CN103407984A - Carbon nano-tube purification method based on weak oxidizing atmosphere oxidation assisted acid treatment - Google Patents
Carbon nano-tube purification method based on weak oxidizing atmosphere oxidation assisted acid treatment Download PDFInfo
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Abstract
The present invention belongs to the technical field of carbon nano-tube purification treatment processes, and particularly relates to a carbon nano-tube purification method based on a weak oxidizing atmosphere oxidation assisted acid treatment. According to the method, carbon dioxide, water vapor and other weak oxidants are adopted to oxidize a carbon nano-tube sample, and then an acid washing treatment is adopted to remove a carbon-coated iron structure in the carbon nano-tube. Compared with the conventional purification method, the purification method of the present invention has the following characteristics that: the weak oxidizing atmosphere is adopted to treat the carbon nano-tube sample to destroy the outer layer graphite of the impurity carbon-coated iron structure so as to overcome the difficult problem of difficult removal of iron particles coated in the graphite layer, such that the carbon nano-tube can be protected from loss, and the carbon-coated iron impurity in the carbon nano-tube can be removed through weak oxidation so as to improve purity and quality.
Description
Technical field
The invention belongs to the treatment process technical field of Purification of Carbon Nanotubes, particularly a kind of based on the auxiliary acid-treated purification method of carbon nanometer pipe of weak oxide ambient oxidation.
Background technology
Carbon nanotube, as a kind of advanced function material, because its excellent electricity, mechanical property reach application prospect widely, is the study hotspot in nanometer field always.Yet no matter be carbon nanotube prepared by arc discharge method or chemical Vapor deposition process, in product, all more or less comprise decolorizing carbon, granules of catalyst etc. impurity.Especially in the carbon nanotube that prepared by chemical Vapor deposition process, often contain a large amount of carbon iron clad structures, this structure is coated fully by the graphite flake layer of high stability, be difficult to remove iron contamination wherein with conventional treatment method, and this quality and the performance that can greatly affect prepared carbon nanotube product are expressed.Therefore, the purifying of carbon nanotube is the important step that promotes product purity and quality.
At present developed and applied comparatively general Purifying of Carbon Nanotubes and comprised: centrifugal separation (Bandow S, et al.Applied Physics A-Materials Science& Processing, 1998,67:23), Purified in electrophoresis method (Doorn S K, et al.Journal of the American Chemical Society, 2002,124:3169), acid solution/vapour phase oxidation process (Dujardin, E.et al.Advanced Materials1998,10 (8), 611; Haiqin, R et al.Curr.Appl.Phys.2010,10 (4), 1231-1235), chemical modification method, filtration and chromatographic technique, microwave heating method (P.X.Hou, C.Liu, H.M.Cheng, Carbon2008,46,2003; T.J.Park, S.Banerjee, T.Hemraj-Benny, S.S.Wong, J.Mater.Chem.2006,16,141; A.R.Harutyunyan, B.K.Pradhan, J.P.Chang, G.G.Chen, P.C.Eklund, J.Phys.Chem.B2002,106,8671) etc.In above-mentioned these purification techniques, what process the general use of large batch of carbon nanotube is acid solution oxidation style (hydrochloric acid, sulfuric acid, nitric acid etc.) and vapour phase oxidation process (oxygen, air etc.).But the drawback of these method for oxidation is all may introduce the functional group of oxidisability and the structure of carbon nanotube is caused to comparatively serious damage.Therefore, the very corn of a subject is: develop a kind of simplely, optionally the graphite linings of carbonoxide iron clad structure is beneficial to the wherein removal of iron granule foreign, reduces simultaneously the purification process of carbon nanotube loss of yield and structure deteriorate as far as possible.
Summary of the invention
For the prior art deficiency, the invention provides a kind of based on the auxiliary acid-treated purification method of carbon nanometer pipe of weak oxide ambient oxidation, by destroying the outer graphite of carbon impurity iron clad structure, and then remove the iron particle wherein be wrapped by, improve purity and the quality of carbon nanotube.
A kind of based on the auxiliary acid-treated purification method of carbon nanometer pipe of weak oxide ambient oxidation, its concrete steps are as follows:
(1) adopt chemical vapor deposition for carbon nanotubes, growth is completed to carbon nanotube not purified or process acid-alkali treatment preliminary purification and be placed in reactor; At first to reactor, continue to pass into inertia protection gas, reactor heating is until reaction zone temperature rises to 500～1400 ° of C, after temperature-stable, pass into weak oxidant, be used to destroying the outer graphite of carbon iron clad structure, remove thereby the iron be wrapped by particle is flowed out more easily;
(2) by acid treatment, wash away the iron particle of outflow, improve purity and the quality of sample;
(3) detect the purity of the carbon nanotube sample that obtains, if reach required standard, purifying completes; If do not reach required standard, repeating step (1) and step (2), until purity reaches required standard.
Described inertia protection gas is argon gas, helium or nitrogen.
Described weak oxidant is one or more in carbonic acid gas, water vapour, oxygen and chlorine.
Described while passing into one or more in carbonic acid gas, water vapour, oxygen and chlorine, this part weak oxidant gas accounts for and passes into 1%～50% of gas reactor cumulative volume, and rest part is still inert protective gas.
Acid treatment method in described step (2) be that the sample that will process through weak oxide immerses in excessive hydrochloric acid, nitric acid or sulphuric acid soln, and by the solution stirring heating, temperature maintains 50～100 ° of C, time length 6～12h; With centrifugal or filter type, carry out liquid-solid separation afterwards, and the solid sample drying-granulating that will obtain.
Beneficial effect of the present invention is:
The present invention adopts carbonic acid gas cheap and easy to get, water vapour etc. to process carbon nanotube prepared by chemical Vapor deposition process, has realized the removal to the carbon impurity iron clad structure in carbon nanotube.Solved the problem that the iron particle that is wrapped by the prior art is difficult for removing, can reduce cost-effectively the iron level in carbon nanotube, improved its purity and quality, thereby offered help for the preparation in macroscopic quantity of high quality carbon nanotube.
The accompanying drawing explanation
Fig. 1 is the schematic diagram of the auxiliary acid-treated purification method of carbon nanometer pipe of weak oxide ambient oxidation of the present invention;
Fig. 2 is the process flow sheet of the auxiliary acid-treated purification method of carbon nanometer pipe of weak oxide ambient oxidation of the present invention;
Fig. 3 is the high-resolution-ration transmission electric-lens photo (TEM) of (b) sample after (a) and roasting before the carbonic acid gas roasting in the embodiment of the present invention 1;
The transmission electron microscope photo (TEM) of (b) sample after (a) and purifying before carbon dioxide purification in Fig. 4 embodiment of the present invention 2.
Embodiment
The invention provides a kind ofly based on the auxiliary acid-treated purification method of carbon nanometer pipe of weak oxide ambient oxidation, the present invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1
Carbon dioxide atmosphere oxidation Single Walled Carbon Nanotube in thermogravimetric analyzer:
To take the LDH(laminated dihydroxy composite metal hydroxide of Fe-Mg-Al component) system is catalyst precursor, Single Walled Carbon Nanotube prepared by chemical Vapor deposition process (having passed through the preliminary purifications such as acid-alkali treatment) is placed in crucible, and crucible is put into to thermogravimetric analyzer.Under carbonic acid gas-argon gas mixed atmosphere (volume ratio 1:1), with the speed of 30K/min, be warming up to 1070 ° of C, collect and test remaining residue, and to residue with react front raw sample and carries out the comparison of high-resolution-ration transmission electric-lens (TEM) sign.From figure, being clear that, a large amount of carbon iron clad structures (as Fig. 3 (a)) that exist in raw sample, after carbon dioxide treatment, be coated on the outer field graphite linings of iron particle substantially disappear (as Fig. 3 (b)).
Embodiment 2
The auxiliary Single Walled Carbon Nanotube purifying of carbonic acid gas in fixed bed:
To take the LDH(laminated dihydroxy composite metal hydroxide of Fe-Mg-Al component) system is catalyst precursor, Single Walled Carbon Nanotube prepared by chemical Vapor deposition process (having passed through the preliminary purifications such as acid-alkali treatment) is placed on quartz base plate, and substrate is put into to one section fixed-bed reactor.Under argon gas atmosphere, be warming up to 800 ° of C.After temperature-stable, pass into the carbon dioxide that accounts for total volume concentration 10%, reaction 30min.After reaction finishes, cut off feed carbon dioxide, and make reactor at the argon shield borehole cooling to room temperature.Carbonic acid gas can destroy the outer graphite of carbon iron clad structure, the iron particle is flowed out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 97% by 73%.Simultaneously, before and after purifying, the high-resolution-ration transmission electric-lens photo (TEM) of sample shows, iron particles (as Fig. 4 (a)) a large amount of in raw sample are washed away (as Fig. 4 (b)) in the process of this step purifying.
Embodiment 3
The auxiliary Single Walled Carbon Nanotube purifying of carbonic acid gas in fluidized-bed:
To take the LDH(laminated dihydroxy composite metal hydroxide of Fe-Mg-Al component) system is catalyst precursor, Single Walled Carbon Nanotube sample prepared by chemical Vapor deposition process (growth completes and do not pass through purifying) is placed in the fluidized-bed reactor that diameter is 50mm.Under argon gas atmosphere, be warming up to 950 ° of C.After temperature-stable, pass into the carbon dioxide that accounts for total volume concentration 15%, reaction 3min.After reaction finishes, cut off feed carbon dioxide, and make reactor at the argon shield borehole cooling to room temperature.Utilize the outer graphite of the weak oxide effect destruction carbon iron clad structure of carbonic acid gas, make the iron particle flow out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 97% by 50%.
Embodiment 4
The auxiliary Single Walled Carbon Nanotube purifying of water vapour in fixed bed:
The Fe-MgO system of take is catalyzer, and Single Walled Carbon Nanotube prepared by chemical Vapor deposition process (growth completes and do not pass through purifying) is placed on quartz base plate, and substrate is put into to one section fixed-bed reactor.Under argon gas atmosphere, be warming up to 850 ° of C.After temperature-stable, pass into the water vapour that accounts for total volume concentration 10%, reaction 30min.After reaction finishes, cut off the water vapour charging, and make reactor at the argon shield borehole cooling to room temperature.Water vapour can reach the purpose of destroying carbon iron clad structural outside layers graphite, the iron particle is flowed out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 96% by 7%.
Embodiment 5
The auxiliary double-walled carbon nano-tube purifying of carbonic acid gas in fluidized-bed:
The Fe-MgO system of take is catalyzer, and double-walled carbon nano-tube sample prepared by chemical Vapor deposition process (having passed through the preliminary purifications such as acid-alkali treatment) is placed in the fluidized-bed reactor of diameter 20mm.Under argon gas atmosphere, be warming up to 750 ° of C.After temperature-stable, pass into the carbon dioxide that accounts for total volume concentration 5%, reaction 10min.After reaction finishes, cut off feed carbon dioxide, and make reactor at the argon shield borehole cooling to room temperature.Utilize the outer graphite of the weak oxide effect destruction carbon iron clad structure of carbonic acid gas, make the iron particle flow out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 95% by 88%.
Embodiment 6
The auxiliary double-walled carbon nano-tube purifying of carbonic acid gas-steam mixture in fixed bed:
The Fe-MgO system of take is catalyzer, and double-walled carbon nano-tube prepared by chemical Vapor deposition process (having passed through the preliminary purifications such as acid-alkali treatment) is placed on quartz base plate, and substrate is put into to one section fixed-bed reactor.Under argon gas atmosphere, be warming up to 600 ° of C.After temperature-stable, pass into the water vapour-carbon dioxide mixture (volume ratio 1:1) that accounts for total volume concentration 20%, reaction 20min.After reaction finishes, cut off the charging of carbonic acid gas-steam mixture, and make reactor at the argon shield borehole cooling to room temperature.Carbonic acid gas-water vapour has destroyed the outer graphite of carbon iron clad structure, the iron particle is flowed out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 97% by 88%.
Embodiment 7
The auxiliary carbon nanotube of carbonic acid gas-Graphene heterocomplex purifying in fixed bed:
The Fe-MgO system of take is catalyzer, and carbon nanotube prepared by chemical Vapor deposition process-Graphene heterocomplex (growth completes and do not pass through purifying) is placed on quartz base plate, and substrate is put into to one section fixed-bed reactor.Under argon gas atmosphere, be warming up to 1000 ° of C.After temperature-stable, pass into the carbon dioxide that accounts for total volume concentration 20%, reaction 1h.After reaction finishes, cut off feed carbon dioxide, and make reactor at the argon shield borehole cooling to room temperature.Carbonic acid gas can destroy the outer graphite of carbon iron clad structure, the iron particle is flowed out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 98% by 20%.
Embodiment 8
The auxiliary carbon nanotube of water vapour-carbon dioxide mixture-Graphene heterocomplex purifying in fluidized-bed:
The Fe-MgO system of take is catalyzer, and carbon nanotube prepared by chemical Vapor deposition process-Graphene heterocomplex (having passed through the preliminary purifications such as acid-alkali treatment) is placed in the fluidized-bed reactor of diameter 20mm.Under argon gas atmosphere, be warming up to 700 ° of C.After temperature-stable, pass into the water vapour-carbon dioxide mixture (water vapour and carbonic acid gas volume ratio 1:2) that accounts for total volume concentration 15%, reaction 30min.After reaction finishes, cut off water vapour-carbon dioxide mixture charging, and make reactor at the argon shield borehole cooling to room temperature.Utilize the outer graphite of the weak oxide effect destruction carbon iron clad structure of water vapour-carbon dioxide mixture, make the iron particle flow out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 95% by 75%.
Embodiment 9
The auxiliary few-wall carbon nanotube purifying of carbonic acid gas in fluidized-bed:
The Fe-MgO system of take is catalyzer, and few-wall carbon nanotube sample prepared by chemical Vapor deposition process (having passed through the preliminary purifications such as acid-alkali treatment) is placed in the fluidized-bed reactor of diameter 20mm.Under argon gas atmosphere, be warming up to 900 ° of C.After temperature-stable, pass into the carbon dioxide that accounts for total volume concentration 20%, reaction 20min.After reaction finishes, cut off feed carbon dioxide, and make reactor at the argon shield borehole cooling to room temperature.Utilize the outer graphite of the weak oxide effect destruction carbon iron clad structure of carbonic acid gas, make the iron particle flow out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 96% by 85%.
The auxiliary multi-walled carbon nano-tubes purifying of water vapour in fixed bed:
The Fe-MgO system of take is catalyzer, and multi-walled carbon nano-tubes prepared by chemical Vapor deposition process (growth completes and do not pass through purifying) is placed on quartz base plate, and substrate is put into to one section fixed-bed reactor.Under argon gas atmosphere, be warming up to 500 ° of C.After temperature-stable, pass into the water vapour that accounts for total volume concentration 10%, reaction 10min.After reaction finishes, cut off the water vapour charging, and make reactor at the argon shield borehole cooling to room temperature.Water vapour has destroyed the outer graphite of carbon iron clad structure, the iron particle is flowed out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 93% by 30%.
Embodiment 11
The auxiliary multi-walled carbon nano-tubes purifying of carbonic acid gas in fluidized-bed:
The Fe-MgO system of take is catalyzer, and multi-walled carbon nano-tubes prepared by chemical Vapor deposition process (having passed through the preliminary purifications such as acid-alkali treatment) is placed in the fluidized-bed reactor of diameter 20mm.Under argon gas atmosphere, be warming up to 550 ° of C.After temperature-stable, pass into the carbonic acid gas that accounts for total volume concentration 1%, reaction 30min.After reaction finishes, cut off feed carbon dioxide, and make reactor at the argon shield borehole cooling to room temperature.Carbonic acid gas has destroyed the outer graphite of carbon iron clad structure, the iron particle is flowed out and be easy to be gone by pickling.Through after cleanup acid treatment, the thermogravimetric analysis result of sample before and after the comparison purifying, carbon content is promoted to 95% by 80%.
Claims (5)
1. based on the weak oxide ambient oxidation, assist acid-treated purification method of carbon nanometer pipe for one kind, it is characterized in that, concrete steps are as follows:
(1) adopt chemical vapor deposition for carbon nanotubes, growth is completed to carbon nanotube not purified or process acid-alkali treatment preliminary purification and be placed in reactor; At first to reactor, continue to pass into inertia protection gas, reactor heating is until reaction zone temperature rises to 500～1400 ° of C, after temperature-stable, pass into weak oxidant, be used to destroying the outer graphite of carbon iron clad structure, remove thereby the iron be wrapped by particle is flowed out more easily;
(2) by acid treatment, wash away the iron particle of outflow, improve purity and the quality of sample;
(3) detect the purity of the carbon nanotube sample that obtains, if reach required standard, purifying completes; If do not reach required standard, repeating step (1) and step (2), until purity reaches required standard.
2. purification method of carbon nanometer pipe according to claim 1 is characterized in that: described inertia protection gas is argon gas, helium or nitrogen.
3. purification method of carbon nanometer pipe according to claim 1, it is characterized in that: described weak oxidant is one or more in carbonic acid gas, water vapour, oxygen and chlorine.
4. purification method of carbon nanometer pipe according to claim 3; it is characterized in that: described while passing into one or more in carbonic acid gas, water vapour, oxygen and chlorine; this part weak oxidant gas accounts for and passes into 1%～50% of gas reactor cumulative volume, and rest part is still inert protective gas.
5. purification method of carbon nanometer pipe according to claim 1, it is characterized in that: acid treatment method in described step (2), through the sample that weak oxide is processed, to immerse in excessive hydrochloric acid, nitric acid or sulphuric acid soln, and solution stirring is heated, temperature maintains 50～100 ° of C, time length 6～12h; With centrifugal or filter type, carry out liquid-solid separation afterwards, and the solid sample drying-granulating that will obtain.
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| 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 |
| CN106185867A (en) * | 2016-08-22 | 2016-12-07 | 赖世权 | The purity of CNT improves method |
| CN106185873A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | Intelligent carbon nanotube purification system |
| CN106315560A (en) * | 2016-08-22 | 2017-01-11 | 赖世权 | Carbon nanotube purification method |
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| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
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| CN107074548A (en) * | 2015-09-15 | 2017-08-18 | Lg化学株式会社 | With the crystalline CNT of improvement |
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| CN110065937A (en) * | 2018-01-23 | 2019-07-30 | 清华大学 | The method of oxidation multi-wall carbon nano-tube tube |
| CN109650379A (en) * | 2019-02-19 | 2019-04-19 | 厦门大学 | A kind of single-walled carbon nanotube graded oxidation purification process |
| CN110562960A (en) * | 2019-09-05 | 2019-12-13 | 太原理工大学 | preparation and purification method of coal-based carbon nano tube |
| CN110562960B (en) * | 2019-09-05 | 2022-08-02 | 太原理工大学 | Preparation and purification method of coal-based carbon nano tube |
| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
| CN115703635A (en) * | 2021-08-11 | 2023-02-17 | 南京行创新材料有限公司 | Method for purifying carbon nano tube |
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