CN103232637B - Graphene/polypropylene conductive nano composite material and preparation method thereof - Google Patents
Graphene/polypropylene conductive nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a graphene/polypropylene conductive nano composite material and a preparation method thereof, belonging to the technical field of polymer nano composite materials. On the basis of 100 parts by mass, the graphene/polypropylene conductive nano composite material contains 92.5-97.5 parts by mass of polypropylene (as a base), 1-3 parts by mass of graphene (as a conductive filler) and 1.5-4.5 parts by mass of maleic anhydride grafted polypropylene (for promoting dispersion of the graphene); and the graphene/polypropylene conductive nano composite material is prepared by solution blending and hot pressing. A series of graphene/polypropylene conductive nano composite materials in different proportions can be obtained by changing the mass percent of the graphene in the composite system. The prepared graphene/polypropylene conductive nano composite material can be used in the fields of conductive materials, electromagnetic shielding materials, antistatic materials and the like.
Description
Technical field
The invention belongs to polymer nanocomposites technical field, be specifically related to a kind of Graphene/polypropyleconductive conductive nano composite material and preparation method thereof.
Background technology
Graphene is found to be in 2004 first, and the method utilizing micromechanics to be separated by K.S.Novoselov with A.K.Geim etc. has prepared stable sheet Graphene.Since then, in nearest several years, the research about Graphene obtains comprehensive attention.Graphene is by the two-dirnentional structure of monolayer carbon atom packing, shows as hexagonal honeycomb, and it has large specific surface area, excellent electricity, mechanics, thermal property etc., and these all make Graphene become ideal polymer packing.But the surface energy that Graphene is higher makes it easily reunite in polymeric matrix and solvent, causes detrimentally affect to its performance, so in the process preparing mixture, the scattering problem of solution Graphene becomes the emphasis in research.Conventional laboratory facilities have solution blending, melt blending and in-situ polymerization.In recent years, existing many bibliographical informations cross Graphene/polypropylene-base conducing composite material, the method that An etc. adopt double-screw melt blending to extrude has prepared EG/PP conductive nano composite material (An J E, Jeon G W, Jeong Y G.Preparation and properties of polypropylene nanocomposites reinforced with exfoliated graphene [J] .Fibers and Polymers, 2012,13 (4): 507-514.); Li etc. utilize solution blended process to obtain GnPs/PP conducing composite material (Li Y, Zhu J, Wei S, et al.Poly (propylene)/Graphene Nanoplatelet Nanocomposites:Melt Rheological Behavior and Thermal, Electrical, and Electronic Properties [J] .Macromolecular Chemistry and Physics, 2011,212 (18): 1951-1959.).Although these methods have prepared the good Graphene/polypropyleconductive conductive nano composite material of conductivity, also and be not all perfect, as complicated in experiment operational means, the compound conductive percolation threshold obtained is higher etc.Therefore, seek a kind of succinctly easy experimental technique, and low percolation threshold can be obtained simultaneously, Graphene/polypropyleconductive conductive nano composite material that conductivity is good will be significant to production application.
Summary of the invention
The object of this invention is to provide good Graphene/polypropyleconductive conductive nano composite material of a kind of low percolation threshold conductivity and preparation method thereof.
Graphene/polypropyleconductive conductive nano composite material of the present invention, with quality be 100 parts of calculating, the maleic anhydride inoculated polypropylene (promoting the dispersion of Graphene) of the polypropylene (as matrix) containing 92.5 ~ 97.5 mass parts, the Graphene (as conductive filler material) of 1 ~ 3 mass parts and 1.5 ~ 4.5 mass parts, is obtained by hot pressing after solution blending.
Graphene/polypropyleconductive conductive nano composite material of the present invention, refer to polypropylene matrix to be external phase, with the Graphene of nano-scale for disperse phase, by following laboratory facilities, graphene uniform is scattered in polypropylene, forms the compound system that contains nano-sized materials mutually.Graphene/polypropyleconductive conductive nano composite material involved in all embodiments, defines identical all therewith.
The preparation method of Graphene/polypropyleconductive conductive nano composite material of the present invention, its step is as follows:
(1) preparation of graphene dispersing solution
The Graphene of 1.0 ~ 3.0 mass parts is joined in the dimethylbenzene of 100 ~ 600 mass parts, at normal temperatures ultrasonic disperse 3 ~ 5h, obtained graphene dispersing solution;
(2) preparation of polymers soln
Be dissolved in the dimethylbenzene of 600 ~ 800 mass parts by the polypropylene of the maleic anhydride inoculated polypropylene of 1.5 ~ 4.5 mass parts and 92.5 ~ 97.5 mass parts, under 110 ~ 140 ° of C conditions, mechanical stirring, solution blending form continuously homogeneous polymers soln;
(3) preparation of Graphene/polypropyleconductive conductive nano composite material
The graphene dispersing solution of step (1) is joined in the polymers soln of step (2), add dimethylbenzene, the concentration controlling whole mixed system is 0.5 ~ 1g/10ml, mechanical stirring 4 ~ 6h is continued under temperature-resistant prerequisite, while hot said mixture is poured into (dehydrated alcohol mass parts is 20 ~ 50 times of xylene mass part) in dehydrated alcohol excessive greatly, absolute ethanol washing 3 ~ 5 times are used again after filtration product, dry 10 ~ 15h in 50 ~ 60 ° of C baking ovens, by the product that obtains at 210 ~ 240 ° of C, hot pressing is carried out under the condition of 9 ~ 10MPa, obtain Graphene/polypropyleconductive conductive nano composite material.
By changing the massfraction of Graphene in complex systems, obtain the Graphene/polypropyleconductive conductive nano composite material of a series of different ratios.The Graphene/polypropyleconductive conductive nano composite material of preparation can be used for the fields such as electro-conductive material, electromagnetic shielding material, antistatic material.
Performance test
The electric property of Graphene/polypropyleconductive conductive nano composite material is divided into direct current performance, AC electrical properties and dielectric properties.Direct current performance adopts digital multimeter FLUCK17B and Agilent4339B type megger to test.AC electrical properties and dielectric properties adopt Agilent4294A precise impedance analyser to test.Test result is shown in Fig. 1 ~ Fig. 3.
Tool of the present invention has the following advantages:
1. the present invention adopts and makes polypropylene and maleic anhydride inoculated polypropylene be mixed to form homogeneous phase holding system altogether to promote the dispersion of Graphene, and utilize dehydrated alcohol discharging, dehydrated alcohol is cheap and easy to get, reduces costs.
2. obtained Graphene/polypropyleconductive conductive nano composite material percolation threshold is low, and electrical property is good.
Accompanying drawing explanation
Fig. 1: the direct current volume conductance profile figure of virgin pp material prepared by the Graphene/polypropyleconductive conductive nano composite material of different Graphene content prepared by embodiment 1 ~ 6 and comparative example 1.As can be seen from Figure 1, virgin pp is insulating material, and the direct current volume conductance of the Graphene/nanometer composite polypropylene material obtained after adding Graphene improves, and achieves the transformation from isolator to conductor.In the embedded figure of Fig. 1, by seepage theory formula
give percolation threshold linear fit curve, the conduction percolation threshold of matrix material
Fig. 2: the interchange volume conductance graphic representation of virgin pp material prepared by the Graphene/polypropyleconductive conductive nano composite material of different Graphene content prepared by embodiment 1 ~ 6 and comparative example 1.Under same frequency, the interchange volume conductance of matrix material raises with the increase of Graphene content; When the content of Graphene is more than 1.5wt%, the interchange volume conductance of matrix material does not change with frequency substantially.
Fig. 3: the specific inductivity graphic representation of virgin pp material prepared by the Graphene/polypropyleconductive conductive nano composite material of different Graphene content prepared by embodiment 1 ~ 6 and comparative example 1.When Graphene content is 1.5wt%, the specific inductivity of matrix material is about 10 times of virgin pp material.
Embodiment
Be described method of the present invention below by specific embodiment, the specific descriptions of described embodiment just to claim of the present invention, claim includes but not limited to described embodiment content.
Reagent described in following embodiment and material if no special instructions, all can obtain from commercial channels; Described experimental technique, if no special instructions, is ordinary method.
Embodiment 1. prepares the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 1.0wt%
By the graphene dispersion of 0.01g in the dimethylbenzene of 1ml, ultrasonic disperse 3h in processor for ultrasonic wave at normal temperatures, obtained graphene dispersing solution.Join in 8ml dimethylbenzene by 0.975g polypropylene and 0.015g maleic anhydride inoculated polypropylene, under 110 ° of C, mechanical stirring, solution blending form continuously homogeneous polymers soln.Joined in above-mentioned polymers soln by above-mentioned graphene dispersing solution, add dimethylbenzene 1ml, the concentration controlling whole mixed system is 1g/10ml.Mechanical stirring 4h is continued under temperature-resistant prerequisite, while hot said mixture is poured in the dehydrated alcohol of 200ml, absolute ethanol washing 3 times are used again after filtration product, by above-mentioned product dry 10h in 50 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 210 ° of C, 9MPa, obtains the Graphene/polypropyleconductive conductive nano composite material that Graphene mass content is 1.0%.The DC conductivity of matrix material is listed in table 1.
Embodiment 2. prepares the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 1.3wt%
By the graphene dispersion of 0.013g in the dimethylbenzene of 1.5ml, ultrasonic disperse 3h in processor for ultrasonic wave at normal temperatures, obtained graphene dispersing solution.Join in 6.5ml dimethylbenzene by the polypropylene of 0.9675g and the maleic anhydride inoculated polypropylene of 0.0195g, under 120 ° of C, mechanical stirring, solution blending form continuously homogeneous polymers soln.Joined in above-mentioned polymers soln by above-mentioned graphene dispersing solution, add dimethylbenzene 3ml, the concentration controlling whole mixed system is about 0.91g/10ml.Mechanical stirring 4.5h is continued under temperature-resistant prerequisite, while hot said mixture is poured in the dehydrated alcohol of 250ml, absolute ethanol washing 3 times are used again after filtration product, by above-mentioned product dry 11h in 50 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 215 ° of C, 9MPa, obtains the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 1.3wt%.The DC conductivity of matrix material is listed in table 1.
Embodiment 3. prepares the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 1.5wt%
By the graphene dispersion of 0.015g in the dimethylbenzene of 2ml, ultrasonic disperse 4h in processor for ultrasonic wave at normal temperatures, obtained graphene dispersing solution.Join in 6ml dimethylbenzene by the polypropylene of 0.9625g and the maleic anhydride inoculated polypropylene of 0.0225g, under 125 ° of C, mechanical stirring, solution blending form continuously homogeneous polymers soln.Joined in above-mentioned polymers soln by above-mentioned graphene dispersing solution, add dimethylbenzene 4ml, the concentration controlling whole mixed system is 0.83g/10ml.Mechanical stirring 5h is continued under temperature-resistant prerequisite, while hot said mixture is poured in the dehydrated alcohol of 280ml, absolute ethanol washing 3 times are used again after filtration product, by above-mentioned product dry 12h in 55 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 220 ° of C, 9.5MPa, obtains the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 1.5wt%.The DC conductivity of matrix material is listed in table 1.
Embodiment 4. prepares the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 2.0wt%
By the graphene dispersion of 0.02g in the dimethylbenzene of 3.5ml, ultrasonic disperse 4.5h in processor for ultrasonic wave at normal temperatures, obtained graphene dispersing solution.Join in 7ml dimethylbenzene by the polypropylene of 0.95g and the maleic anhydride inoculated polypropylene of 0.03g, under 130 ° of C, mechanical stirring, solution blending form continuously homogeneous polymers soln.Joined in above-mentioned polymers soln by above-mentioned graphene dispersing solution, add dimethylbenzene 4.5ml, the concentration controlling whole mixed system is 0.67g/10ml.Mechanical stirring 5.5h is continued under temperature-resistant prerequisite, while hot said mixture is poured in the dehydrated alcohol of 350ml, absolute ethanol washing 4 times are used again after filtration product, by above-mentioned product dry 14h in 50 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 225 ° of C, 10MPa, obtains the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 2.0wt%.The DC conductivity of matrix material is listed in table 1.
Embodiment 5. prepares the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 2.5wt%
By the graphene dispersion of 0.025g in the dimethylbenzene of 5ml, ultrasonic disperse 5h in processor for ultrasonic wave at normal temperatures, obtained graphene dispersing solution.Join in 6ml dimethylbenzene by the polypropylene of 0.9375g and the maleic anhydride inoculated polypropylene of 0.0375g, under 135 ° of C, mechanical stirring, solution blending form continuously homogeneous polymers soln.Joined in above-mentioned polymers soln by above-mentioned graphene dispersing solution, add dimethylbenzene 6ml, the concentration controlling whole mixed system is 0.59g/10ml.Mechanical stirring 6h is continued under temperature-resistant prerequisite, while hot said mixture is poured in the dehydrated alcohol of 400ml, absolute ethanol washing 5 times are used again after filtration product, by above-mentioned product dry 15h in 60 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 230 ° of C, 10MPa, obtains the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 2.5wt%.The DC conductivity of matrix material is listed in table 1.
Embodiment 6. prepares the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 3.0wt%
By the graphene dispersion of 0.03g in the dimethylbenzene of 6ml, ultrasonic disperse 5h in processor for ultrasonic wave at normal temperatures, obtained graphene dispersing solution.Join in 6ml dimethylbenzene by the polypropylene of 0.925g and the maleic anhydride inoculated polypropylene of 0.045g, under 140 ° of C, mechanical stirring, solution blending form continuously homogeneous polymers soln.Joined in above-mentioned polymers soln by above-mentioned graphene dispersing solution, add dimethylbenzene 8ml, the concentration controlling whole mixed system is 0.5g/10ml.Mechanical stirring 6h is continued under temperature-resistant prerequisite, while hot said mixture is poured in the dehydrated alcohol of 500ml, absolute ethanol washing 5 times are used again after filtration product, by above-mentioned product dry 15h in 60 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 240 ° of C, 10MPa, obtains the Graphene/polypropyleconductive conductive nano composite material that Graphene content is 3.0wt%.The DC conductivity of matrix material is listed in table 1.
Comparative example 1. virgin pp material
Joined by 1g polypropylene in 10ml dimethylbenzene, under 120 ° of C, mechanical stirring 5h forms continuously homogeneous polymers soln.While hot above-mentioned polymers soln is poured in the dehydrated alcohol of 200ml, absolute ethanol washing 3 times are used again after filtration product, by above-mentioned product dry 12h in 50 ° of C baking ovens after suction filtration, the product obtained is carried out hot pressing under the condition of 210 ° of C, 9MPa, obtains virgin pp material.The DC conductivity of virgin pp material is listed in table 1.
After direct current volume conductance test under room temperature, carrying out the percolation threshold that linear fit obtains Graphene/polypropyleconductive conductive nano composite material is 1.2wt%, degree of fitting R
2=0.98954.
The test result of table 1 embodiment 1 ~ 6 and comparative example 1
As can be seen from Table 1, virgin pp is insulating material, and after interpolation Graphene, the specific conductivity of the Graphene/polypropylene composite material obtained rises with the increase of Graphene content, achieves the transformation from isolator to conductor.
Claims (1)
1. a preparation method for Graphene/polypropyleconductive conductive nano composite material, its step is as follows:
(1) preparation of graphene dispersing solution
The Graphene of 1.0 ~ 3.0 mass parts is joined in the dimethylbenzene of 100 ~ 600 mass parts, at normal temperatures ultrasonic disperse 3 ~ 5h, obtained graphene dispersing solution;
(2) preparation of polymers soln
Be dissolved in the dimethylbenzene of 600 ~ 800 mass parts by the polypropylene of the maleic anhydride inoculated polypropylene of 1.5 ~ 4.5 mass parts and 92.5 ~ 97.5 mass parts, under 110 ~ 140 DEG C of conditions, mechanical stirring, solution blending form continuously homogeneous polymers soln;
(3) preparation of Graphene/polypropyleconductive conductive nano composite material
The graphene dispersing solution of step (1) is joined in the polymers soln of step (2), add dimethylbenzene, the concentration controlling whole mixed system is 0.5 ~ 1g/10ml, mechanical stirring 4 ~ 6h is continued under temperature-resistant prerequisite, while hot said mixture is poured in dehydrated alcohol excessive greatly, absolute ethanol washing 3 ~ 5 times are used again after filtration product, dry 10 ~ 15h in 50 ~ 60 DEG C of baking ovens, by the product obtained 210 ~ 240 DEG C, carry out hot pressing under the condition of 9 ~ 10MPa, obtain Graphene/polypropyleconductive conductive nano composite material.
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| CN111171449B (en) * | 2020-02-05 | 2022-10-28 | 上海大学 | High-thermal-conductivity polypropylene/graphene composite material and preparation method thereof |
| CN111534012A (en) * | 2020-06-15 | 2020-08-14 | 广东电网有限责任公司电力科学研究院 | Polypropylene/graphite conductive composite material and preparation method and application thereof |
| CN112175286B (en) * | 2020-09-02 | 2021-08-06 | 兰州大学 | Graphene-polypropylene composite master batch and preparation method and application thereof |
| CN113150487B (en) * | 2021-02-07 | 2022-10-28 | 南方电网科学研究院有限责任公司 | Preparation method of thermoplastic shielding material |
| CN115569966A (en) * | 2022-11-03 | 2023-01-06 | 山东金利特新材料有限责任公司 | Recycling method of waste filter element |
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| CN102602915A (en) * | 2012-03-02 | 2012-07-25 | 北京化工大学 | Method for reducing graphene oxide and preparing conductive nanometer composite material |
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