CN101327415A - Dispersing method of polyalcohol dispersing agent of one-dimensional carbon nano material - Google Patents
Dispersing method of polyalcohol dispersing agent of one-dimensional carbon nano material Download PDFInfo
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- CN101327415A CN101327415A CNA2008100409592A CN200810040959A CN101327415A CN 101327415 A CN101327415 A CN 101327415A CN A2008100409592 A CNA2008100409592 A CN A2008100409592A CN 200810040959 A CN200810040959 A CN 200810040959A CN 101327415 A CN101327415 A CN 101327415A
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Abstract
The present invention relates to a carbon nano-material polymer dispersant and a dispersing method thereof. The carbon nano-material polymer dispersant is characterized in that the carbon nano-material polymer dispersant is alkyl fibrin or a derivative of the alkyl fibrin; a general structural formula is shown at right; in the formula, R is equal to H, CmH2m plus 1 or CpH2pOH, and n, p and m are any positive integer; the dispersing method is characterized in that a one-dimensional carbon nano-material surface is functionalized by forming the non covalent bond combination between a main chain of the polymer dispersant and the one-dimensional carbon nano-material surface; then the surface functionalized one-dimensional carbon nano-material is dispersed in solvent by the dispersant, so as to disperse the one-dimensional carbon nano-material in the solvent.
Description
Technical field
The present invention relates to a kind of dispersant and process for dispersing of one-dimensional carbon nano material, relate in particular to a kind of polymeric dispersant of one-dimensional carbon nano material, this polymeric dispersant is used for disperseing one-dimensional carbon nano material at solvent.Method belongs to nano material and field of nanocomposite materials.
Background technology
One-dimensional carbon nano material becomes the focus of Recent study and application with its huge draw ratio and good rerum natura.Wherein, CNT can be regarded the tubular structure that is formed through coiling by Graphene as, roll into one with good electricity, mechanics and thermal property, and caused worldwide very big concern (S.Reich, C.Thomsen, J.Maultzsch.Carbon Nanotubes:Basic Concepts and PhysicalProperties, 2004, WILEY-VCH Verlag GmbH﹠amp; KGaA).The potential application relevant with one-dimensional carbon nano material almost related to modern scientific research and aspect of social life, all shows good prospects for application as fields such as microelectronics, composite, sensor, probe, the energy, biologies.
The preparation method of CNT has multiple, and main have arc discharge method, laser evaporation method and a chemical vapour deposition technique etc.Wherein, chemical vapour deposition technique is good with its controllability, easy large-scale production etc. becomes the main mode that current CNT is commercially produced, and reached so far to produce tens tons scale (A.Thayer.Carbon Nanotubes By The Metric Ton.Chem.﹠amp per year; Eng.News, 2007,85:29).
But the application of CNT still is faced with huge technical barrier, is dissolved in any known solvent hardly as CNT.In addition, CNT has very big specific area and powerful to each other Van der Waals force, and the big L/D ratio that one-dimensional material had (often surpassing 1000), make easy bunchy of CNT or winding mutually, be difficult to disperse, thereby greatly limited the application of CNT, therefore, development just becomes an emphasis of CNT research and application to effective process for dispersing of CNT.
It is reported, wherein a kind of method that CNT is disperseed is that chemical modification is carried out on its surface, make it form combining on the covalent bond basis with other molecule, thereby reach the purpose (D.Tasis of dispersion, N.Tagmatarchis, A.Bianco, M.Prato.Chem Rev.2006,106 (3): 1105-36.).The shortcoming of this method is the body construction of its meeting heavy damage CNT and good physical property.From this aspect, utilize CNT and other intermolecular physical action that it is disperseed to have bigger meaning, thereby also become the important directions that the research CNT disperses.As having a large amount of research and utilization surfactants, nucleotides etc. that CNT is disperseed.But the dispersant of these CNTs that it has been found that still exists various problems, and not high as dispersibility, nucleotides costs an arm and a leg, and the consumption of surfactant is often very big, can greatly influence the performance of subsequent products etc.
In sum, the good CNT dispersant of exploitation has extremely important scientific research meaning and practical value.
Summary of the invention
The object of the present invention is to provide a kind of high-efficiency polymer dispersant to one-dimensional carbon nano material, and a kind of process for dispersing of one-dimensional carbon nano material.The design of invention is as follows: by form very strong physical action between one-dimensional carbon nano material and polymeric dispersant main chain, make this polymer be attached to the one-dimensional carbon nano material surface, can not destroy the body construction of one-dimensional carbon nano material simultaneously again; Simultaneously, the mutual repulsion that the function group that is had by polymer itself is asked makes that the one-dimensional carbon nano material after the functionalization is disconnected from each other, reaches the purpose that one-dimensional carbon nano material is disperseed.In the practical operation, can dispersant and one-dimensional carbon nano material be mixed, as grinding, ball milling, ultrasonic etc. by the whole bag of tricks.In theory, the one-dimensional carbon nano material of this polymers functionization can be dissolved in any solvent.By research, find that this method has a plurality of significant advantages: (1) can be so that on the basis that one-dimensional carbon nano material disperses, keep its basic structure, thereby help bringing into play physical characteristics such as the significant mechanics of one-dimensional carbon nano material, electricity, optics, calorifics; (2) on the other hand, be attached to the polymer on one-dimensional carbon nano material surface, its functional group can be further reacts with other molecule; (3) the needed polymeric dispersant of the one-dimensional carbon nano material of discrete units quality is few, and the mass ratio of one-dimensional carbon nano material and polymeric dispersant can reach more than 5.
The invention provides a kind of polymeric dispersant of one-dimensional carbon nano material, it is characterized in that described polymeric dispersant is the derivative of alkylcellulose or alkylcellulose, general formula of molecular structure is:
R=H, C in the formula
mH
2m+1Perhaps C
pH
2pOH
N, p, m are any positive integer, can be infinity in theory;
Described dispersant comprises 6 functional groups at least, and each functional group is any class in the following three class groups:
R=H, C
mH
2m+1Perhaps C
pH
2pOH
P, m are any positive integer, can be infinity in theory;
Described one-dimensional carbon nano material is SWCN, multi-walled carbon nano-tubes or carbon nano-fiber, with and above-mentioned any the two or three's mixture;
Described dispersant is the derivative of alkylcellulose or alkylcellulose;
The derivative of described alkylcellulose or alkylcellulose is methylcellulose, CMC, hydroxypropyl methylcellulose, hydroxypropyl methylcellulose, HEMC, hydroxyethylcellulose, ethyl cellulose, methyl hydroxyethylcellulose, hydroxypropyl cellulose or hydroxymethyl-propyl cellulose etc.
Described process for dispersing is by forming the combination of non-covalent bond between the main chain of polymeric dispersant and one-dimensional carbon nano material surface, one-dimensional carbon nano material is surface-functionalized, one-dimensional carbon nano material after surface-functionalized then is scattered in the solvent by the functional group of dispersant, thereby realizes the dispersion of one-dimensional carbon nano material in solvent.The strong physical action that forms makes the fibrous carbon nano-material surface topped by dispersant.
Disperseing the solvent of one-dimensional carbon nano material is acetone, chlorobenzene, water, acetate, acetonitrile, benzene, aniline, benzonitrile, toluene, trimethylbenzene, phenmethylol, bromobenzene, ethylbenzene, nitrobenzene, iodobenzene, 1,3,5-trimethylbenzene, meta-xylene, ortho-xylene, paraxylene, o-dichlorohenzene, m-dichlorobenzene, 1,2,4-trichloro-benzenes, paracide bromofom, carbon disulfide, carbon tetrachloride, cyclohexylamine, decahydronaphthalenes, methylene bromide, dimethoxymethane, oxirane, carrene, nitromethane, octane, pentane, 1,1,1-trichloroethanes, 1,1,2-trichloroethanes, 1,1,2,2 tetrachloroethanes, N, the N dimethyl formamide, ethamine, tetramethylethylenediamine, triethylamine, formaldehyde, formic acid, heptane, hexane, methylamine, methylene bromide, picoline, morpholine, naphthalene, phenol, pyrimidine, the pyrroles, pyrrolidines, quinoline, tetrachloro-ethylene, oxolane, the N-methyl pyrrolidone, tetrahydroquinoline, tetralin, thiophene, trichloro-ethylene or ionic liquid etc.The foundation of selective solvent at first is to dissolve dispersant (derivative of alkylcellulose or alkylcellulose), secondly is that the active force of solvent and dispersant should be less than the active force between dispersant and one-dimensional carbon nano material.
The invention provides in a word on a kind of new, non-covalent bond basis, in organic and inorganic solvent, disperse one-dimensional carbon nano material dispersant process for dispersing.By the physical action between one-dimensional carbon nano material surface and a kind of polymeric dispersant (derivative of alkylcellulose and alkylcellulose thereof), realize functionalization to the one-dimensional carbon nano material surface; This polymeric dispersant contains at least one functional group, and this functional group makes the one-dimensional carbon nano material after surface-functionalized be scattered in all kinds of solvents.
Description of drawings
Fig. 1. use and do not use the one-dimensional carbon nano material solution behind three months of dispersant.From left to right be followed successively by: acetone/SWCN (0.5mg/mL, SWCN/solvent acetone); Hydroxypropyl methylcellulose/acetone/SWCN (0.5mg/mL, SWCN/solvent acetone); Hydroxypropyl methylcellulose/acetone/single wall carbon nanotube (5mg/mL, SWCN/solvent acetone); Hydroxypropyl methylcellulose/acetone/multi-walled carbon nano-tubes (0.5mg/mL, SWCN/solvent acetone);
Fig. 2. 1. ultraviolet-visible light-the infrared absorption curve of one-dimensional carbon nano material is SWNTs-Acetone: acetone/SWCN (0.5mg/mL, SWCN/solvent acetone); 2. be 1% NaTDC/SWCN (0.5mg/mL, SWCN/aqueous solvent); 3. be SWNTs-Acetone-MC: hydroxypropyl methylcellulose/acetone/SWCN (0.5mg/mL, SWCN/solvent acetone).
The specific embodiment
By the elaboration of following specific embodiment, further specify substantive distinguishing features of the present invention and obvious improvement, but the present invention only is confined to embodiment by no means.
Embodiment 1
The one-dimensional carbon nano material of 5mg (this sentences SWCN as an example) mixes with 10mL acetone, with the ultrasonic 1h of the ultrasonic device of probe-type, adds the 9mg hydroxypropyl methylcellulose, ultrasonic again 1h.The liquid of Xing Chenging is the solution of a black, no obvious sediment like this, through 9, after 000Xg is centrifugal, can (show as Fig. 1) more than 3 months by stable existence.Simultaneously, also prepared the ultrasonic liquid of acetone/CNT that does not add hydroxypropyl methylcellulose and compared, to show the dispersion effect to CNT (showing) of hydroxypropyl methylcellulose as Fig. 1.The Cmax of the CNT that hydroxypropyl methylcellulose/acetone/SWCN ultrasonic method forms can reach the SWCN (showing as Fig. 1) that disperses 5mg in unit solvent.Be noted that the used one-dimensional carbon nano material of present embodiment both can be SWCN, also can be multi-walled carbon nano-tubes and carbon nano-fiber.Simultaneously, above-mentioned one-dimensional carbon nano material also is not limited to specific material supplier.
In order to further specify the dispersibility of hydroxypropyl methylcellulose, further measured the ultraviolet-visible light-infrared absorption spectroscopy (showing) of hydroxypropyl methylcellulose/acetone/SWCN solution with method for preparing as Fig. 2 to one-dimensional carbon nano material.Simultaneously, we have also prepared the ultrasonic solution of nanotube with the NaTDC that CNT is had a fine dispersion ability of generally acknowledging, compare.The ultraviolet-visible light of carbon nano-tube solution-infrared absorption spectroscopy principle is based on following characteristics (J.Chen, M.Hamon, H.Hu, Y.Chen, A.Rao, P.Eklund, and R.Haddon.Science, 1998,282:95.): if SWCN has good dispersiveness in solution, exist, then because the special electronic structure characteristics (valence band and conduction band can form special van hove singularity structure) of SWCN with the form of single or tuftlet, can cause forming strong absorption, and form some sharp-pointed peaks at ultraviolet-visible light-infrared region.As can be seen from Fig. 2, the SWCN spectrum that in acetone/Gonak, forms (curve 3), there is a large amount of absworption peaks, simultaneously, its absorption intensity is higher than the absorption intensity (curve 2) of the SWCN of deoxycholic acid sodium solution formation far away, thereby has proved the fine dispersion ability of hydroxypropyl methylcellulose to SWCN.Corresponding is, does not have the SWCN in the acetone soln of hydroxypropyl methylcellulose almost not have tangible absworption peak to exist.
Simultaneously, in order to study the dispersibility of hydroxypropyl methylcellulose quantitatively to one-dimensional carbon nano material, we also utilize the Beer-Lambert principle, as benchmark, measured the dispersion efficiency of hydroxypropyl methylcellulose with the zone of the no obvious absorption peaks in 924nm place in ultraviolet-visible light-infrared absorption spectroscopy to SWCN.The result shows that its dispersion efficiency can reach 97%, far above 5.6% under 64% and the single acetone soln condition of deoxycholic acid sodium solution.
The dispersant that uses is other alkylcellulose except that hydroxypropyl methylcellulose or the derivative of alkylcellulose, makes the similar results that solvent also can obtain embodiment 1 and embodiment 2 as methylcellulose CMC, HEMC, hydroxyethylcellulose, ethyl cellulose, methyl hydroxyethylcellulose etc. with acetone.
Embodiment 4
The alkylcellulose or derivatives thereof is scattered in the solvent except that acetone, as chlorobenzene, water, acetate, acetonitrile, benzene, aniline, benzonitrile, toluene, trimethylbenzene, phenmethylol, bromobenzene, ethylbenzene, nitrobenzene, iodobenzene, 1,3, the 5-trimethylbenzene, meta-xylene, ortho-xylene, paraxylene, o-dichlorohenzene, m-dichlorobenzene, 1,2, the 4-trichloro-benzenes, the paracide bromofom, carbon disulfide, carbon tetrachloride, cyclohexylamine, decahydronaphthalenes, methylene bromide, dimethoxymethane, oxirane, carrene, nitromethane, octane, pentane, 1,1, the 1-trichloroethanes, 1,1, the 2-trichloroethanes, 1,1,2,2 tetrachloroethanes, N, the N dimethyl formamide, ethamine, tetramethylethylenediamine, triethylamine, formaldehyde, formic acid, heptane, hexane, methylamine, methylene bromide, picoline, morpholine, naphthalene, phenol, pyrimidine, the pyrroles, pyrrolidines, quinoline, tetrachloro-ethylene, oxolane, the N-methyl pyrrolidone, tetrahydroquinoline, tetralin, thiophene, trichloro-ethylene or ionic liquid, also obtain similar results.
Claims (6)
1, a kind of polymeric dispersant of one-dimensional carbon nano material is characterized in that described polymeric dispersant is the derivative of alkylcellulose or alkylcellulose, and general formula of molecular structure is:
R=H, C in the formula
mH
2m+1Perhaps C
pH
2pOH
N, p, any positive integer of m=.
2, by the polymeric dispersant of the described one-dimensional carbon nano material of claim 1, it is characterized in that described dispersant comprises 6 functional groups at least, each functional group is any class in the following three class groups:
R=H, C
mH
2m+1Perhaps C
pH
2pOH
P, m are any positive integer.
3, by the polymeric dispersant of the described one-dimensional carbon nano material of claim 1, it is characterized in that described one-dimensional carbon nano material is SWCN, multi-walled carbon nano-tubes or carbon nano-fiber, and any the two or three's mixture.
4, by the polymeric dispersant of the described one-dimensional carbon nano material of claim 1, the derivative that it is characterized in that described alkylcellulose or alkylcellulose is methylcellulose, CMC, hydroxypropyl methylcellulose, hydroxypropyl methylcellulose, HEMC, hydroxyethylcellulose, ethyl cellulose, methyl hydroxyethylcellulose, hydroxypropyl cellulose or hydroxymethyl-propyl cellulose.
5, use the method for disperseing one-dimensional carbon nano material as the polymeric dispersant of claim 1 or 4 described one-dimensional carbon nano materials, it is characterized in that described process for dispersing is the combination that forms non-covalent bond between main chain by polymeric dispersant and one-dimensional carbon nano material surface, one-dimensional carbon nano material is surface-functionalized, one-dimensional carbon nano material after surface-functionalized then is scattered in the solvent by the functional group of dispersant, thereby realizes the dispersion of one-dimensional carbon nano material in solvent.
6, method by the described dispersion one-dimensional carbon nano material of claim 5 is characterized in that described solvent is an acetone, chlorobenzene, water, acetate, acetonitrile, benzene, aniline, benzonitrile, toluene, trimethylbenzene, phenmethylol, bromobenzene, ethylbenzene, nitrobenzene, iodobenzene, 1,3, the 5-trimethylbenzene, meta-xylene, ortho-xylene, paraxylene, o-dichlorohenzene, m-dichlorobenzene, 1,2,4-trichloro-benzenes, paracide bromofom, carbon disulfide, carbon tetrachloride, cyclohexylamine, decahydronaphthalenes, methylene bromide, dimethoxymethane, oxirane, carrene, nitromethane, octane, pentane, 1,1,1-trichloroethanes, 1,1,2-trichloroethanes, 1,1,2,2 tetrachloroethanes, N, the N dimethyl formamide, ethamine, tetramethylethylenediamine, triethylamine, formaldehyde, formic acid, heptane, hexane, methylamine, methylene bromide, picoline, morpholine, naphthalene, phenol, pyrimidine, the pyrroles, pyrrolidines, quinoline, tetrachloro-ethylene, oxolane, N-methyl pyrrolidone, tetrahydroquinoline, tetralin, thiophene, trichloro-ethylene or ionic liquid.
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| CN102464914A (en) * | 2010-11-04 | 2012-05-23 | 索尼公司 | Conductive ink, method of preparing the same, and method of preparing transparent conductive film |
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| CN106587013A (en) * | 2016-12-06 | 2017-04-26 | 江南大学 | Switch-type carbon nanotube dispersant |
| US20180086932A1 (en) * | 2011-04-22 | 2018-03-29 | Mark C. Hersam | Methods for Preparation of Concentrated Graphene Ink Compositions and Related Composite Materials |
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| CN102464914A (en) * | 2010-11-04 | 2012-05-23 | 索尼公司 | Conductive ink, method of preparing the same, and method of preparing transparent conductive film |
| US20180086932A1 (en) * | 2011-04-22 | 2018-03-29 | Mark C. Hersam | Methods for Preparation of Concentrated Graphene Ink Compositions and Related Composite Materials |
| US10676629B2 (en) * | 2011-04-22 | 2020-06-09 | Northwestern University | Methods for preparation of concentrated graphene ink compositions and related composite materials |
| CN103147355A (en) * | 2013-02-26 | 2013-06-12 | 中南林业科技大学 | Preparation method of biomass nano fiber conductive paper |
| CN103147355B (en) * | 2013-02-26 | 2015-12-23 | 中南林业科技大学 | A kind of preparation method of biomass nano fiber conductive paper |
| CN103721624A (en) * | 2013-11-18 | 2014-04-16 | 大连创达技术交易市场有限公司 | Surfactant composition |
| CN109642220A (en) * | 2016-08-29 | 2019-04-16 | 国立研究开发法人产业技术综合研究所 | Glucose sensor reagent, glucose sensor, the manufacturing method of glucose sensor and Glucose Measure device |
| CN109642220B (en) * | 2016-08-29 | 2023-09-15 | 国立研究开发法人产业技术综合研究所 | Reagent for glucose sensor, method for producing glucose sensor, and glucose measuring device |
| CN106587013A (en) * | 2016-12-06 | 2017-04-26 | 江南大学 | Switch-type carbon nanotube dispersant |
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