyst carriers.Traditional method of purification, such as high temperature graphitization method and acid wash difficulty is big, at high cost, low efficiency, it is difficult to reach
The purpose of quick high purity carbon nanotube.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, proposes a kind of carbon nanotube method of purification, can be improved
Carbon nanotube purification efficiency reduces energy consumption and pollution.
The present invention is achieved by the following technical solutions:
The present invention includes:
Heating element is made in carbon nanotube to be purified to be connected in impulse circuit；
Heating element is placed in electrified regulation and logical chlorine under vacuum condition, until carbon nano tube surface gold in heating element
Belong to, metal oxide and chlorine reaction gasification generate high-purity carbon nano tube；
It is passed through mixed gas of the inert gas exclusion including metal chloride gas, cools down high-purity carbon nano tube,
Complete carbon nanotube purification.
Metals content impurity is less than 20ppm in the high-purity carbon nano tube.
Described to heat using Current Heating mode, pulse current magnitude 10mA-100A, the current impulse time is
0.1-10s。
The temperature of carbon nanotube is 500-1500 DEG C in the heating process.
The heating element is by the way that carbon nanotube to be purified to be compacted obtain, the heating element and a pair of of high temperature resistant electrode
Connection.
Technical effect
Compared with prior art, the present invention utilizes the good capacity of heat transmission of carbon nanotube and chemical stability, utilizes arteries and veins
Rush electric current directly generates carbon nanotube electrified regulation, carbon nanotube heat (Q=I after being powered2It Rt) can be efficient to itself
Heat the intervention without ambient heat or heat-conducting medium；By adjusting the time of pulse current to chlorine and carbon nano tube surface
Metal, metal oxide react the purity requirement for reaching carbon nanotube completely, and the carbon nano pipe purity of preparation is high, and metal is miscellaneous
Matter content is less than 20ppm；Operation of the present invention is simple, and purifying velocity is fast, can scale application, economical and efficient and environmental protection.
Detailed description of the invention
Fig. 1 is purifying plant structural schematic diagram in embodiment 1；
Fig. 2 is the SEM photograph that embodiment 1 purifies obtained crystal whisker-shaped multi-walled carbon nanotube；
Fig. 3 is the SEM photograph that embodiment 2 purifies obtained bobbles shape multi-walled carbon nanotube；
In figure: quartz container 1, heating element 2, the pulse power 3, graphite electrode 4, vacuum evacuation device 5, optics temperature measurer 6.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention will be described in detail.
As shown in Figure 1, the present embodiments relate to a kind of carbon nanotube purifying plants, comprising:
Quartz container 1 places the heating element 2 that carbon nanotube to be handled is pressed into；Quartz container be equipped with air inlet and
Gas outlet；
The pulse power 3, power supply positive and negative electrode are connected separately with a graphite electrode 4；Two graphite electrodes 4 are arranged in quartz container 1
In be connected with heating element 2；
Vacuum evacuation device 5 is connected with the gas outlet of quartz container 1, vacuumizes to quartz container 1.
The quartz container is equipped with temperature-measuring port, and the temperature-measuring port is equipped with optics temperature measurer 6, for monitoring the temperature of carbon nanotube
Degree.
Embodiment 1
The present embodiment is used for the purification of crystal whisker-shaped multi-walled carbon nanotube, specific operation process to be as follows:
S1, 500g crystal whisker-shaped multi-walled carbon nanotube is pressed into heating element；
S2, the heating element after compacting is put into quartz container, is connect with two graphite electrodes；
S3, vacuumize, logical argon gas, repetitive operation 3 times, thoroughly exclude air；It vacuumizes again, makes the vacuum degree of quartz container
It is maintained at 9.0 × 10-8mbar；
S4, using pulse Electric heating, it is passed through electric current 1A, current impulse generates Joule heat by graphite electrode in 1s
It impacts, the temperature of carbon nanotube is sharply increased to 500 DEG C in heating element, chlorine is passed through at this time, by the iron of carbon nano tube surface
Simple substance and iron oxide are oxidized to ferric trichloride, ferric trichloride (315 DEG C of boiling point) gasification；
S5, then lead to nitrogen and chlorine, ferric trichloride and oxygen are discharged, make in quartz container in inert gas shielding atmosphere
In, cooling obtains metals content impurity and is less than the high-purity carbon nanotube of 20ppm, purity greater than 99.9%, and scanning electron microscope (SEM) photograph is as schemed
Shown in 2.
Embodiment 2
The present embodiment is used for the purification of bobbles shape multi-walled carbon nanotube, specific operation process to be as follows:
S1, 500g bobbles shape multi-walled carbon nanotube is pressed into heating element；
S2, the heating element after compacting is put into quartz container, is connect with two graphite electrodes；
S3, vacuumize, logical argon gas, repetitive operation 3 times, thoroughly exclude air；It vacuumizes again, makes the vacuum degree of quartz container
It is maintained at 9.0 × 10-8mbar；
S4, using pulse Electric heating, it is passed through electric current 2A, current impulse generates Joule heat by graphite electrode in 1s
It impacts, the temperature of carbon nanotube is sharply increased to 1500 DEG C in heating element, chlorine is passed through at this time, by the iron of carbon nano tube surface
Simple substance, nickel simple substance, ferroso-ferric oxide, nickel oxide, aluminium oxide, magnesia are oxidized into ferric trichloride, tri-chlorination nickel, tri-chlorination
Aluminium, magnesium dichloride；
S5, then lead to nitrogen and chlorine, oxygen and the metal chloride of gasification are discharged, make in quartz container in inert gas
In protective atmosphere, cooling obtains metals content impurity and is less than the high-purity carbon nanotube of 20ppm, purity greater than 99.9%, scanning electricity
Mirror figure is as shown in Figure 3.
It is emphasized that: the above is only presently preferred embodiments of the present invention, not make in any form to the present invention
Limitation, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention,
All of which are still within the scope of the technical scheme of the invention.
Claims (5)
1. a kind of carbon nanotube method of purification characterized by comprising
Heating element is made in carbon nanotube to be purified to be connected in impulse circuit；
Heating element is placed in electrified regulation and logical chlorine under vacuum condition, until carbon nano tube surface metal, gold in heating element
Belong to oxide and chlorine reaction gasification generates high-purity carbon nano tube；
It is passed through mixed gas to the high-purity carbon nano tube that inert gas excludes including metal chloride gas and is in inertia
Under gas protection status, cooling high-purity carbon nano tube completes carbon nanotube purification.
2. carbon nanotube method of purification according to claim 1, characterized in that metal impurities in the high-purity carbon nano tube
Content is less than 20ppm.
3. carbon nanotube method of purification according to claim 1, characterized in that the heating uses Current Heating side
Formula, pulse current magnitude 10mA-100A, current impulse time are 0.1-10s.
4. carbon nanotube method of purification according to claim 3, characterized in that the temperature of carbon nanotube in the heating process
It is 500-1500 DEG C.
5. carbon nanotube method of purification according to claim 1, characterized in that the heating element is by receiving carbon to be purified
Mitron is compacted obtain, and the heating element is connect with a pair of of high temperature resistant electrode.
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| CN201811633818.1A CN109502572A (en) | 2018-12-29 | 2018-12-29 | Carbon nanotube method of purification |
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| CN201811633818.1A CN109502572A (en) | 2018-12-29 | 2018-12-29 | Carbon nanotube method of purification |
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| CN201811633818.1A Pending CN109502572A (en) | 2018-12-29 | 2018-12-29 | Carbon nanotube method of purification |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
| CN110643846A (en) * | 2019-11-07 | 2020-01-03 | 苏州第一元素纳米技术有限公司 | Preparation method of carbon nano tube reinforced magnesium alloy |
| CN112028056A (en) * | 2020-08-27 | 2020-12-04 | 青岛昊鑫新能源科技有限公司 | Method for efficiently purifying carbon nanotubes by microwave heating |
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| CN1094695A (en) * | 1994-05-13 | 1994-11-09 | 中国矿业大学北京研究生部 | High-temp chlorination refining process for natural graphite |
| CN104192823A (en) * | 2014-08-08 | 2014-12-10 | 无锡东恒新能源科技有限公司 | Vapor purification method of carbon nanotubes |
| CN104401963A (en) * | 2014-10-27 | 2015-03-11 | 山东诚合新材料有限公司 | Carbon nanotube purification method capable of removing residual metals |
| WO2018178929A2 (en) * | 2017-03-31 | 2018-10-04 | HYDRO-QUéBEC | Method for the purification of raw carbon nanotubes |
| CN208297264U (en) * | 2018-05-04 | 2018-12-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | The mechanical property testing system of carbon nano-tube fibre at high operating temperatures |
-
2018
- 2018-12-29 CN CN201811633818.1A patent/CN109502572A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094695A (en) * | 1994-05-13 | 1994-11-09 | 中国矿业大学北京研究生部 | High-temp chlorination refining process for natural graphite |
| CN104192823A (en) * | 2014-08-08 | 2014-12-10 | 无锡东恒新能源科技有限公司 | Vapor purification method of carbon nanotubes |
| CN104401963A (en) * | 2014-10-27 | 2015-03-11 | 山东诚合新材料有限公司 | Carbon nanotube purification method capable of removing residual metals |
| WO2018178929A2 (en) * | 2017-03-31 | 2018-10-04 | HYDRO-QUéBEC | Method for the purification of raw carbon nanotubes |
| CN208297264U (en) * | 2018-05-04 | 2018-12-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | The mechanical property testing system of carbon nano-tube fibre at high operating temperatures |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
| CN110643846A (en) * | 2019-11-07 | 2020-01-03 | 苏州第一元素纳米技术有限公司 | Preparation method of carbon nano tube reinforced magnesium alloy |
| CN112028056A (en) * | 2020-08-27 | 2020-12-04 | 青岛昊鑫新能源科技有限公司 | Method for efficiently purifying carbon nanotubes by microwave heating |
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Address after: Room 105 and 207, 101 Building, Northwest Namie City, 99 Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province, 215000 Applicant after: SUZHOU FIRST ELEMENT NANO TECHNOLOGY CO.,LTD. Address before: Room 105 and 207, 101 Building, Northwest District of Suzhou Namie City, No. 99 Jinjihu Avenue, Wuzhong District Industrial Park, Suzhou City, Jiangsu Province, 215000 Applicant before: SUZHOU FIRST ELEMENT NANO TECHNOLOGY CO.,LTD. |
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Application publication date: 20190322 |