CN100562491C - The method of a kind of purification of Multi-wall Carbon Nanotubes or carbon nano fiber - Google Patents
The method of a kind of purification of Multi-wall Carbon Nanotubes or carbon nano fiber Download PDFInfo
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Abstract
The present invention relates to the purification techniques of carbon nanotube/nano carbon fiber, be specially a kind of purification process that comprises impurity such as metal catalyst and carbon nano-particle in multi-walled carbon nano-tubes/carbon nano fiber primary sample of removing.This method comprises that original multi-walled carbon nano-tubes/carbon nano fiber is carried out high temperature graphitization handles the volatile impurity of high temperature such as (1800-3000 ℃) removal metal catalyst, and the defective in the elimination multiple-wall carbon nanotube, utilize the ultrasonic graphitized carbon nano pipe/carbon nano fiber sample of dispersant solution to carry out homodisperse subsequently with different carbon structures, make different carbon structures form discrete phase, remove by filter in the sample discrete carbon nano-particle at last and obtain high-purity carbon nano tube/carbon nano fiber sample.This method has simply, characteristics such as purity is high, easy industrialization.
Description
Technical field
The present invention relates to the purification techniques of carbon nanotube/nano carbon fiber, be specially a kind of method of purification of Multi-wall Carbon Nanotubes/carbon nano fiber.
Background technology
The carbon nanotube/nano carbon fiber has become the research forward position and the focus in fields such as physics, chemistry, biology, material owing to having particular structure feature, unusual physicochemical property and enjoying people to pay close attention in following high-tech area potential using value.Arc process and catalytic chemical vapor deposition technique (catalytic chemical vapor decomposition are mainly adopted in a large amount of preparations of carbon current nanotube/carbon nano fiber, CCVD), the carbon nanotube/nano carbon fiber of preparing is usually with more or less impurity, as charcoal impurity such as metal catalyst and amorphous carbon, soccerballene, carbon nano-particles, especially the carbon nanotube/nano carbon fiber that comes out of suitability for industrialized production, its foreign matter content is higher.It is poor that the carbon nanotube/nano carbon fiber of CCVD method preparation also has degree of crystallinity, the characteristics that defective is many.Yet can the structural integrity of carbon nanotube/nano carbon fiber and purity height have decisive significance to giving full play to its excellent mechanical property and electric property.Therefore, desire is furtherd investigate the characteristic of this novel material, and for the application of carbon nanotube/nano carbon fiber is cleared away the obstacles, research just seems very important and necessary to the purifying of carbon nanotube/nano carbon fiber.The purifying of carbon nanotube/nano carbon fiber mainly contains three aspect implications: the one, remove granules of catalyst, and the 2nd, remove the impurity charcoal, the 3rd, eliminate the textural defect in the carbon nanotube/nano carbon fibre growth process.Purifying to the carbon nanotube/nano carbon fiber mainly is to utilize carbon nanotube/nano carbon fiber and the difference of impurity at aspects such as physics and chemistry to reach the purification purpose, and purification process mainly is divided into physical method and chemical process.Physical method mainly be utilize that ultrasonic concussion is handled, centrifugal, deposition, filtration, solution suspends or method separating impurity and carbon nanotube/nano carbon fiber such as gel chromatography, thereby obtain pure carbon nanotube/nano carbon fiber.Physical method destroys little to the carbon nanotube/nano carbon fiber structural, but purity, efficient are low, are not easy to industrialization.Chemical process mainly is that oxidation adds pickling, and pickling can be removed metal catalyst, and oxidation can be removed charcoal impurity.But these class methods also cause the change or even the havoc of carbon nanotube/nano carbon fiber structural integrity in purifying carbon nano-tube/carbon nano fiber, because though the impurity charcoal is oxidized prior to the carbon nanotube/nano carbon fiber in theory, but the condition of atmospheric oxidation or strong acid oxidation is wayward in the actually operating, especially under the big situation of treatment capacity, the ununiformity that has oxidizing reaction is difficult to guarantee that the carbon nanotube/nano carbon fiber is not etched.
Summary of the invention
The present invention is directed to the deficiency of existing carbon nanotube/nano carbon fiber purification process and a kind of purification process of structure and performance novel, that efficiently, do not destroy multi-walled carbon nano-tubes/carbon nano fiber is provided, be characterized in removing metal catalyst by graphitization processing, improve the degree of crystallinity of carbon nanotube/nano carbon fiber, eliminate the microtexture defective; And utilize dispersion agent that different shapes particulate selectivity dissemination is isolated carbon nano-particle impurity in the carbon nanotube/nano carbon fiber sample, structure to the carbon nanotube/nano carbon fiber can not damage, and can obtain purity height, carbon nanotube/nano carbon fiber that performance is good.
Technical scheme of the present invention is:
The method of a kind of purification of Multi-wall Carbon Nanotubes or carbon nano fiber, concrete steps are as follows:
(1) with the high temperature graphitization heat treating method original carbon nanotube or carbon nano fiber sample are handled: original carbon nanotube or carbon nano fiber sample are put into plumbago crucible, place graphitizing furnace; Feed rare gas element, thermal treatment temp is 1800-3000 ℃, and soaking time is 10-300min;
(2) disperse graphite carbon nano tube or carbon nano fiber sample with dispersant solution, apply supersound process simultaneously: after graphitized carbon nano pipe or carbon nano fiber mechanical disintegration, be immersed in the dispersant solution, stir 30-120min, apply supersound process 10-180min; Dispersion agent is at least a kind of of sodium stearate, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, acrylic copolymer, hydrolysis acrylamide, amino alkyl acrylates multipolymer, the acrylamide copolymer that contains quaternary ammonium group, sapn, tween, polyvinyl alcohol, EO affixture, the weight concentration of dispersion agent in dispersant solution is 0.01-3%, and the weight of dispersion agent is the 5-60% of carbon nanotube or carbon nano fiber weight;
(3) remove carbon nano-particle with mesh gauze filter: disperse carbon nanotube or the carbon nano fiber suspension obtain through dispersion agent with 200-500 purpose screen filtration, the carbon nano-particle of non-tubular shape preferentially by the dispersion agent stable dispersion in liquid phase, be separated by filtration;
(4) filter cake that filtration is obtained is scattered in supersound process in the solvent once more, forms suspension, filters once more;
Repeating step (4) to be operated to filtrate colourless, finally obtaining filter cake is exactly highly purified carbon nanotube or carbon nano fiber.
Described solvent is at least a kind of of water, ethanol, butanols, acetone, benzene, dimethylbenzene, toluene, vinyl acetic monomer, N-BUTYL ACETATE.
In the described step (2), the granularity of graphitized carbon nano pipe or carbon nano fiber is the 10-100 order after the mechanical disintegration.
In the described step (2), stir a kind of into mechanical stirring or magnetic agitation.
Advantage of the present invention and beneficial effect are:
1. the present invention's purifying carbon nano-tube/carbon nano fiber on a large scale, and guarantee in purifying carbon nano-tube/carbon nano fiber the not structure of destroying carbon nanometer tube/carbon nano fiber and performance.High-temperature heat treatment (greying) method on the one hand can evaporate carbon nanotube/carbon nano fiber inside (as top, tube cavity) metal, the structural integrity of carbon nanotube/nano carbon fiber be can improve on the other hand effectively, degree of crystallinity and thermostability improved.But through after the graphitization processing, the impurity charcoal in the carbon nanotube/nano carbon fiber, particularly carbon nano-particle is not removed, and on the contrary, because experienced pyroprocessing equally, the degree of graphitization of carbon nano-particle also is improved, and is difficult to remove with usual way.Can see carbon nano-particle and other random carbon nano-particle of a large amount of this polyhedral structures in the sample after the greying.
2. dispersion agent of the present invention is used for the dispersion of carbon nano-particle, and has been determined the intensity and the scope of its mutual model ylid bloom action power and surfactant-dispersed effect by the composition of discrete particles, shape, dimension.The shape of carbon nano-particle and multi-walled carbon nano-tubes/carbon nano fiber, size, dimension have determined the significant difference of model ylid bloom action potential energy therebetween, and promptly multi-walled carbon nano-tubes/carbon nano fiber is than the easier reunion of carbon nano-particle, more difficult dispersion.Correct kind, the consumption of selecting dispersion agent, make its optionally dispersed carbon nano particle, and can not dispersing Nano carbon tubes/carbon nano fiber, thereby with carbon nano-particle and carbon nanotube/nano carbon fibre separation, can not damage the carbon nanotube/nano carbon fiber structural by the simple filtration separation method.
3. the present invention is with respect to classical acid oxidative purification method, has that technology is simple, easy to operate, purification efficiency is high, to the destructive little advantage of carbon nanotube/nano carbon fiber structural, is suitable for industrialization.Adopt the inventive method, carbon nanotube/nano carbon fiber purity can reach more than 97%, purification efficiency reach 80-90% (because of metal catalyst content different different).
Description of drawings
(a before Fig. 1 carbon nanotube greying
1-a
3) back (b
1-b
3) the transmission electron microscope photo.
The thermogravimetric curve of (a) back (b) before Fig. 2 carbon nanotube greying.
Fig. 3 adopts that dispersant solution disperses, the electron scanning micrograph of sample after the separating treatment, (a) isolated carbon nano-particle, (b) carbon nanotube of purifying.
Embodiment
Below in conjunction with embodiment and comparative example the present invention is illustrated:
Embodiment 1
The multi-walled carbon nano-tubes sample of CCVD method batch preparations (diameter 20-100nm) places in the plumbago crucible, is put into then in the graphitizing furnace, is warming up to 2500-2700 ℃ under argon shield, and soaking time is 60min, is cooled to room temperature and takes out sample.Membranaceous carbon nanotube sample after the greying with pulverizer smash (granularity is the 10-100 order) standby.High-molecular type dispersing agent (Dispers710) is mixed with the solution of 0.08wt% with ethanol.0.5g graphitized carbon nano pipe is added in the 100g dispersant solution, and behind the magnetic agitation 60min, ultrasonic concussion 20min in ultrasonic cleaning machine obtains the suspension of the carbon nanotube of black.Use 400 these suspension of purpose strainer filtering then, filter cake ultra-sonic dispersion again repeatedly washs in ethanol, filters, until filtrate become colourless, limpid till.The filter cake that finally obtains promptly is the multi-walled carbon nano-tubes of purifying, and purity reaches more than 98%.
(a before the carbon nanotube greying
1-a
3) back (b
1-b
3) the transmission electron microscope photo as shown in Figure 1, the tube wall of carbon nanotube is by disordered structure (Fig. 1 a
2) become laminated structure (Fig. 1 b straight, high-crystallinity
2).The most significant effect is that most metal catalysts all have been evaporated, and has stayed carbon nano-particle (Fig. 1 b hollow, that formed by multilayer polyhedron intussusception
3).The thermogravimetric curve of (a) back (b) as shown in Figure 2 before the carbon nanotube greying, the content of catalyzer is 5wt% in the original carbon nanotube sample, carbon nanotube sample after the greying does not contain or only contains the metal catalyst of trace, and the thermostability of greying sample strengthens.The pattern of the carbon nanotube (b) behind Dispers710 dispersion, isolated carbon nano-particle (a) and the purifying as shown in Figure 3, the carbon nano-particle that is separated (filtrate part) all be hollow, size differs, the carbon ball of diameter about 200nm also can be separated, the sample that finally obtains (filter cake part) is very pure, the overwhelming majority is a carbon nanotube, and a small amount of spherical particle is only arranged.
Embodiment 2
The carbon nano fiber sample of CCVD method batch preparations (diameter 300-500nm) places in the plumbago crucible, is put into then in the graphitizing furnace, is warming up to 2200-2500 ℃ under argon shield, and soaking time is 120min, is cooled to room temperature and takes out sample.Membranaceous carbon nano fiber sample sample after the greying with pulverizer smash (granularity is the 10-100 order) standby.The sodium lauryl sulphate water is mixed with the solution of 0.1wt%.0.5g graphitization nano carbon fiber sample is added in the 120g dispersant solution, and behind the magnetic agitation 60min, ultrasonic concussion 90min in ultrasonic cleaning machine obtains the suspension of the carbon nano fiber sample of black.Use 400 these suspension of purpose strainer filtering then, filter cake ultra-sonic dispersion again repeatedly washs in water, filters, until filtrate become colourless, limpid till.The filter cake that finally obtains promptly is the carbon nano fiber sample of purifying, and purity reaches more than 98%.
Embodiment 3
The multi-walled carbon nano-tubes sample of CCVD method batch preparations (diameter 20-100nm) places in the plumbago crucible, is put into then in the graphitizing furnace, is warming up to 2800-2900 ℃ under argon shield, and soaking time is 30min, is cooled to room temperature and takes out sample.Membranaceous carbon nanotube sample after the greying with pulverizer smash (granularity is the 10-100 order) standby.Dispersion agent (Hydropalat 1080) water is mixed with the solution of 0.15wt%.0.5g graphitized carbon nano pipe is added in the 100g dispersant solution, and behind the magnetic agitation 60min, ultrasonic concussion 30min in ultrasonic cleaning machine obtains the suspension of the carbon nanotube of black.Use 400 these suspension of purpose strainer filtering then, filter cake ultra-sonic dispersion again repeatedly washs in water, filters, until filtrate become colourless, limpid till.The filter cake that finally obtains promptly is the multi-walled carbon nano-tubes of purifying, and purity reaches more than 97%.
Embodiment 4
The multi-walled carbon nano-tubes sample of CCVD method batch preparations (diameter 20-100nm) places in the plumbago crucible, is put into then in the graphitizing furnace, is warming up to 2400-2600 ℃ under argon shield, and soaking time is 90min, is cooled to room temperature and takes out sample.Membranaceous carbon nanotube sample after the greying with pulverizer smash (granularity is the 10-100 order) standby.Dispersion agent (DP983) is mixed with the solution of 0.12wt% with dimethylbenzene.0.5g graphitized carbon nano pipe is added in the 100g dispersant solution, and behind the magnetic agitation 60min, ultrasonic concussion 25min in ultrasonic cleaning machine obtains the suspension of the carbon nanotube of black.Use 400 these suspension of purpose strainer filtering then, filter cake ultra-sonic dispersion again repeatedly washs in dimethylbenzene, filters, until filtrate become colourless, limpid till.The filter cake that finally obtains promptly is the multi-walled carbon nano-tubes of purifying, and purity reaches more than 98%.
Comparative example 1
The multi-walled carbon nano-tubes sample of CCVD method batch preparations (diameter 20-100nm) with pulverizer smash (granularity is the 10-100 order) standby.High-molecular type dispersing agent (Dispers710) is mixed with the solution of 0.08wt% with ethanol.0.5g graphitized carbon nano pipe is added in the 100g dispersant solution, and behind the magnetic agitation 60min, ultrasonic concussion 20min in ultrasonic cleaning machine obtains the suspension of the carbon nanotube of black.Use 400 these suspension of purpose strainer filtering then, the filter cake that obtains is the mixture of multi-walled carbon nano-tubes, carbon nano-particle and metal catalyst.
Comparative example 2
The multi-walled carbon nano-tubes sample of CCVD method batch preparations (diameter 20-100nm) places in the plumbago crucible, is put into then in the graphitizing furnace, is warming up to 2500-2700 ℃ under argon shield, and soaking time is 60min, is cooled to room temperature and takes out sample.Membranaceous carbon nanotube sample after the greying with pulverizer smash (granularity is the 10-100 order) standby.0.5g graphitized carbon nano pipe is added in the 200g alcohol solvent, and behind the magnetic agitation 60min, ultrasonic concussion 40min in ultrasonic cleaning machine obtains the suspension of the carbon nanotube of black.Use 400 these suspension of purpose strainer filtering then, the filter cake that obtains is the mixture of multi-walled carbon nano-tubes and carbon nano-particle.
Claims (4)
1, the method for a kind of purification of Multi-wall Carbon Nanotubes or carbon nano fiber is characterized in that concrete steps are as follows:
(1) with the high temperature graphitization heat treating method original carbon nanotube or carbon nano fiber sample are handled: original carbon nanotube or carbon nano fiber sample are put into plumbago crucible, place graphitizing furnace; Feed rare gas element, thermal treatment temp is 1800-3000 ℃, and soaking time is 10-300min;
(2) disperse graphite carbon nano tube or carbon nano fiber sample with dispersant solution, apply supersound process simultaneously: after graphitized carbon nano pipe or carbon nano fiber mechanical disintegration, be immersed in the dispersant solution, stir 30-120min, apply supersound process 10-180min; Dispersion agent is at least a kind of of sodium stearate, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, acrylic copolymer, hydrolysis acrylamide, amino alkyl acrylates multipolymer, the acrylamide copolymer that contains quaternary ammonium group, sapn, tween, polyvinyl alcohol, EO affixture, the weight concentration of dispersion agent in dispersant solution is 0.01-3%, and the weight of dispersion agent is the 5-60% of carbon nanotube or carbon nano fiber weight;
(3) remove carbon nano-particle with mesh gauze filter: disperse carbon nanotube or the carbon nano fiber suspension obtain through dispersion agent with 200-500 purpose screen filtration, the carbon nano-particle of non-tubular shape preferentially by the dispersion agent stable dispersion in liquid phase, be separated by filtration;
(4) filter cake that filtration is obtained is scattered in supersound process in the solvent once more, forms suspension, filters once more;
Repeating step (4) to be operated to filtrate colourless, finally obtaining filter cake is exactly highly purified carbon nanotube or carbon nano fiber.
2, according to the method for described purification of Multi-wall Carbon Nanotubes of claim 1 or carbon nano fiber, it is characterized in that: described solvent is at least a kind of of water, ethanol, butanols, acetone, benzene, dimethylbenzene, toluene, vinyl acetic monomer, N-BUTYL ACETATE.
3, according to the method for described purification of Multi-wall Carbon Nanotubes of claim 1 or carbon nano fiber, it is characterized in that: in the described step (2), the granularity of graphitized carbon nano pipe or carbon nano fiber is the 10-100 order after the mechanical disintegration.
4, according to the method for described purification of Multi-wall Carbon Nanotubes of claim 1 or carbon nano fiber, it is characterized in that: in the described step (2), stir a kind of into mechanical stirring or magnetic agitation.
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