CN103073930A - Preparation method and application of alkylated functional graphene - Google Patents
Preparation method and application of alkylated functional graphene Download PDFInfo
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Abstract
The invention relates to a preparation method and an application of alkylated functional graphene. The preparation method comprises the steps of dispersing graphene oxide prepared by an improved Hummers method into a micromolecular ketone compound and water mixed solution (0.1-5mg/mL) in different proportions according to a stoichiometric ratio, conducting ultrasonic oscillation and stripping for 1-8h at a room temperature, separating, and obtaining the functional graphene. The functional graphene and PA66 (Poly A 66) as raw materials, a graphene/PA66 nano composite is obtained by a fusion blending method, and the weight percentage of the functional graphene in the composite is 0.01-1%. The preparation method of the modified graphene is simple, convenient and quick, and the dispersity of the graphene in a polymeric matrix can be improved significantly. The invention further discloses a preparation method of the graphene/PA666 nano composite. The mechanical property, antistatic property, moisture absorption and thermal stability of the prepared nano composite can be improved obviously.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of alkylation function Graphene, belong to nanometer novel material and Application Areas.
Background technology
Be accompanied by the fast development of making rapid progress of science and technology, traditional single-material more and more can not satisfy the demand of industrial circle, the demand of society has proposed harsher standard to the requirement of material, and therefore, this also requires the scientific research personnel to develop the material of the more excellent or new capability of performance.Nylon 66(PA66) use starts from [Deng Rusheng in 1956 as engineering plastics, Wei Yuanfang, Chen Buning. polyamide resin and application thereof, Beijing, chemical press, 2002:1], it is owing to many merits is widely used in automobile, communications and transportation and the field such as electric, but have that water-absorbent is large, acid resistance is poor, weathering resistance is not good and the shortcoming such as suction after strain, thereby limited its Application Areas.Nano composite material is because thereby the adding of nano material can change the over-all properties that its micro interface promotes material, and therefore, development of new possesses the high-performance nano matrix material, widens the Application Areas of material to satisfy the material application demand of future development.
Graphene is in New Two Dimensional nano material [the K. S. Novoselov of the carbon atom process sp2 hydridization formation of found monoatomic layer in 2004, A. K. Geim, et al. Science, 2004,306 (5696): 666-669], since its unique structure and performance, the technological revolution of having risen material circle.The extremely excellent over-all properties of Graphene is given Graphene is used for matrix material as the nanometer reinforcing filler unlimited potentiality, have in recent years many bibliographical informations, make Graphene play good reinforced effects to resin matrix, what just require that Graphene can be good is scattered in the resin matrix, there is good interface to be combined with resin matrix, yet, because the characteristic of this body structure of Graphene, it is very easily reunited, be difficult to be dispersed in the resin matrix.[the S. Stankovich such as Ruffo, D.A. Dikin, G.H.B. Dommett, et al. Nature, 442 (2006) 282-286] take the lead in having prepared Graphene-pipe/polyhenylethylene nano composite conducting material, they use phenyl isocyanate that graphene oxide is carried out functionalization, then it are dispersed in the polystyrene solution, add dimethylhydrazine and reduce, obtained to possess the nano composite material of electroconductibility.Subsequently, they are [S. Stankovich, R.D. Piner, X. Chen, et al. Journal of Materials Chemistry, 16 (2006) 155-158] utilize poly (sodium 4-styrenesulfonate) (PSS) that graphene oxide is carried out modification, by the interaction of the π between them-π key, improved the agglomeration of Graphene.Subsequently, [the T. Ramanathan such as Brinson, A.A. Abdala, S. Stankovich, et al. Nature Nanotechnology 3 (2008) 327-331] studied the performance of Graphene-polyacrylonitrile and Graphene-polymethyl methacrylate nano matrix material, found that, behind the Graphene of adding 1% and 0.05%, the second-order transition temperature of 2 individual system and modulus, tensile strength and heat decomposition temperature all are largely increased in above-mentioned 2 individual system.In addition, can also be by atom transfer radical polymerization (ATRP) initiator be bonded on the Graphene, ATRP reaction subsequently makes polystyrene chain be grafted to Graphene, the polymkeric substance of grafting can significantly improve the dissolving of Graphene in organic solvent, and the polymeric matrix behind the introducing Graphene, mechanical property has obtained larger lifting.
Along with deepening continuously of Graphene/polymer composites research, its range of application and the performance boost that brings will further be developed, but the bad dispersibility of Graphene in resin matrix, a little less than being combined in the interface between the polymkeric substance, all the time be not well solved, thereby the various excellent properties that affected Graphene itself can not obtain maximum performance.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application thereof of function Graphene, it is controlled that described function Graphene has alkylation, with advantages such as the polymer resin matrix consistency are good, simultaneously, described PA66 based nano composite material has outstanding mechanical property, static resistance, moisture absorption and thermostability energy.The preparation method of this new function Graphene is simple, and reliable, cost is low, and the PA66 based nano composite material can prepare the matrix material masterbatch of high density.
Its surface of the function Graphene that the present invention relates to is upper with chemical bonding mode absorbing fats family ketone compounds, and the alkyl chain length of absorption is controlled; The PA66 based nano composite material that wherein obtains, function Graphene content concn is higher, is uniformly dispersed, and can be used as masterbatch.
The preparation method of a kind of function Graphene that the present invention proposes, concrete steps are as follows:
(1) obtain graphene oxide by improving the Hummers method, its mono-layer graphite oxide alkene content accounts for more than 90%;
(2) graphene oxide that step (1) is obtained is scattered in ketone micromolecular compound and water mixed solution or ketone micromolecular compound and the alcohol mixed solution by stoichiometric ratio, ultrasonic lift-off processing 1 ~ 8h under 40kHz power 300W separates obtaining the controlled function graphene dispersing solution of alkylation degree;
(3) the function graphene dispersing solution that step (2) is obtained places ethanol-water solution, and washing is also centrifugal under 10000 rev/mins of speed, at last with the throw out lyophilize, prepares the function Graphene.
Among the present invention, graphene oxide is scattered in the ketone micromolecular compound by stoichiometry described in the step (2), and its stoichiometry is 0.1～10mg/mL.
Among the present invention, the ketone micromolecular compound is the alkanones compound described in the step (2).
Among the present invention, described alkanones compound is more than one in ketone, 2-heptanone, methyln-hexyl ketone, methyl n-heptyl ketone or 2-ten triketones of acetone, butanone, 2 pentanone, 2-.
Among the present invention, the volume ratio of ketone micromolecular compound and water or ethanol is 1:0～10:1 described in the step (2).
Among the present invention, the alkanones compound is adsorbed in the lip-deep defect structure of graphene oxide or topological framework in the chemical bonding mode in the alkylation function Graphene that makes in the step (2), and the alkanones compounds content of chemisorption is 0.1～1%.
The alkylation function Graphene that the inventive method obtains is as the application of polymer matrix composite filler.
Among the present invention, alkylation function Graphene is as the application of function Graphene/PA66 based nano composite material, and concrete steps are as follows:
(1) with the aqueous solution of alkylation function Graphene and 50% nylon salt by weight for 1:10 mixes, supersound process makes function Graphene/PA66 masterbatch by situ aggregation method.
(2) the function Graphene that step (1) is obtained/PA66 masterbatch and PA66 resin mix by high speed disintegrator, and wherein: the weight ratio of function Graphene and PA66 resin is: (0.1～2): (98～99.9); Then extrude the PA66 based nano composite material that obtains to contain the function Graphene through melt blending.
Compared with prior art, the preparation method of the preparation method of Novel alkyl function graphite provided by the invention and PA66 based nano composite material thereof has following several having a few:
1. the preparation method of the Novel alkyl function Graphene that the present invention relates to belongs to single stage method, and is simple, and used solvent can reclaim, and not only greatly reduces cost but also avoids environmental pollution; On the other hand, higher by standby its alkyl modified degree of function Graphene of this legal system.
2. the lip-deep fatty carbon chain of alkylation function Graphene of preparation is to be adsorbed in the Graphene surface in the chemical bonding mode, and this is so that the chemical stability lifting of function Graphene.
3. the alkylation function Graphene and the PA66 resin matrix that obtain have good consistency, have greatly improved the interface combination degree between Nano filling and polymkeric substance, thereby can give play to this excellent properties in matrix material of Graphene.
4. the present invention adopts situ aggregation method to prepare the function Graphene of high density content/PA66 masterbatch, but this has further improved the processed-type that the later stage prepares matrix material, and the more existing PA66 matrix material of the matrix material that makes has more outstanding over-all properties, particularly mechanical property.
Description of drawings
Fig. 1 is the FTIR spectrogram of alkylation function Graphene of the present invention, wherein: a, graphene oxide; B, the function Graphene of acetone treatment (embodiment 1); C, the function Graphene (embodiment 2) that 2 pentanone is processed; D, the function Graphene (embodiment 4) that methyl n-heptyl ketone is processed; E, the function Graphene (embodiment 6) that 2-ten triketones are processed.
Fig. 2 is the contact angle photo of alkylation function graphene powder of the present invention, wherein: a, graphene oxide; B, the function Graphene of acetone treatment (embodiment 1); C, the function Graphene (embodiment 2) that 2 pentanone is processed; D, the function Graphene (embodiment 5) that methyln-hexyl ketone is processed; E, the function Graphene (embodiment 4) that methyl n-heptyl ketone is processed; F, the function Graphene (embodiment 6) that 2-ten triketones are processed.
Fig. 3 is the SEM spectrogram of function Graphene of the present invention/PA66 based nano composite material, wherein: a, graphene oxide; B, alkylation function Graphene (embodiment 1); C, graphene oxide/PA66 based composites; D, 1% function Graphene/PA66 based composites (embodiment 1).
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1: 0.5g is dispersed in 50mL acetone-distilled water (acetone and water are 10:1 by volume) by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 3 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 10:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 10% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:5 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 2% function Graphene.
Embodiment 2: 0.8g is dispersed in 100mL2-pentanone-distilled water (2 pentanone and water are 5:1 by volume) by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 1 hour, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 10:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 10% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:10 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 1% function Graphene.
Embodiment 3: 0.5g is dispersed in the 100mL2-heptanone by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 5 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 20:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 5% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:5 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 1% function Graphene.
Embodiment 4: 0.3g is dispersed in the 100mL2-nonanone by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 8 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 10:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 10% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 3:10 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 1.5% function Graphene.
Embodiment 5: 0.1g is dispersed in the 100mL2-octanone by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 8 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 20:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 5% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:10 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 0.5% function Graphene.
Embodiment 6: 0.03g is dispersed in 100mL2-ten triketones by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 6 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 20:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 5% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:20 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 0.25% function Graphene.
Embodiment 7: 0.01g is dispersed in 100mL acetone/2-ten triketone solution (acetone and 2-ten triketones are 4:1 by volume) by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 2 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 20:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 5% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:25 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 0.2% function Graphene.
Embodiment 8: 0.2g is dispersed in 100mL acetone/2-heptanone solution (acetone and 2-heptanone are 1:1 by volume) by the standby mono-layer graphite oxide alkene of Hummers legal system, ultrasonic 2 hours, obtain the function graphene dispersing solution, then dispersion liquid is placed ethanol-water solution, repeated multiple times washing is also centrifugal under 10000 rev/mins of speed, with the throw out lyophilize, prepare alkylation function Graphene at last.Prepare the aqueous solution of 50% nylon salt, by weight 20:1 alkylation function Graphene is added wherein, ultrasonic 1h, make 5% function Graphene/PA66 masterbatch by situ aggregation method, then, the function Graphene of above-mentioned preparation/PA66 masterbatch and PA66 resin are mixed by high speed disintegrator for 1:50 in mass ratio, extrude through melt blending then that to obtain weight content be the PA66 based nano composite material of 0.1% function Graphene.
Claims (8)
1. the preparation method of an alkylation function Graphene is characterized in that concrete steps are as follows:
(1) obtain graphene oxide by improving the Hummers method, its mono-layer graphite oxide alkene content accounts for more than 90%;
(2) graphene oxide that step (1) is obtained is scattered in ketone micromolecular compound and water mixed solution or ketone micromolecular compound and the alcohol mixed solution by stoichiometric ratio, ultrasonic lift-off processing 1 ~ 8h under 40kHz power 300W separates obtaining the controlled function graphene dispersing solution of alkylation degree;
(3) the function graphene dispersing solution that step (2) is obtained places ethanol-water solution, and washing is also centrifugal under 10000 rev/mins of speed, at last with the throw out lyophilize, prepares the function Graphene.
2. the preparation method of alkylation function Graphene according to claim 1 is characterized in that graphene oxide is scattered in the ketone micromolecular compound by stoichiometry described in the step (2), and its stoichiometry is 0.1～10mg/mL.
3. the preparation method of alkylation function Graphene according to claim 1 is characterized in that the ketone micromolecular compound is the alkanones compound described in the step (2).
4. the preparation method of alkylation function Graphene according to claim 3 is characterized in that described alkanones
Small moleculesCompound is the alkanones compound, comprises more than one in ketone, 2-heptanone, methyln-hexyl ketone, methyl n-heptyl ketone or 2-ten triketones of acetone, butanone, 2 pentanone, 2-.
5. the preparation method of alkylation function Graphene according to claim 1 is characterized in that the volume ratio of ketone micromolecular compound described in the step (2) and water or ethanol is 1:0～10:1.
6. the preparation method of alkylation function Graphene according to claim 1, it is characterized in that the alkylation function Graphene alkanones compound that makes in the step (2) is adsorbed in the lip-deep defect structure of graphene oxide or topological framework in the chemical bonding mode, the alkanones compounds content of chemisorption is 0.1～1%.
One kind as claimed in claim 1 the alkylation function Graphene that obtains of preparation method as the application of polymer matrix composite filler.
8. application according to claim 7 is characterized in that alkylation function Graphene as the application of function Graphene/PA66 based nano composite material, and concrete steps are as follows:
(1) with the aqueous solution of alkylation function Graphene and 50% nylon salt by weight for 1:10 mixes, supersound process makes function Graphene/PA66 masterbatch by situ aggregation method;
(2) the function Graphene that step (1) is obtained/PA66 masterbatch and PA66 resin mix by high speed disintegrator, and wherein: the weight ratio of function Graphene and PA66 resin is: (0.1～2): (98～99.9); Then extrude the PA66 based nano composite material that obtains to contain the function Graphene through melt blending.
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| CN103450674A (en) * | 2013-09-11 | 2013-12-18 | 上海大学 | Nylon 6/graphene nanometer composite material with high thermal conductivity and preparation method thereof |
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