CN115626633B - Purification method of single-walled carbon nanotube - Google Patents
Purification method of single-walled carbon nanotube Download PDFInfo
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- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000000746 purification Methods 0.000 title abstract description 25
- 239000012065 filter cake Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 17
- 238000010992 reflux Methods 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 10
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000464 low-speed centrifugation Methods 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000004227 thermal cracking Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- 238000010891 electric arc Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 239000003929 acidic solution Substances 0.000 claims 2
- 238000001471 micro-filtration Methods 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000010306 acid treatment Methods 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000001962 electrophoresis Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002270 exclusion chromatography Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000004792 oxidative damage Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
- C01B32/159—Carbon nanotubes single-walled
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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
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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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
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Abstract
The invention belongs to the technical field of carbon nano material purification, and particularly relates to a purification method of a single-walled carbon nano tube. In order to develop a more suitable single-walled carbon nanotube purifying method, the invention uniformly calcines a crude single-walled carbon nanotube product and sodium peroxide or sodium nitrate, a calcined sample is dispersed in water, a filter cake is collected by filtration, the filter cake is dispersed in water again, and then nitric acid solution is added for stirring reflux treatment; centrifuging to remove supernatant after refluxing, and washing with water to neutrality; uniformly dispersing the washed sample, and collecting single-walled carbon nanotubes in the upper layer solution through low-speed centrifugation and microporous filtration; and drying and crushing the collected sample, and then placing the sample in a hydrogen-Ar mixed gas atmosphere for low-temperature calcination treatment to obtain a purified single-walled carbon nanotube product. The single-wall carbon nanotube purified by the method has the purity of more than 95 percent, high purification efficiency and good product quality.
Description
Technical Field
The invention belongs to the technical field of carbon nano material purification, and particularly relates to a purification method of a single-walled carbon nano tube.
Background
Single-walled carbon nanotubes have been widely used in various fields such as nanoelectronics, energy devices, and biosensors because of their excellent electrical, chemical, thermal, and mechanical properties since they were discovered in 1993. Currently, single-walled carbon nanotubes are generally prepared by methods such as arc discharge, laser evaporation, thermal cracking with catalysts, and the like. In the production process of single-wall carbon nanotubes, besides the large-scale preparation process, the purification process is also a key to influence the application of the single-wall carbon nanotubes, because the prepared single-wall carbon nanotube samples generally contain a large amount of impurities, and the common impurities mainly comprise two major types of carbon impurities (graphite particles, carbon nanoparticles, amorphous carbon and the like formed in the growth process of the carbon nanotubes) and metal impurities (derived from transition metal catalysts). The presence of these impurities severely affects the properties and applications of single-walled carbon nanotubes. Therefore, developing a highly efficient purification method is important for obtaining high purity single-walled carbon nanotube products.
By utilizing the characteristics that the physical properties of carbon impurities are different from those of single-wall carbon nanotubes (such as density, stability, metallic property and the like), and the metal impurities are easy to dissolve in acid or sublimate at high temperature, the existing method for purifying the single-wall carbon nanotubes mainly comprises the following steps: (1) physical purification method: including centrifugation, electrophoresis, filtration, and space exclusion chromatography; (2) chemical purification method: including a gas phase oxidation purification method, a liquid phase oxidation purification method, etc.; (3) comprehensive purification method: including acid treatment and gas phase oxidation, acid treatment and high temperature annealing, acid treatment and gas phase oxidation and high temperature annealing, acid treatment and electrophoresis, microporous filtration and electrolysis, etc. In purifying single-walled carbon nanotubes, most important is the care to prevent the carbon tubes from oxidative damage, as well as the economics and efficiency of the process. At present, a great deal of researches show that the most effective method for removing metal impurities is to acidify the carbon tube, because the temperature of the acidizing treatment is lower, the equipment requirement is lower, and compared with a high-temperature purification method, the economical efficiency is better, and the mass production is easier to realize. However, the acidification treatment cannot deeply dissolve the metal particles wrapped on the inner wall of the carbon nano tube, and other methods are needed to assist in reducing the impurity content. Therefore, it is necessary to develop a more suitable purification method to ensure that the carbon layer on the surface of the metal particles is completely dissolved out while not seriously damaging the structure of the single-walled carbon nanotubes, thereby greatly improving the purity of the single-walled carbon nanotubes.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a purification method of single-walled carbon nanotubes, which can efficiently remove metal impurities and improve the purity of single-walled carbon nanotube products through the oxidation of sodium peroxide/sodium nitrate.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
the invention provides a purification method of single-walled carbon nanotubes, which comprises the following steps:
s1, uniformly mixing a single-walled carbon nanotube crude product with sodium peroxide or sodium nitrate, and then calcining;
s2, dispersing the calcined sample in water, filtering and collecting a filter cake, dispersing the filter cake in water again, and adding an acid solution for stirring and refluxing reaction;
s3, centrifuging the suspension after backflow to remove supernatant, washing the suspension with water to be neutral, uniformly dispersing the washed sample, and collecting a filter cake through low-speed centrifugation and microporous filtration;
s4, drying and crushing the filter cake collected in the step S3, and then placing the filter cake in a hydrogen-Ar mixed gas atmosphere for low-temperature calcination treatment to obtain a purified single-walled carbon nanotube product.
Based on the characteristic of poor stability of carbon impurity elements, although the single-wall carbon nano tube with better stability is easily separated by high-temperature air annealing treatment, if an elastic layer on the surface of a metal catalyst particle can be damaged by a certain method in the step, the purification difficulty is greatly reduced. Therefore, a small amount of sodium peroxide/sodium nitrate is added into the crude single-walled carbon nanotube product, and then high-temperature air annealing treatment is carried out, so that carbon impurities are removed by oxidization, and a carbon layer attached to the surface of a metal is selectively oxidized, so that nano particles of the metal catalyst are exposed, further, the metal impurities can be effectively removed in the next acid treatment process, and the purity of the single-walled carbon nanotube product is improved.
Preferably, in the step S1, the addition mass of sodium peroxide or sodium nitrate is 1-10% of the crude single-walled carbon nanotube product.
Preferably, in step S1, the temperature of the calcination treatment is 300-500 ℃ and the time is 10-60min.
Preferably, in the step S2, the acid solution is a nitric acid solution, the mass ratio of the acid solution to the filter cake is 50-100:1, and the concentration of the nitric acid solution is 4-10mol/L.
Preferably, in step S2, the mass ratio of the calcined sample or filter cake to water is 1:10-20.
Preferably, in step S2, the reaction time of the stirring reflux reaction is 4-12 hours.
Preferably, in the step S3, the low-speed centrifugation is performed at 5000rpm for 10-30min, and the microporous filtration is performed by using a microporous filter membrane of 0.22 μm.
Preferably, in step S4, the temperature of the low-temperature calcination treatment is 200-300 ℃ and the time is 30-120min.
Preferably, in step S4, the drying is performed at 80-120℃for 8-12 hours.
Preferably, the crude single-walled carbon nanotube is prepared by arc discharge method, laser evaporation method, chemical vapor deposition method, or catalytic thermal cracking method.
Preferably, in step S3, the centrifugation is performed at 10000rpm for 30-60min.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a purification method of a single-walled carbon nanotube, which specifically comprises the following steps: uniformly calcining the crude single-wall carbon nano tube product and sodium peroxide or sodium nitrate, dispersing the calcined sample in water, filtering to collect a filter cake, dispersing the filter cake in water again, and adding a nitric acid solution for stirring and refluxing treatment; centrifuging to remove supernatant after refluxing, and washing with water to neutrality; uniformly dispersing the washed sample, and collecting single-walled carbon nanotubes in the upper layer solution through low-speed centrifugation and microporous filtration; and drying and crushing the collected sample, and then placing the sample in a hydrogen-Ar mixed gas atmosphere for low-temperature calcination treatment to obtain a purified single-walled carbon nanotube product. The single-wall carbon nanotube purified by the method has the purity of more than 95 percent, high purification efficiency and good product quality.
Drawings
Fig. 1 is a process route diagram for purifying single-walled carbon nanotubes.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1 purification method of Single-walled carbon nanotubes
As shown in the purification process route of fig. 1, the method comprises the steps of:
(1) Adding 0.1g of sodium peroxide into 1g of single-walled carbon nanotube crude product (purchased from Nanjing Xianfeng nano materials science and technology Co., ltd., purity of 50% and prepared by a mobile catalysis method), fully grinding and uniformly mixing, and then placing the mixture powder into a muffle furnace to be calcined at a calcining temperature of 400 ℃ for 60min;
(2) Adding 100g of pure water into the calcined mixture, carrying out ultrasonic treatment for 10min, filtering by using a microporous filter membrane with the diameter of 0.22 mu m to remove sodium salt, and collecting a filter cake;
(3) Adding 30g of pure water into the filter cake, adding 100mL of nitric acid with the concentration of 8mol/L, and stirring at 200rpm for reflux reaction for 8 hours;
(4) Centrifuging the suspension after reflux at 10000rpm for 45min, removing supernatant, washing with pure water to neutrality, adding 100mL of pure water to ultrasonically disperse the washed sample, centrifuging at 5000rpm for 30min, filtering the supernatant obtained by centrifugation with a microporous filter membrane of 0.22 μm, collecting filter cake, and collecting single-walled carbon nanotubes from the supernatant;
(5) Drying the filter cake sample in a vacuum drying oven at 80-120deg.C for 8-12 hr, pulverizing, transferring to a tube furnace at 250deg.C, and mixing with hydrogen-Ar gas (95% Ar+5% H) 2 ) Calcination treatment is carried out for 30min under atmosphere, thus obtaining 0.28g of purified single-walled carbon nanotube product. The purity was 95%, ash content 0.05% and yield 32%.
Example 2 purification method of Single-walled carbon nanotubes
As shown in the purification process route of fig. 1, the method comprises the steps of:
(1) Adding 10mL of ethanol solution of sodium nitrate (containing 0.1g of sodium nitrate) into 1g of single-walled carbon nanotube crude product, fully grinding, uniformly mixing and drying, and placing the dried mixture powder into a muffle furnace to be calcined at a calcining temperature of 350 ℃ for 60min;
(2) Adding 100g of pure water into the calcined mixture, carrying out ultrasonic treatment for 10min, filtering by using a microporous filter membrane with the diameter of 0.22 mu m to remove sodium salt, and collecting a filter cake;
(3) Adding 30g of pure water into the filter cake, adding 100mL of nitric acid with the concentration of 8mol/L, and stirring at 200rpm for reflux reaction for 8 hours;
(4) Centrifuging the suspension after reflux at 10000rpm for 45min, removing supernatant, washing with pure water to neutrality, adding 100mL of pure water to ultrasonically disperse the washed sample, centrifuging at 5000rpm for 30min, filtering the supernatant obtained by centrifugation with a microporous filter membrane of 0.22 μm, collecting filter cake, and collecting single-walled carbon nanotubes from the supernatant;
(5) Drying the filter cake sample in a vacuum drying oven at 80-120deg.C for 8-12 hr, pulverizing, transferring to a tube furnace at 250deg.C, and mixing with hydrogen-Ar gas (95% Ar+5% H) 2 ) Calcining for 30min under atmosphere to obtain 0.35g of purified single-walled carbon nanotube product. The purity was found to be 96%, the ash content 0.03% and the yield 28%.
Method for purifying single-walled carbon nanotubes of comparative example 1
(1) Calcining 1g of the crude single-walled carbon nanotube product in a muffle furnace at a calcining temperature of 350 ℃ for 60min;
(2) Adding 100g of pure water into the calcined mixture, carrying out ultrasonic treatment for 10min, filtering by using a microporous filter membrane with the diameter of 0.22 mu m to remove sodium salt, and collecting a filter cake;
(3) Adding 30g of pure water into the filter cake, adding 100mL of nitric acid with the concentration of 8mol/L, and stirring at 200rpm for reflux reaction for 8 hours;
(4) Centrifuging the suspension after reflux at 10000rpm for 45min, removing supernatant, washing with pure water to neutrality, adding 100mL of pure water to ultrasonically disperse the washed sample, centrifuging at 5000rpm for 30min, filtering the supernatant obtained by centrifugation with a microporous filter membrane of 0.22 μm, collecting filter cake, and collecting single-walled carbon nanotubes from the supernatant;
(5) Drying the filter cake sample in a vacuum drying oven at 80-120deg.C for 8-12 hr, pulverizing, transferring to a tube furnace at 250deg.C, and mixing with hydrogen-Ar gas (95% Ar+5% H) 2 ) Calcination treatment for 30min under atmosphere gave 0.4g of purified single-walled carbon nanotube product, which was found to have a purity of 90%, ash content of 0.5% and yield of 40%.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (8)
1. A method for purifying single-walled carbon nanotubes, comprising the steps of:
s1, uniformly mixing a single-walled carbon nanotube crude product with sodium peroxide or sodium nitrate, and then calcining; the addition mass of sodium peroxide or sodium nitrate is 1-10% of the crude single-walled carbon nanotube, the calcination treatment temperature is 350-400 ℃ and the calcination treatment time is 10-60min;
s2, dispersing the calcined sample in water, filtering and collecting a filter cake, dispersing the filter cake in water again, and adding an acid solution for stirring and refluxing reaction;
s3, centrifuging the suspension after backflow to remove supernatant, washing the suspension with water to be neutral, uniformly dispersing the washed sample, and collecting a filter cake through low-speed centrifugation and microporous filtration;
s4, drying and crushing the filter cake collected in the step S3, and then placing the filter cake in a hydrogen-Ar mixed gas atmosphere for low-temperature calcination treatment to obtain a purified single-walled carbon nanotube product.
2. The method for purifying single-walled carbon nanotubes according to claim 1, wherein in the step S2, the acidic solution is a nitric acid solution, the mass ratio of the acidic solution to the filter cake is 50-100:1, and the concentration of the nitric acid solution is 4-10mol/L.
3. The method according to claim 1, wherein in the step S2, the mass ratio of the calcined sample or filter cake to water is 1:10-20.
4. The method according to claim 1, wherein in the step S2, the reaction time of the stirring reflux reaction is 4 to 12 hours.
5. The method according to claim 1, wherein in the step S3, the low-speed centrifugation is performed at 5000rpm for 10-30min, and the microfiltration is performed with a 0.22 μm microfiltration membrane.
6. The method according to claim 1, wherein in step S4, the low-temperature calcination treatment is performed at 200-300 ℃ for 30-120min.
7. The method according to claim 1, wherein in step S4, the drying is performed at 80-120 ℃ for 8-12 hours.
8. The method for purifying single-walled carbon nanotubes according to claim 1, wherein the crude single-walled carbon nanotubes are prepared by arc discharge, laser evaporation, chemical vapor deposition, or catalytic thermal cracking.
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| CN101177254A (en) * | 2006-11-10 | 2008-05-14 | 同济大学 | Hydrophilicity carbon nanometer-tube and preparation method thereof |
| CN106829933A (en) * | 2017-03-19 | 2017-06-13 | 兰州理工大学 | A kind of method for going to remove water reclaimed water dirt and heavy metal ion |
| CN107082419A (en) * | 2017-04-14 | 2017-08-22 | 广西大学 | A kind of preparation method of flexible fiber electrode |
| 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 | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177254A (en) * | 2006-11-10 | 2008-05-14 | 同济大学 | Hydrophilicity carbon nanometer-tube and preparation method thereof |
| CN106829933A (en) * | 2017-03-19 | 2017-06-13 | 兰州理工大学 | A kind of method for going to remove water reclaimed water dirt and heavy metal ion |
| CN107082419A (en) * | 2017-04-14 | 2017-08-22 | 广西大学 | A kind of preparation method of flexible fiber electrode |
| 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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