CN103232637A - 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 the polymer nanocomposites technical field, be specifically related to a kind of Graphene/polypropylene conductive nano composite material and preparation method thereof.
Background technology
Graphene is found to be in 2004 first, has prepared stable sheet Graphene by K.S.Novoselov with the method that A.K.Geim etc. utilizes micromechanics to separate.Since then, in nearest several years, obtained comprehensive attention about the research of Graphene.Graphene is the two-dirnentional structure that is formed by the monolayer carbon atom packing, shows as the hexagonal honeycomb, and it has big specific surface area, excellent electricity, mechanics, thermal property etc., and these all make Graphene become comparatively desirable polymer packing.But the higher surface energy of Graphene makes it easily reunite in polymeric matrix and solvent, and its performance is caused detrimentally affect, so in the process of preparation mixture, the scattering problem of solution Graphene becomes the emphasis in the research.Laboratory facilities commonly used have solution blending, melt blending and in-situ polymerization.In recent years, existing many bibliographical informations are crossed Graphene/polypropylene-base conducing composite material, the method that employing double-screw melt blending such as An are extruded 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.).Though these methods have been prepared conductivity Graphene/polypropylene conductive nano composite material preferably, also and not all be perfectly, as experiment operational means complexity, the mixture that obtains conduction seepage flow threshold value is higher etc.Therefore, seek a kind of succinct easily experimental technique of row, and can obtain low seepage flow threshold value simultaneously, Graphene/polypropylene conductive nano composite material that conductivity is good will be significant to production application.
Summary of the invention
The purpose of this invention is to provide good Graphene/polypropylene conductive nano composite material of a kind of low seepage flow threshold value conductivity and preparation method thereof.
Graphene of the present invention/polypropylene conductive nano composite material, with quality be 100 parts of calculating, contain the polypropylene (as matrix) of 92.5～97.5 mass parts, the Graphene (as conductive filler material) of 1～3 mass parts and the maleic anhydride inoculated polypropylene (promoting the dispersion of Graphene) of 1.5～4.5 mass parts, obtain by hot pressing behind the solution blending.
Graphene of the present invention/polypropylene conductive nano composite material, refer to the polypropylene matrix to be external phase, Graphene with nano-scale is disperse phase, by following laboratory facilities Graphene is scattered in the polypropylene equably, and formation one contains the compound system of nano-sized materials mutually.Involved Graphene/polypropylene conductive nano composite material among all embodiment all defines identical therewith.
The preparation method of Graphene of the present invention/polypropylene conductive nano composite material, its step is as follows:
(1) preparation of Graphene dispersion liquid
The Graphene of 1.0～3.0 mass parts is joined in the dimethylbenzene of 100～600 mass parts, and ultra-sonic dispersion 3～5h makes the Graphene dispersion liquid at normal temperatures;
(2) preparation of polymers soln
The maleic anhydride inoculated polypropylene of 1.5～4.5 mass parts and the polypropylene of 92.5～97.5 mass parts are dissolved in the dimethylbenzene of 600～800 mass parts, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 110～140 ° of C conditions;
(3) preparation of Graphene/polypropylene conductive nano composite material
The Graphene dispersion liquid of step (1) is joined in the polymers soln of step (2), add dimethylbenzene, the concentration of controlling whole mixed system is 0.5～1g/10ml, under temperature-resistant prerequisite, continue mechanical stirring 4～6h, while hot said mixture is poured in the big excessive dehydrated alcohol (the dehydrated alcohol mass parts is 20～50 times of dimethylbenzene mass parts), use absolute ethanol washing 3～5 times after the filtration product again, dry 10～15h in 50～60 ° of C baking ovens, with the product that obtains at 210～240 ° of C, carry out hot pressing under the condition of 9～10MPa, obtain Graphene/polypropylene conductive nano composite material.
By changing the massfraction of Graphene in complex systems, obtain the Graphene/polypropylene conductive nano composite material of a series of different ratioss.Graphene/polypropylene conductive the nano composite material of preparation can be used for fields such as electro-conductive material, electromagnetic shielding material, antistatic material.
Performance test
The electric property of Graphene/polypropylene conductive nano composite material is divided into direct current performance, alternating-current performance and dielectric properties.The direct current performance adopts digital multimeter FLUCK17B and Agilent4339B type megger to test.Alternating-current performance and dielectric properties adopt the accurate electric impedance analyzer of Agilent4294A to test.Test result is seen Fig. 1～Fig. 3.
The present invention has following advantage:
1. the present invention adopts and makes polypropylene and maleic anhydride inoculated polypropylene mixing formation homogeneous phase hold system altogether to promote the dispersion of Graphene, utilizes the dehydrated alcohol discharging, and dehydrated alcohol is cheap and easy to get, reduces cost.
2. the Graphene that makes/polypropylene conductive nano composite material seepage flow threshold value is low, and electrical property is good.
Description of drawings
The direct current volume conductance graphic representation of the virgin pp material of the Graphene/polypropylene conductive nano composite material of the different Graphene content of Fig. 1: embodiment 1～6 preparation and Comparative Examples 1 preparation.As can be seen from Figure 1, virgin pp is insulating material, improves in the direct current volume conductance of adding the Graphene/nanometer composite polypropylene material that obtains behind the Graphene, has realized the transformation from the isolator to the conductor.In the embedded figure of Fig. 1, by the seepage theory formula
Provided the linear matched curve of seepage flow threshold value, the conduction seepage flow threshold value of matrix material
The interchange volume conductance graphic representation of the virgin pp material of the Graphene/polypropylene conductive nano composite material of the different Graphene content of Fig. 2: embodiment 1～6 preparation and Comparative Examples 1 preparation.Under same frequency, the interchange volume conductance of matrix material raises with the increase of Graphene content; When the content of Graphene surpassed 1.5wt%, the interchange volume conductance of matrix material did not change with frequency substantially.
The specific inductivity graphic representation of the virgin pp material of the Graphene/polypropylene conductive nano composite material of the different Graphene content of Fig. 3: embodiment 1～6 preparation and Comparative Examples 1 preparation.When Graphene content was 1.5wt%, the specific inductivity of matrix material was about 10 times of virgin pp material.
Embodiment
Below by specific embodiment method of the present invention is described, just to the specific descriptions of claim of the present invention, claim includes but not limited to described embodiment content to described embodiment.
Reagent described in the following embodiment and material all can obtain if no special instructions from commercial channels; Described experimental technique if no special instructions, is ordinary method.
The Graphene of 0.01g is scattered in the dimethylbenzene of 1ml, and ultra-sonic dispersion 3h in processor for ultrasonic wave makes the Graphene dispersion liquid at normal temperatures.0.975g polypropylene and 0.015g maleic anhydride inoculated polypropylene are joined in the 8ml dimethylbenzene, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 110 ° of C.Above-mentioned Graphene dispersion liquid is joined in the above-mentioned polymers soln, add dimethylbenzene 1ml, the concentration of controlling whole mixed system is 1g/10ml.Under temperature-resistant prerequisite, continue mechanical stirring 4h, while hot said mixture is poured in the dehydrated alcohol of 200ml, use absolute ethanol washing 3 times after the filtration product again, behind the suction filtration with above-mentioned product dry 10h in 50 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 210 ° of C, 9MPa, obtain the Graphene mass content and be Graphene/polypropylene conductive nano composite material of 1.0%.The dc conductivity of matrix material is listed in the table 1.
The Graphene of 0.013g is scattered in the dimethylbenzene of 1.5ml, and ultra-sonic dispersion 3h in processor for ultrasonic wave makes the Graphene dispersion liquid at normal temperatures.The polypropylene of 0.9675g and the maleic anhydride inoculated polypropylene of 0.0195g are joined in the 6.5ml dimethylbenzene, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 120 ° of C.Above-mentioned Graphene dispersion liquid is joined in the above-mentioned polymers soln, add dimethylbenzene 3ml, the concentration of controlling whole mixed system is about 0.91g/10ml.Under temperature-resistant prerequisite, continue mechanical stirring 4.5h, while hot said mixture is poured in the dehydrated alcohol of 250ml, use absolute ethanol washing 3 times after the filtration product again, behind the suction filtration with above-mentioned product dry 11h in 50 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 215 ° of C, 9MPa, obtaining Graphene content is Graphene/polypropylene conductive nano composite material of 1.3wt%.The dc conductivity of matrix material is listed in the table 1.
The Graphene of 0.015g is scattered in the dimethylbenzene of 2ml, and ultra-sonic dispersion 4h in processor for ultrasonic wave makes the Graphene dispersion liquid at normal temperatures.The polypropylene of 0.9625g and the maleic anhydride inoculated polypropylene of 0.0225g are joined in the 6ml dimethylbenzene, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 125 ° of C.Above-mentioned Graphene dispersion liquid is joined in the above-mentioned polymers soln, add dimethylbenzene 4ml, the concentration of controlling whole mixed system is 0.83g/10ml.Under temperature-resistant prerequisite, continue mechanical stirring 5h, while hot said mixture is poured in the dehydrated alcohol of 280ml, use absolute ethanol washing 3 times after the filtration product again, behind the suction filtration with above-mentioned product dry 12h in 55 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 220 ° of C, 9.5MPa, obtaining Graphene content is Graphene/polypropylene conductive nano composite material of 1.5wt%.The dc conductivity of matrix material is listed in the table 1.
The Graphene of 0.02g is scattered in the dimethylbenzene of 3.5ml, and ultra-sonic dispersion 4.5h in processor for ultrasonic wave makes the Graphene dispersion liquid at normal temperatures.The polypropylene of 0.95g and the maleic anhydride inoculated polypropylene of 0.03g are joined in the 7ml dimethylbenzene, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 130 ° of C.Above-mentioned Graphene dispersion liquid is joined in the above-mentioned polymers soln, add dimethylbenzene 4.5ml, the concentration of controlling whole mixed system is 0.67g/10ml.Under temperature-resistant prerequisite, continue mechanical stirring 5.5h, while hot said mixture is poured in the dehydrated alcohol of 350ml, use absolute ethanol washing 4 times after the filtration product again, behind the suction filtration with above-mentioned product dry 14h in 50 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 225 ° of C, 10MPa, obtaining Graphene content is Graphene/polypropylene conductive nano composite material of 2.0wt%.The dc conductivity of matrix material is listed in the table 1.
The Graphene of 0.025g is scattered in the dimethylbenzene of 5ml, and ultra-sonic dispersion 5h in processor for ultrasonic wave makes the Graphene dispersion liquid at normal temperatures.The polypropylene of 0.9375g and the maleic anhydride inoculated polypropylene of 0.0375g are joined in the 6ml dimethylbenzene, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 135 ° of C.Above-mentioned Graphene dispersion liquid is joined in the above-mentioned polymers soln, add dimethylbenzene 6ml, the concentration of controlling whole mixed system is 0.59g/10ml.Under temperature-resistant prerequisite, continue mechanical stirring 6h, while hot said mixture is poured in the dehydrated alcohol of 400ml, use absolute ethanol washing 5 times after the filtration product again, behind the suction filtration with above-mentioned product dry 15h in 60 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 230 ° of C, 10MPa, obtaining Graphene content is Graphene/polypropylene conductive nano composite material of 2.5wt%.The dc conductivity of matrix material is listed in the table 1.
The Graphene of 0.03g is scattered in the dimethylbenzene of 6ml, and ultra-sonic dispersion 5h in processor for ultrasonic wave makes the Graphene dispersion liquid at normal temperatures.The polypropylene of 0.925g and the maleic anhydride inoculated polypropylene of 0.045g are joined in the 6ml dimethylbenzene, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 140 ° of C.Above-mentioned Graphene dispersion liquid is joined in the above-mentioned polymers soln, add dimethylbenzene 8ml, the concentration of controlling whole mixed system is 0.5g/10ml.Under temperature-resistant prerequisite, continue mechanical stirring 6h, while hot said mixture is poured in the dehydrated alcohol of 500ml, use absolute ethanol washing 5 times after the filtration product again, behind the suction filtration with above-mentioned product dry 15h in 60 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 240 ° of C, 10MPa, obtaining Graphene content is Graphene/polypropylene conductive nano composite material of 3.0wt%.The dc conductivity of matrix material is listed in the table 1.
Comparative Examples 1. virgin pp materials
The 1g polypropylene is joined in the 10ml dimethylbenzene, and mechanical stirring 5h forms the polymers soln of continuous homogeneous under 120 ° of C.While hot above-mentioned polymers soln is poured in the dehydrated alcohol of 200ml, use absolute ethanol washing 3 times after the filtration product again, with above-mentioned product dry 12h in 50 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 210 ° of C, 9MPa behind the suction filtration, obtain the virgin pp material.The dc conductivity of virgin pp material is listed in the table 1.
After direct current volume conductance test under the room temperature, carrying out the seepage flow threshold value that linear fit obtains Graphene/polypropylene 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 Examples 1
As can be seen from Table 1, virgin pp is insulating material, and after adding Graphene, the specific conductivity of the Graphene/polypropylene composite material that obtains rises with the increase of Graphene content, has realized the transformation from the isolator to the conductor.
Claims (3)
1. Graphene/polypropylene conductive matrix material is characterized in that: with quality be 100 parts of calculating, be made up of the polypropylene of 92.5～97.5 mass parts, the Graphene of 1～3 mass parts and the maleic anhydride inoculated polypropylene of 1.5～4.5 mass parts.
2. the preparation method of Graphene/polypropylene conductive nano composite material, its step is as follows:
(1) preparation of Graphene dispersion liquid
The Graphene of 1.0～3.0 mass parts is joined in the dimethylbenzene of 100～600 mass parts, and ultra-sonic dispersion 3～5h makes the Graphene dispersion liquid at normal temperatures;
(2) preparation of polymers soln
The maleic anhydride inoculated polypropylene of 1.5～4.5 mass parts and the polypropylene of 92.5～97.5 mass parts are dissolved in the dimethylbenzene of 600～800 mass parts, and mechanical stirring, solution blending form the polymers soln of continuous homogeneous under 110～140 ° of C conditions;
(3) preparation of Graphene/polypropylene conductive nano composite material
The Graphene dispersion liquid of step (1) is joined in the polymers soln of step (2), add dimethylbenzene, the concentration of controlling whole mixed system is 0.5～1g/10ml, under temperature-resistant prerequisite, continue mechanical stirring 4～6h, while hot said mixture is poured in the big excessive dehydrated alcohol, use absolute ethanol washing 3～5 times after the filtration product again, dry 10～15h in 50～60 ° of C baking ovens, the product that obtains is carried out hot pressing under the condition of 210～240 ° of C, 9～10MPa, obtain Graphene/polypropylene conductive nano composite material.
3. the described Graphene of the claim 1/application of polypropylene conductive nano composite material aspect electro-conductive material, electromagnetic shielding material or antistatic material.
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| CN103980614A (en) * | 2014-05-21 | 2014-08-13 | 吴江市英力达塑料包装有限公司 | Graphene filled polypropylene material and preparation method thereof |
| CN104278360A (en) * | 2014-09-28 | 2015-01-14 | 苏州长盛机电有限公司 | Preparation method of graphene-doped conductive composite fiber |
| CN105932101A (en) * | 2016-05-20 | 2016-09-07 | 广东蒙泰纺织纤维有限公司 | Polypropylene fiber solar microcell and manufacturing method thereof |
| CN106188837A (en) * | 2016-07-11 | 2016-12-07 | 南昌大学 | A kind of FeNi alloy nano powder body and the composite material and preparation method thereof of thermoplastic resin PP |
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| CN108948491A (en) * | 2018-07-04 | 2018-12-07 | 中国地质大学（北京） | A kind of composite material and preparation method with electro-magnetic screen function |
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