CN103979526A - Purifying method of macroscopic body of carbon nano tube - Google Patents
Purifying method of macroscopic body of carbon nano tube Download PDFInfo
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- CN103979526A CN103979526A CN201410218259.3A CN201410218259A CN103979526A CN 103979526 A CN103979526 A CN 103979526A CN 201410218259 A CN201410218259 A CN 201410218259A CN 103979526 A CN103979526 A CN 103979526A
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Abstract
The invention provides a purifying method of a macroscopic body of a carbon nano tube. The method comprises the following steps: S1, constructing an electrolytic device, wherein the electrolytic device comprises a cathode, an anode and an electrolyte which are located in an electrolytic bath; and S2, attaching the macroscopic body of the carbon nano tube to the anode and electrifying for electrolysis and purification. Compared with the prior art, the macroscopic body of the carbon nano tube is purified by the electrolytic method, so that the problem that metal catalysts inside the macroscopic body of the carbon nano tube are hard to remove for the macroscopic body of the carbon nano tube soaked by a conventional acidic solution, and the macroscopic body of the carbon nano tube is thoroughly purified. The purifying method provided by the invention is simple and convenient in process and method, low in cost, wide in application and suitable for popularization and application on a large scale.
Description
Technical field
The present invention relates to nano material and manufacture field, relate in particular to a kind of purification process of carbon nano-tube macroscopic body.
Background technology
Carbon nano-tube macroscopic body is that it is the important component part of carbon nanotube research field by a large amount of carbon nanotubes macroscopic material forming that is mutually intertwined and connected.Carbon nano-tube macroscopic body has the features such as high strength, high conductivity, frivolous, good snappiness and chemical stability, has obtained certain progress in the applied research in the fields such as electron electric power, energy storage, intelligent sensing, matrix material, aerospace.Aspect prepared by carbon nano-tube macroscopic body, people have successively been developed carbon nano-tube solution spin coating and filtration method, floating catalytic gas phase direct growth method, and can spinning vertical carbon nanotube array direct spinning etc. preparation method.Wherein the above two are difficult to avoid existing in carbon nano-tube macroscopic body part metals granules of catalyst in preparation method, and this will inevitably can have influence on its performance performance and follow-up Application and Development.
At present, mainly concentrate on the purifying of carbon nanotube dust for purification process and the technology of carbon nano-tube macroscopic body, the purification process of the carbon nano-tube macroscopic body beyond carbon nanotube dust is also rarely had to report; Moreover the purification process of common acid soak can only be removed some metal catalysts on carbon nano-tube macroscopic body top layer, its inner a large amount of metal catalyst is almost difficult to remove.In view of the problem of above existence, a kind of purification process of effective carbon nano-tube macroscopic body is needed badly and is developed application.
Summary of the invention
The object of the present invention is to provide a kind of purification process of carbon nano-tube macroscopic body of simple and efficient, with low cost, easy handling.
For achieving the above object, the invention provides a kind of purification process of carbon nano-tube macroscopic body, the method comprises the following steps:
S1, structure electrolyzer, described electrolyzer comprises the yin, yang electrode and the ionogen that are positioned at electrolyzer;
S2, carbon nano-tube macroscopic body is attached on described positive electrode, electrolysis purifying is carried out in energising.
As a further improvement on the present invention, the material of described yin, yang electrode is graphite or other inert metal.
As a further improvement on the present invention, described yin, yang electrode be shaped as pole shape.
As a further improvement on the present invention, described " carbon nano-tube macroscopic body is attached on described positive electrode " specifically comprises:
Adopt the mode of sandwich structure that carbon nano-tube macroscopic body and the stack of non-dust cloth interval are wound on the pole shape positive electrode of described electrolyzer.
As a further improvement on the present invention, described yin, yang electrode be shaped as tabular.
As a further improvement on the present invention, described " carbon nano-tube macroscopic body is attached on described positive electrode " specifically comprises:
Described carbon nano-tube macroscopic body is directly fitted on the tabular positive electrode of described electrolyzer.
As a further improvement on the present invention, described ionogen is acid solution, and described acid solution is selected from one or more the combination in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, oxalic acid, phenylformic acid, succinic acid, three oxygen methylsulfonic acids.
As a further improvement on the present invention, step S2 also comprises:
In the process of the purifying of carbon nano-tube macroscopic body, constantly stir described ionogen.
As a further improvement on the present invention, voltage range when described " electrolysis purifying is carried out in energising " is 0.5 ~ 30V, and range of current is 0.1 ~ 5A, and electrolysis time is 0.5 ~ 48h.
As a further improvement on the present invention, before described step S2, also comprise: carbon nano-tube macroscopic body is carried out to thermooxidizing pre-treatment in air or in other oxygen-containing atmosphere and/or carbon nano-tube macroscopic body is soaked and carries out pre-treatment in acid solution.
The invention has the beneficial effects as follows: the present invention adopts electrolysis process purifying carbon nano-tube macroscopic body, solved the conventional problem that is difficult to remove carbon nano-tube macroscopic body interior metal catalyzer with acid solution immersion carbon nano-tube macroscopic body.Technique of the present invention and method be simple and efficient, with low cost, be widely used, and proper scale is applied.
Brief description of the drawings
Fig. 1 is the structural representation of electrolyzer the first embodiment in carbon nano-tube macroscopic body purification process of the present invention;
The structural representation of electrolyzer the second embodiment in Fig. 2 carbon nano-tube macroscopic body purification process of the present invention;
Fig. 3 is carbon nano-tube macroscopic body purification process block diagram;
Fig. 4 is the transmission electron microscope photo of not purified carbon nano-tube macroscopic body;
Fig. 5 is the transmission electron microscope photo of the carbon nano-tube macroscopic body after electrolysis purifying;
Fig. 6 is the thermogravimetric analysis figure of carbon nano-tube macroscopic body after different purification process.
Embodiment
Describe the present invention below with reference to each embodiment shown in the drawings.But these embodiments do not limit the present invention, the conversion in structure, method or function that those of ordinary skill in the art makes according to these embodiments is all included in protection scope of the present invention.
In the present invention, indication carbon nano-tube macroscopic body can comprise carbon nano-tube film, carbon nanotube paper, carbon nanotube cloth, carbon nanotube lamella thing, carbon nano-tube fibre and cloth thereof.Normally, such carbon nano-tube macroscopic body can become the modes such as embrane method to prepare by thermal chemical vapor deposition method, floating catalytic chemical Vapor deposition process, carbon nanotube powders dispersion liquid spin-coating film method and suction filtration, but the carbon nano-tube macroscopic body no matter by which kind of preparation method obtaining, its inside all can kish catalyzer, and the present invention adopts electrolysis process purifying carbon nano-tube macroscopic body that residual metal catalyst in carbon nano-tube macroscopic body is removed.
Shown in ginseng Fig. 1, for the structural representation of the first embodiment electrolyzer in carbon nano-tube macroscopic body purification process of the present invention, electrolyzer 10 comprises electrolyzer, the positive electrode 11 being connected with DC power anode and the negative electrode 12 being connected with DC power cathode are set in electrolyzer, in electrolyzer, are injected with ionogen 13.Ionogen 13 is acid solution, what adopt due to ionogen 13 is acid solution, and correspondingly two electrodes of negative and positive preferably adopt noble electrode for example, to prevent the corrosion of acid solution to it: Graphite Electrodes or other inert metal electrode, in present embodiment, preferably graphite is as electrode materials.Positive electrode 11 be shaped as tabular, carbon nano-tube macroscopic body 20 is directly fitted on flat positive electrode 11, the shape of negative electrode 12 can be selected arbitrarily.
Shown in ginseng Fig. 2, for the structural representation of the second embodiment electrolyzer in carbon nano-tube macroscopic body purification process of the present invention, the difference of present embodiment and the first embodiment is, in present embodiment, positive electrode 11 is shaped as pole shape, and carbon nano-tube macroscopic body 20 is placed between the non-dust cloth of two-layer cleaning and forms a kind of sandwich structure, then whole carbon nano-tube macroscopic body 20 and the sandwich structure of non-dust cloth composition are reeled layer by layer to pole shape positive electrode 11, finally wrap up with band.
Shown in ginseng Fig. 3, introduce an embodiment of carbon nano-tube macroscopic body purification process of the present invention, in the present embodiment, the method comprises the following steps:
S1, structure electrolyzer, electrolyzer comprises the yin, yang electrode and the ionogen that are positioned at electrolyzer.Two electrodes of negative and positive adopt Graphite Electrodes, and ionogen is acid solution, and preferably, acid solution can be any one or a few combination of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, oxalic acid, phenylformic acid, succinic acid, three oxygen methylsulfonic acids.In addition, before electrolysis purifying, can do some pre-treatment to reach the object of the kish impurity of more thoroughly removing in carbon nano-tube macroscopic body to carbon nano-tube macroscopic body, as carbon nano-tube macroscopic body carried out to thermooxidizing pre-treatment in air or in other oxygen-containing atmospheres, for example process 5-120min at the air atmosphere of 150-500 DEG C, the benefit of processing is like this, can in advance the kish simple substance in carbon nano-tube macroscopic body be changed into metal oxide, metal oxide more easily and acid solution react and become metal ion and be added in electrolytic solution; Or by carbon nano-tube macroscopic body dipping pretreatment in the acid solution of 20-200 DEG C, or above-mentioned two kinds of pretreatment processs are combined with.
S2, carbon nano-tube macroscopic body is attached on positive electrode, electrolysis purifying is carried out in energising.
Here, the adhering mode of carbon nano-tube macroscopic body and positive electrode has two kinds, is respectively the adhering mode in corresponding above-mentioned electrolyzer the first embodiment and the second embodiment, repeats no more here.Certainly,, in the embodiment of other replacements, also can adopt other suitable adhering mode.
The positive electrode that is attached with carbon nano-tube macroscopic body is immersed in ionogen completely, and negative electrode is immersed in ionogen too, regulates electrolyte concentration and electrolytic parameter, electrolysis is carried out in energising, voltage range when electrolysis is 0.5-30V, and range of current is 0.1-5A, and electrolysis time is 0.5-48h.In electrolytic process, by the oxidizing reaction occurring on positive electrode, iron residual in the carbon nano-tube macroscopic body adhering on positive electrode, nickel, cobalt, molybdenum, copper, zinc, magnesium and the residual metal catalyst of other possibilities are oxidized to high valence ion state by original zeroth order simple substance state, and by constantly stirring electrolyte solution, to impel now oxidized high volence metal ion to depart from and enter into electrolyte solution from carbon nano-tube macroscopic body, metal catalyst residual in carbon nano-tube macroscopic body is removed, be able to purifying.Shown in ginseng Fig. 4 and Fig. 5, for the transmission electron microscope photo of not purified carbon nano-tube macroscopic body and the carbon nano-tube macroscopic body after electrolysis process purifying of the present invention, in Fig. 4, stain particle is metal catalyst particles residual in carbon nano-tube macroscopic body, and stain particle in Fig. 5 is little, two figure contrasts can clearly find out that purification process of the present invention can be effectively by metal catalyst particles removal residual in carbon nano-tube macroscopic body, purifying carbon nano-tube macroscopic body.In addition, can be found out by the thermogravimetric analysis figure of Fig. 6, in original carbon nano-tube macroscopic body (pristine CNT), the content of metal catalyst is about 10%; After conventional acid soak is processed, the metal catalyst in carbon nano-tube macroscopic body can only be partly removed, as respectively through 10%H
2sO
4be about respectively 6% and 4% with the metal catalyst of final residual after 37%HCl immersion purification process; And through 2%H
2sO
4after electrolysis purification process, in carbon nano-tube macroscopic body, the final residual quality of metal catalyst is down to and is less than 0.6%.Therefore, its metal catalyst content is below 0.6% after electrolytic process purifying for carbon nano-tube macroscopic body, and than the method for only soaking purifying carbon nano-tube macroscopic body with acid solution of routine, purification effect of the present invention is better.
In order better to set forth the present invention, below provide the specific embodiment of some carbon nano-tube macroscopic body purification process.
Embodiment 1
Adopt the H that massfraction is 2%
2sO
4do ionogen, graphite does anodic-cathodic, and positive electrode 11 is connected with DC power anode, and negative electrode 12 is connected with DC power cathode, in the present embodiment, positive electrode 11 be shaped as tabular.Carbon nano-tube macroscopic body 20 is directly fitted on flat positive electrode 11 to the two sides of flat positive electrode 11 carbon nano-tube macroscopic body of all can fitting.The flat positive electrode of laminating carbon nano-tube macroscopic body is immersed in ionogen completely, and negative electrode is immersed in ionogen too, and direct supply voltage is adjusted to 2-4V, and electric current is adjusted to 0.2-0.5A, and electrolysis time is 12-15h.In electrolysis treatment process, ionogen is stirred, to make residual metal simple-substance catalyzer in carbon nano-tube macroscopic body be oxidized to high valence state by zeroth order, dissolve and enter in electrolyte solution with ionic species.After electrolysis, the carbon nano-tube macroscopic body after electrolysis purifying 20 is taken out from electrolyzer 10, carbon nano-tube macroscopic body 20 is cleaned 4-5 time with deionized water, then in loft drier (not shown), dry, finally obtain the carbon nano-tube macroscopic body after purifying.
Embodiment 2
Adopt the H that massfraction is 10%
2sO
4do ionogen, graphite does anodic-cathodic, and positive electrode 11 is electrically connected with DC power anode, and negative electrode 12 is electrically connected with DC power cathode, in the present embodiment, positive electrode 11 be shaped as tabular.Carbon nano-tube macroscopic body 20 is directly fitted on flat positive electrode 11 to the two sides of flat positive electrode 11 carbon nano-tube macroscopic body of all can fitting.The flat positive electrode of laminating carbon nano-tube macroscopic body is immersed in ionogen completely, and negative electrode is immersed in ionogen too, and the voltage of direct supply is adjusted to 1-3V, and electric current is adjusted to 0.1-0.3A, and electrolysis time is 3-5h.In electrolysis treatment process, ionogen is stirred, to make residual metal simple-substance catalyzer in carbon nano-tube macroscopic body be oxidized to high valence state by zeroth order, dissolve and enter in electrolyte solution with ionic species.After electrolysis, the carbon nano-tube macroscopic body after electrolysis purifying is taken out from electrolyzer 10, carbon nano-tube macroscopic body is cleaned 4-5 time with deionized water, then in loft drier, dry, finally obtain the carbon nano-tube macroscopic body after purifying.
Embodiment 3
Adopt the H that massfraction is 2%
2sO
4do ionogen, graphite does anodic-cathodic, and positive electrode 11 is electrically connected with DC power anode, and negative electrode 12 is electrically connected with DC power cathode, in the present embodiment, positive electrode 11 be shaped as pole shape.Carbon nano-tube macroscopic body 20 is placed between the non-dust cloth of two-layer cleaning and forms a kind of sandwich structure, closely be connected with bar-shaped positive electrode with one end of carbon nano-tube macroscopic body 20, then the sandwich structure of whole carbon nano-tube macroscopic body and non-dust cloth composition is reeled layer by layer to bar-shaped positive electrode 11, finally wrap up with band.The bar-shaped positive electrode of the carbon nano-tube macroscopic body of sandwich structure is immersed in ionogen completely, and negative electrode 12 is immersed in ionogen too, and the voltage of direct supply is adjusted to 2-4V, and electric current is adjusted to 0.2-0.5A, and electrolysis time is 12-15h.In electrolysis treatment process, ionogen is stirred, to make residual metal simple-substance catalyzer in carbon nano-tube macroscopic body be oxidized to high valence state by zeroth order, dissolve and enter in electrolyte solution with ionic species.After electrolysis, the carbon nano-tube macroscopic body after electrolysis purifying is taken out from electrolyzer 10, carbon nano-tube macroscopic body is cleaned 4-5 time with deionized water, then in loft drier, dry, finally just obtain the carbon nano-tube macroscopic body after purifying.
Embodiment 4
Adopt the H that massfraction is 10%
2sO
4do ionogen, graphite does anodic-cathodic, and positive electrode 11 is electrically connected with DC power anode, and negative electrode 12 is electrically connected with DC power cathode, in the present embodiment, positive electrode 11 be shaped as pole shape.Carbon nano-tube macroscopic body 20 is placed between the non-dust cloth of two-layer cleaning and forms a kind of sandwich structure, closely be connected with bar-shaped positive electrode with one end of carbon nano-tube macroscopic body 20, then the sandwich structure of whole carbon nano-tube macroscopic body and non-dust cloth composition is reeled layer by layer to bar-shaped positive electrode 11, finally wrap up with band.The bar-shaped positive electrode of the carbon nano-tube macroscopic body of sandwich structure is immersed in ionogen completely, and negative electrode 12 is immersed in ionogen too, and the voltage of direct supply is adjusted to 1-3V, and electric current is adjusted to 0.1-0.3A, and electrolysis time is 3-5h.In electrolysis treatment process, ionogen is stirred, to make residual metal simple-substance catalyzer in carbon nano-tube macroscopic body be oxidized to high valence state by zeroth order, dissolve and enter in electrolyte solution with ionic species.After electrolysis, the carbon nano-tube macroscopic body after electrolysis purifying is taken out from electrolyzer, carbon nano-tube macroscopic body is cleaned 4-5 time with deionized water, then in loft drier, dry, finally just obtain the carbon nano-tube macroscopic body after purifying.
Be to be understood that, although this specification sheets is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Listed a series of detailed description is above only illustrating for feasibility embodiment of the present invention; they are not in order to limit the scope of the invention, all do not depart from the equivalent embodiment that skill spirit of the present invention does or change and all should be included in protection scope of the present invention within.
Claims (10)
1. a purification process for carbon nano-tube macroscopic body, is characterized in that, the method comprises the following steps:
S1, structure electrolyzer, described electrolyzer comprises the yin, yang electrode and the ionogen that are positioned at electrolyzer;
S2, carbon nano-tube macroscopic body is attached on described positive electrode, electrolysis purifying is carried out in energising.
2. the purification process of carbon nano-tube macroscopic body according to claim 1, is characterized in that, the material of described yin, yang electrode is graphite or other inert metal.
3. the purification process of carbon nano-tube macroscopic body according to claim 1, is characterized in that, described yin, yang electrode be shaped as pole shape.
4. the purification process of carbon nano-tube macroscopic body according to claim 3, is characterized in that, described " carbon nano-tube macroscopic body is attached on described positive electrode " specifically comprises:
Adopt the mode of sandwich structure that carbon nano-tube macroscopic body and the stack of non-dust cloth interval are wound on the pole shape positive electrode of described electrolyzer.
5. the purification process of carbon nano-tube macroscopic body according to claim 1, is characterized in that, described yin, yang electrode be shaped as tabular.
6. the purification process of carbon nano-tube macroscopic body according to claim 5, is characterized in that, described " carbon nano-tube macroscopic body is attached on described positive electrode " specifically comprises:
Described carbon nano-tube macroscopic body is directly fitted on the tabular positive electrode of described electrolyzer.
7. the purification process of carbon nano-tube macroscopic body according to claim 1, it is characterized in that, described ionogen is acid solution, and described acid solution is selected from one or more the combination in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, oxalic acid, phenylformic acid, succinic acid, three oxygen methylsulfonic acids.
8. the purification process of carbon nano-tube macroscopic body according to claim 1, is characterized in that, step S2 also comprises:
In the purge process of carbon nano-tube macroscopic body, constantly stir described ionogen.
9. the purification process of carbon nano-tube macroscopic body according to claim 1, is characterized in that, voltage range when described " electrolysis purifying is carried out in energising " is 0.5 ~ 30V, and range of current is 0.1 ~ 5A, and electrolysis time is 0.5 ~ 48h.
10. the purification process of carbon nano-tube macroscopic body according to claim 1, it is characterized in that, before described step S2, also comprise: carbon nano-tube macroscopic body is carried out to thermooxidizing pre-treatment in air or in other oxygen-containing atmosphere and/or carbon nano-tube macroscopic body is soaked and carries out pre-treatment in acid solution.
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