CN1475438A - Purification method of carbon nano pipe and its device - Google Patents
Purification method of carbon nano pipe and its device Download PDFInfo
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- CN1475438A CN1475438A CNA031501214A CN03150121A CN1475438A CN 1475438 A CN1475438 A CN 1475438A CN A031501214 A CNA031501214 A CN A031501214A CN 03150121 A CN03150121 A CN 03150121A CN 1475438 A CN1475438 A CN 1475438A
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- carbon nanotube
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- gas
- carbon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000000746 purification Methods 0.000 title claims description 18
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 30
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 30
- 230000001590 oxidative effect Effects 0.000 claims abstract description 16
- 239000011343 solid material Substances 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 230000009286 beneficial effect Effects 0.000 claims description 3
- 230000007812 deficiency Effects 0.000 claims description 3
- 238000005243 fluidization Methods 0.000 claims description 3
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910017116 Fe—Mo Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 230000004888 barrier function Effects 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 2
- 230000004931 aggregating effect Effects 0.000 abstract 1
- 229910003481 amorphous carbon Inorganic materials 0.000 abstract 1
- 239000002109 single walled nanotube Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 5
- 239000002048 multi walled nanotube Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 150000001721 carbon Chemical group 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- -1 electron device Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
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Abstract
An equipment for purifying the carbon nanotubes is a nano aggregating fluidized-bed reactor composed of gas distributor, fluidized bed, gas-solid separator, feeding inlet and discharging outlet. Its process features that the oxidizing gas and fluidized gas are introduced to said reactor from its bottom to make the solid material in fluidized state, and the raw carbon nanotubes are fluidized and selectively oxidized to remove the amorphous carbon and the carbon coated on the surface of catalyst.
Description
Technical field
The invention belongs to the nano material preparation technical field, particularly utilize the gas phase selective oxidation to remove the purification process and the device thereof of a kind of carbon nanotube of carbon elimination phase impurity.
Background technology
Carbon nanotube is a kind of tubular nanometer material of being made up of carbon atom.Tube wall contains the multilayer carbon atom and is called as multi-walled carbon nano-tubes (MWNT), contains the monolayer carbon atom and is called as Single Walled Carbon Nanotube (SWNT).Carbon nanotube has been paid close attention to by the investigator with its particular structure and excellent performance since being found always, has potential application foreground at aspects such as novel conductive/high-strength composite material, electron device, catalyst support materials.Than MWNT, the structure of SWNT is perfect more, and performance is excellent more, so the preparation of SWNT and utilisation technology become the focus that the investigator pays close attention to.The synthetic method of Single Walled Carbon Nanotube mainly contains arc process, laser evaporation method and catalystic pyrolysis at present.In the Single Walled Carbon Nanotube product that aforesaid method makes usually with decolorizing carbon and include the greying carbon-coating of nano-metal particle.The existence of these impurity has greatly hindered the research of carbon nanotube and application.
Report in " K.Hernadi; A.Siska; L.Thi ê n-Nga, L Forr ó, I.Kiricsi; Reactivityof different kinds of carbon during oxidative purification ofcatalytically prepared carbon nanotubes; Solid State Ionics, 2001,141-142:203-209 ", utilize the minute differences of different carbon phase chemistry stability, can remove decolorizing carbon impurity by the method for selective chemical oxidation.Our experiment shows, under the katalysis of metal, it is oxidized prior to Single Walled Carbon Nanotube to overlay on the outer greying carbon-coating of metal catalyst particles, therefore, can remove carbon phase impurity in the product by strict controlled oxidation reaction conditions, remove catalyzer through pickling again and can obtain high-purity Single Walled Carbon Nanotube.
Because the reactivity worth difference of various form carbon phases (as: decolorizing carbon, nano carbon particle, graphite scrap, Single Walled Carbon Nanotube and multi-walled carbon nano-tubes) is little, so the control of the condition of oxidising process is extremely important.Dysoxidation causes purification effect poor; Hyperoxidation then can cause carbon nanotube destroyed, and product yield is low.Prior art adopts the method for fixed bed roasting usually.Because the oxidising process heat release, the heat of generation then can cause local peroxidation as can not in time shifting out, so material bed in the fixed bed can not be too thick, seriously limited treatment capacity.At " Jeong-Mi Moon; Kay Hyeok An; Young Hee Lee; et al.; High-yieldpurification process of singlewalled carbon nanotubes; J.Phys.Chem.B, 2001,105:5677-5681 " middle report; people such as Jeong-Mi Moon are positioned over sample in the one horizontal silica tube, and constantly the rotation silica tube causes the solid materials upset in oxidising process, thereby heat transfer is strengthened; but this method needs continuous rotational response device, so the energy consumption height.
Summary of the invention
The purification process and the device thereof that the purpose of this invention is to provide a kind of carbon nanotube, it is characterized in that: the purification devices of described carbon nanotube is the poly-bolus flow fluidized bed reactor of nanometer, be that the outside that gas distributor 1, heating/cooling device cover 2 is enclosed within reactor beds body 4 is housed in the bottom of reactor beds body 4, gas-solid separator 5 is installed in reactor beds body 4 tops, and charging bole 6 and discharge opening 7 are contained in the upper and lower side of reactor beds body 4 respectively.
The purification process of described carbon nanotube is to utilize from the oxidizing gas of the poly-bolus flow fluidized bed reactor of nanometer bottom feeding and the surging force of fluidizing agent, stir the solid materials 3 in the reactor, make its abundant fluidisation and selective oxidation reaction takes place, decolorizing carbon in the carbon nanotube crude product and the carbon-coating that is coated on the granules of catalyst surface are removed; Its purge process is: will contain charging bole 6 addings of the carbon nanotube crude product solid materials 3 of band carried catalyst and carbon phase impurity from reactor top, oxidizing gas feeds continuously from fluidized-bed reactor bed body 4 bottoms, through behind the gas distributor 1, the thick product of carbon nanotube is fluidized and selective oxidation reaction takes place simultaneously, residual gas and gaseous product are discharged from fluidized-bed reactor bed body 4 tops through gas-solid separator 5; When the oxidizing gas consumption is little, deficiency is so that during solid matter streams, topping up such as nitrogen are as fluidizing agent.Reacted solid materials 3 draws off from the discharge opening 7 of fluidized-bed reactor bottom.
Described band carried catalyst is: Fe/MgO, Fe/Al
2O
3, Fe/SiO
2, Fe-Mo/MgO, Ni/MgO, it also has thermal barrier except that having katalysis in reaction process effect is beneficial to and keeps uniform temperature field in the reactor; Can utilize corresponding acid solution to remove catalyzer after the reaction, obtain high pure nano-carbon tube.
Described oxidizing gas is: oxygen, air, CO
2, H
2O steam.
Beneficial effect of the present invention: 1. this device promptly can be realized periodical operation, also can realize operate continuously.Periodical operation can guarantee the reaction times of homogeneous, and purification effect is good, but its processing power is strong not as good as operate continuously.2. oxidizing gas and fluidizing agent feed from reactor bottom simultaneously, and solid materials form with coacervate in reaction process is in fluidized state, and it is fully reacted, and decolorizing carbon in the carbon nanotube crude product and the carbon-coating that is coated on catalyst surface are removed.3. be not only applicable to Single Walled Carbon Nanotube and be applicable to purifying double-walled carbon nano-tube or multi-walled carbon nano-tubes yet.4. because fluidized-bed reactor heat transfer/mass transfer coefficient height, so be easy to keep uniform temperature field and concentration field in the reactor, very strong to purge process, fluidized-bed reactor also has advantages such as treatment capacity is big, material handling makes things convenient for simultaneously.
Description of drawings:
Fig. 1 is the poly-bolus flow fluidized bed reactor structural representation of nanometer.
Embodiment
The present invention is a kind of purification process and device thereof of carbon nanotube.The structure of its purification devices nanometer is as shown in Figure 1 gathered bolus flow fluidized bed reactor structural representation.Be that the outside that gas distributor 1, heating/cooling device cover 2 is enclosed within reactor beds body 4 is housed in the bottom of reactor beds body 4, gas-solid separator 5 is installed in reactor beds body 4 tops, and charging bole 6 and discharge opening 7 are contained in the upper and lower side of reactor beds body 4 respectively.
The purification process of above-mentioned carbon nanotube is to utilize from the oxidizing gas of the poly-bolus flow fluidized bed reactor of nanometer bottom feeding and the surging force of fluidizing agent, stir the solid materials 3 in the reactor, make its abundant fluidisation and selective oxidation reaction takes place, decolorizing carbon in the carbon nanotube crude product and the carbon-coating that is coated on catalyst surface are removed; Its purge process is: will contain charging bole 6 addings of the carbon nanotube crude product solid materials 3 of band carried catalyst and carbon phase impurity from reactor top, oxidizing gas feeds continuously from fluidized-bed reactor bed body 4 bottoms, through behind the gas distributor 1, make solid materials 3 be in fluidized state.The temperature of solid materials is by heating/cooling device 2 control in bed body and the bed, under specific temperature (350～800 ℃), the thick product of carbon nanotube is fluidized and selective oxidation reaction takes place simultaneously.Residual gas and gaseous product are discharged from fluidized-bed reactor 4 tops through gas-solid separator 5.When the oxidizing gas consumption is little, deficiency is so that during solid matter streams, topping up such as nitrogen are as fluidizing agent.Reacted solid materials 3 draws off from the discharge opening 7 of fluidized-bed reactor bottom.This device has two kinds of operating method:
In andnon-continuous operation manner, solid materials is from 6 disposable the packing into of charging bole on reactor top, feed fluidizing agent and be preheated to temperature of reaction, then switch the gas mixture that feeds oxidizing gas and fluidizing agent, after under preset temperature, reacting for some time (0.5～5 hour), stop to feed oxidizing gas, treat to stop to feed fluidizing agent after the material cooling, from the discharge opening 7 disposable solid materialss that draw off of fluidized-bed reactor bottom.
In the operate continuously mode, solid materials adds continuously from the charging bole 6 on reactor top, simultaneously from the discharge opening 7 continuous extraction part solid materialss of reactor lower part.The turnover inventory keeps balance, and it is constant to keep the fluidized-bed layer height.Reaction times is regulated by discharging speed.
Claims (4)
1. the purification devices of a carbon nanotube, it is characterized in that: the purification devices of described carbon nanotube is the poly-bolus flow fluidized bed reactor of nanometer, be that the outside that gas distributor (1), heating/cooling device cover (2) are enclosed within reactor beds body (4) is housed in the bottom of reactor beds body (4), gas-solid separator (5) is installed in reactor beds body (4) top, and charging bole (6) and discharge opening (7) are contained in the upper and lower side of reactor beds body (4) respectively.
2. the purification process of a carbon nanotube, it is characterized in that: the purification process of described carbon nanotube is to utilize from the oxidizing gas of the poly-bolus flow fluidized bed reactor of nanometer bottom feeding and the surging force of fluidizing agent, stir the solid materials (3) in the reactor, make its fluidisation and selective oxidation reaction takes place, decolorizing carbon in the carbon nanotube crude product and the carbon-coating that is coated on catalyst surface are removed; Its purge process is: will contain charging bole (6) adding of the carbon nanotube crude product solid materials (3) of band carried catalyst and carbon phase impurity from reactor top, oxidizing gas feeds continuously from fluidized-bed reactor bed body (4) bottom, behind gas distributor (1), the thick product of carbon nanotube is fluidized and selective oxidation reaction takes place simultaneously, residual gas and gaseous product are discharged from fluidized-bed reactor bed body (4) top through gas-solid separator (5); When the oxidizing gas consumption is little, deficiency is so that during solid matter streams, topping up such as nitrogen are as fluidized gas, and reacted solid materials (3) draws off from the discharge opening (7) of fluidized-bed reactor bottom.
3. according to the purification process of the described carbon nanotube of claim 2, it is characterized in that: the catalyzer of described band carrier is: Fe/MgO, Fe/Al
2O
3, Fe/SiO
2, Fe-Mo/MgO, Ni/MgO, it has catalysis and thermal barrier effect concurrently in reaction process, be beneficial to keep uniform temperature field in the reactor; Can utilize corresponding acid solution to remove catalyzer after the reaction, obtain high pure nano-carbon tube.
4. according to the purification process of the described carbon nanotube of claim 2, it is characterized in that: described oxidizing gas is: oxygen, air, CO
2, H
2O steam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03150121 CN1207187C (en) | 2003-07-18 | 2003-07-18 | Purification method of carbon nano pipe and its device |
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|---|---|---|---|
| CN 03150121 CN1207187C (en) | 2003-07-18 | 2003-07-18 | Purification method of carbon nano pipe and its device |
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|---|---|
| CN1475438A true CN1475438A (en) | 2004-02-18 |
| CN1207187C CN1207187C (en) | 2005-06-22 |
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|---|---|---|---|
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312033C (en) * | 2005-07-01 | 2007-04-25 | 清华大学 | Method for large-batch preparing overlength carbon nano pipe array and its apparatus |
| CN100430128C (en) * | 2006-10-13 | 2008-11-05 | 华东理工大学 | Electrochemical in-situ purifying process of carbon base nanometer electrocatalyst material |
| CN102267693A (en) * | 2011-07-06 | 2011-12-07 | 天津理工大学 | Low-temperature preparation method of carbon nanotube |
| CN101432228B (en) * | 2004-10-01 | 2012-03-28 | 英特尔公司 | Application of static light to a fluid flow of cnts for purposes of sorting the cnts |
| FR2972942A1 (en) * | 2011-03-21 | 2012-09-28 | Arkema France | PROCESS FOR MANUFACTURING CARBON NANOTUBES AND APPARATUS FOR CARRYING OUT THE PROCESS |
| CN101618868B (en) * | 2008-07-03 | 2013-03-13 | 中国科学院成都有机化学有限公司 | Method for removing amorphous carbon in 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 |
| 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 |
| EP2753734A4 (en) * | 2011-09-06 | 2015-10-14 | Southwest Nanotechnologies Inc | Single wall carbon nanotube purification process and improved single wall carbon nanotubes |
| CN105731417A (en) * | 2014-12-11 | 2016-07-06 | 山东大展纳米材料有限公司 | Apparatus and method for purifying carbon nanotubes |
| CN106185870A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | The Carbon nanotube purification system of reuse heat energy |
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2003
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| CN101432228B (en) * | 2004-10-01 | 2012-03-28 | 英特尔公司 | Application of static light to a fluid flow of cnts for purposes of sorting the cnts |
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| CN100430128C (en) * | 2006-10-13 | 2008-11-05 | 华东理工大学 | Electrochemical in-situ purifying process of carbon base nanometer electrocatalyst material |
| CN101618868B (en) * | 2008-07-03 | 2013-03-13 | 中国科学院成都有机化学有限公司 | Method for removing amorphous carbon in carbon nanotubes |
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| 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 |
| 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 |
| CN105731417A (en) * | 2014-12-11 | 2016-07-06 | 山东大展纳米材料有限公司 | Apparatus and method for purifying carbon nanotubes |
| WO2017069393A1 (en) * | 2015-10-23 | 2017-04-27 | 주식회사 엘지화학 | Cnt purification method using fluidized bed reactor |
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| CN107986267A (en) * | 2017-11-14 | 2018-05-04 | 中国电子科技集团公司第三十三研究所 | The method and its heating furnace that a kind of redox graphene powder upgrading is modified |
| CN110697684A (en) * | 2018-07-10 | 2020-01-17 | 中国科学院金属研究所 | Method for preparing coated carbon nano tube conductive microspheres by dry method and application thereof |
| CN110697684B (en) * | 2018-07-10 | 2022-05-31 | 中国科学院金属研究所 | Method for preparing coated carbon nano tube conductive microspheres by dry method and application thereof |
| CN110228804A (en) * | 2019-07-19 | 2019-09-13 | 陕西延长石油（集团）有限责任公司 | A kind of carbon nanotube sulphur modification and purification integral method |
| CN114883117A (en) * | 2021-05-17 | 2022-08-09 | 安徽科技学院 | Preparation method of composite carbon nano tube |
| CN114883117B (en) * | 2021-05-17 | 2023-04-21 | 安徽科技学院 | Preparation method of composite carbon nano tube |
| CN114804077A (en) * | 2022-05-18 | 2022-07-29 | 焦作集越纳米材料技术有限公司 | Method and device for purifying carbon nano tube |
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| Publication number | Publication date |
|---|---|
| CN1207187C (en) | 2005-06-22 |
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