CN109294283A - 一种多相纳米级复合碳材料的制备方法 - Google Patents
一种多相纳米级复合碳材料的制备方法 Download PDFInfo
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- CN109294283A CN109294283A CN201811147399.0A CN201811147399A CN109294283A CN 109294283 A CN109294283 A CN 109294283A CN 201811147399 A CN201811147399 A CN 201811147399A CN 109294283 A CN109294283 A CN 109294283A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Chemical group 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/10—Treatment with macromolecular organic compounds
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- C09C3/12—Treatment with organosilicon compounds
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Abstract
本发明涉及复合碳材料,公开了一种多相纳米级复合碳材料的制备方法。该制备方法包括石墨烯纳米粉体制备,石墨烯粉体和炭黑通入水、乙醇及偶联剂进行原位接枝反应等步骤。该制备方法简单易行,适合工业化生产,能够提高纳米材料在有机基体中的分散,得到的胎面胶具有更优良的耐磨和导电性能。
Description
技术领域
本发明涉及复合碳材料,特别涉及一种多相纳米级复合碳材料的制备方法。
背景技术
碳是自然界分布最广的元素之一,它具有多样的电子轨道特性(SP,SP2,SP3杂化),因此可以形成结构和性质迥然不同的同素异形体,如零维的炭黑和富勒烯,一维的碳纳米管(CNT)和碳纳米纤维(CNF),二维的石墨烯等,这些碳材料具备独特而优异的力学、电学和热学等性质,这些性质使此类纳米材料占有不可替代的地位和作用,并使其成为各种补强填料以及导电、导热的理想材料,因此纳米复合材料的制备与应用研究,日益成为人们的研究重点。
来源于石墨的石墨烯要比合成的碳纳米管从成本上说是更加实用廉价的,发明人考虑到碳纳米管较为贵的成本,最终决定采用廉价的纳米尺度的石墨片层和石墨烯制备多相纳米复合材料;现有技术中也有采用石墨烯和炭黑制备复合材料的,比如中国专利CN201210483568.4公开了一种氧化石墨烯与炭黑复合应用于电化学电容器电极材料中,比如中国专利201310157282.1公开了一种机械共混制备氧化石墨烯/白炭黑/橡胶纳米复合材料的方法,但是这些制备方法都是用了强的氧化剂,所使用的试剂不仅难以挥发而且破坏了石墨烯的结构,影响了其产品的性能,同时氧化还原法或生物质催化法制备的石墨烯含有大量官能团(羧基、羟基、环氧等表面官能团)作为导电剂导电性下降很多数量级,不推荐用作导电剂;也有研究者使用活性剂改性石墨烯,将改性石墨烯和炭黑联合制备复合材料,但是仍然存在石墨烯和炭黑的表面化学惰性大、比表面积大、自身团聚结合力很强,造成与其他聚合物的亲和性差,难以均匀分散在有机基体中。所以选择合适种类和数量的改性剂以及制备方法,来提高纳米材料在有机基体中的分散,同时还使其制备的胎面胶具有高耐磨、低生热和良好导电性能,具有重要意义。
发明内容
为了解决现有技术中的复合纳米碳材料在有机基体中的分散性差,得到的胎面胶的具有耐磨性及导电性差、生热高的问题,本发明提供了一种多相纳米级复合碳材料的制备方法。
为了解决上述技术问题,本发明采用以下技术方案:
一种多相纳米级复合碳材料的制备方法,具体包括以下步骤:
(1.1)将石墨粉体分散在质量浓度为0.1-3%的聚氧乙烯型非离子表面活性剂或氨基酸型离子表面活性剂水溶液中混合,所述石墨粉体和表面活性剂的质量比为1:50-1:150,将混合液放入球磨罐中球磨,静置后倾出上层黑色溶液,将其洗涤抽滤后得到固体,将所述固体放入马弗炉中,升温到100-1200℃,保温至残留表面活性剂炭化,得到比表面积大、层数小于10层的石墨烯粉体;
作为优选,所述球磨机以200-1000rpm转速球磨10-30h;作为优选,所述表面活性剂选自烷基酚聚氧乙烯醚、萘酚聚氧乙烯醚、辛基酚聚氧乙烯醚、双十二烷基二甲基溴化铵、十二烷基苯磺酸钠、十二烷基硫酸钠、十二烷基氨基丙酸钠、十六烷基三甲基溴化铵\聚乙二醇对异辛基苯基醚、月桂酰基谷氨酸钠中的一种。
(1.2)将所述石墨烯粉体和炭黑放入接枝反应器中,然后通入质量浓度为0.5-30%偶联剂水溶液进行原位接枝反应得到接枝反应物;优选地,所述接枝反应的反应温度为0-150℃,反应压力为0-2kg/cm2,反应时间为1-10h;所述石墨烯粉体、炭黑和偶联剂的质量比为1:5-50:1-20,三者比例不合适可能导致复合材料的硬度太大,无法实现混炼,或者能够实现混炼,但是复合材料在胶料中的的分散性能不好,生热高,导电性和耐磨性不好,本发明原料的配比能够很好兼顾复合材料的性能以及与胶料混合的效果。
作为优选,所述偶联剂选自对苯酚磺酸、烯烃基多硫化物、硅硼偶联剂、3-氯丙基三甲氧基硅烷、顺丁烯二酸二丁酯、三甲氧基硅烷基甲硫醇、4,4'-偶氮二(4-氰基戊酸)聚乙二醇酯、(N,N-二甲胺基乙基)丙烯酸酯、氨基磺酸、双-(γ-三乙氧基硅丙基)四硫化物、N-氨乙基-3-氨丙基甲基二甲氧基硅烷、γ-氨丙基三乙氧基硅烷、3-氨基丙基三乙氧基硅烷的一种或几种。
(1.3)将所述接枝反应物搅拌均匀并加热至0-150℃或超声混合,然后将所得料浆雾化、干燥制得微粒状多相纳米级复合碳材料;优选地,超声混合的超声频率为20-130KHz,超声功率≥300W,超声时间为0.5-5h。
因为本发明的发明目的决定了其石墨烯的剥离工艺不需要制备纯度很高的单层石墨烯,本发明制备的石墨烯片层的比表面积大、层数小于10层(大约为2-10层),步骤(1.1)采用的表面活性剂、原料与活性剂的配比、以及球磨工艺的目的是为了将石墨烯片层剥离分散的更快,效果更高,而不是为了制备纯度更高的石墨烯片层。
步骤(1.1)中使用了表面活性剂,多余的活性剂会影响复合材料与胶料的混炼效果,因此,本发明增加了炭化工艺,能够除出表面活性剂,使最终得到的复合材料能够很好的与胶料混炼。
本发明的步骤(1.2)的原位接枝反应中使用了特定的偶联剂,所述偶联剂均带有活泼端基,碳材料石墨烯、炭黑表面所带有的-H、-OH和-COOH等基团可能会与带有活泼端基偶联剂进行反应,并将活泼端基牢固结合在炭黑表面,使炭黑间间距增大,聚集体空隙变大,片层石墨烯与偶联剂复合且能够均匀穿插在炭黑粒子中,最终实现石墨烯与炭黑两种粒子相互的隔离,达到良好分散的效果,并且制备得到的复合材料能够提高胶料的导电性和耐磨性。
附图说明
图1为本发明所提供的石墨烯粉体的SEM电子扫描图;
图2为本发明所提供的多相纳米级复合碳材料的SEM电子扫描图。
具体实施方式
本发明公开了一种多相纳米级复合碳材料的制备方法,本领域技术人员可以借鉴本文内容,适当改进工艺参数实现。特别需要指出的是,所有类似的替换和改动对本领域技术人员来说是显而易见的,它们都被视为包括在本发明当中。本发明的方法及应用已经通过较佳实施例进行了描述,相关人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和应用进行改动或适当变更与组合,来实现和应用本发明技术。
实施例1
1)石墨烯纳米粉体制备:石墨粉,质量浓度为1.5%的聚氧乙烯醚溶液混合放入球磨罐中,石墨粉与聚氧乙烯醚的质量比为1:100,球磨罐大小为20cm,研磨球规格为10mm,球磨机转速为600rpm,球磨时间20h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温650℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;将石墨烯粉体进行电子显微镜扫描,扫描后的图片见图1;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为15%的3-氨基丙基三乙氧基硅烷水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:25:10,反应器温度在100℃,压力在2kg/cm2,反应时间5h,进行原位接枝反应;
3)将所述接枝反应物的混合料浆搅拌均匀并加热至75℃,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料;将该复合碳材料进行电子显微镜扫描,扫描后的图片见图2。
图1和图2显示,多相纳米级复合碳材料的石墨烯片层上均匀穿插着球状炭黑粒子,说明本发明制备的石墨烯/炭黑复合材料中,两者的分散均匀性及稳定性能比较好。
实施例2
1)石墨烯纳米粉体制备:石墨粉,质量浓度为0.1%的十二烷基苯磺酸钠溶液混合放入球磨罐中,石墨粉体与表面活性剂的质量比为1:50,球磨罐大小为20cm,研磨球规格为12mm,球磨机转速为200rpm,球磨时间10h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温100℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为1%的4,4'-偶氮二(4-氰基戊酸)聚乙二醇酯水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:5:1,反应器温度在20℃,压力在1kg/cm2,反应时间1h,进行原位接枝反应;
3)将所述接枝反应物的混合料浆搅拌均匀并加热至20℃,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料。
实施例3
1)石墨烯纳米粉体制备:石墨粉,质量浓度为3%的辛基酚聚氧乙烯醚溶液混合放入球磨罐中,石墨粉与表面活性剂的质量比为1:150,球磨罐大小为20cm,研磨球规格为12mm,球磨机转速为1000rpm,球磨时间30h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温1200℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为3%的3-氯丙基三甲氧基硅烷水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:50:20,反应器温度在150℃,压力在5kg/cm2,反应时间10h,进行原位接枝反应;
3)将所述接枝反应物的混合料浆搅拌均匀并加热至150℃,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料。
实施例4
1)石墨烯纳米粉体制备:石墨粉,质量浓度为1.5%的聚乙二醇对异辛基苯基醚溶液混合放入球磨罐中,石墨粉与表面活性剂的质量比为1:100,球磨罐大小为20cm,研磨球规格为12mm,球磨机转速为450rpm,球磨时间25h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温800℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为5%的双-[γ-(三乙氧基硅)丙基]四硫化物水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:30:12,反应器温度在120℃,压力在3kg/cm2,反应时间4h,进行原位接枝反应;
3)将所述接枝反应物的混合料浆超声混合均匀,超声混合的超声频率为20KHz,超声功率≥300W,超声时间为0.5h,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料。
实施例5
1)石墨烯纳米粉体制备:石墨粉,质量浓度为1.5%的聚乙二醇对异辛基苯基醚溶液混合放入球磨罐中,石墨粉与表面活性剂的质量比为1:70,球磨机转速为750rpm,球磨时间15h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温400℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为5%的N-氨乙基-3-氨丙基甲基二甲氧基硅烷和3-氨基丙基三乙氧基硅烷的水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:40:18,反应器温度在50℃,压力在1kg/cm2,反应时间8h,进行原位接枝反应.
3)将所述接枝反应物的混合料浆超声混合均匀,超声混合的超声频率为130KHz,超声功率≥300W,超声时间为5h,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料。
实施例6
1)石墨烯纳米粉体制备:石墨粉,质量浓度为1.5%的聚氧乙烯醚溶液混合放入球磨罐中,石墨粉与聚氧乙烯醚的质量比为1:100,球磨机转速为600rpm,球磨时间20h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温650℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为15%的硅硼偶联剂水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:25:10,反应器温度在100℃,压力在2kg/cm2,反应时间5h,进行原位接枝反应。
3)将所述接枝反应物的混合料浆搅拌均匀并加热至75℃,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料。
实施例7
1)石墨烯纳米粉体制备:石墨粉,质量浓度为1.5%的聚氧乙烯醚溶液混合放入球磨罐中,石墨粉与聚氧乙烯醚的质量比为1:100,球磨机转速为600rpm,球磨时间20h,静置24h后倾出上层黑色溶液,将此溶液进行洗涤抽滤后所得固体放入马弗炉中,升温650℃,保温一段时间至残留活性剂炭化,得到层数小于10层的石墨烯纳米粉体;
2)接枝反应:将石墨烯粉体和适量炭黑放入带有搅拌齿的接枝反应器中,加入质量浓度为15%的烯烃基多硫化物和3-氨基丙基三乙氧基硅烷的水溶液,石墨烯粉体与炭黑和偶联剂的质量比为1:25:10,反应器温度在100℃,压力在2kg/cm2,反应时间5h,进行原位接枝反应。
3)将所述接枝反应物的混合料浆搅拌均匀并加热至75℃,通过施加压力将料浆送至雾化器,经雾化器雾化并对雾化的料浆进行干燥得到微粒状多相纳米级复合碳材料。
对比例1
仅仅将炭黑添加到胎面胶中,对该胎面胶进行性能测试作为对照项;将实施例1中的工艺步骤的表面活性炭化步骤去掉,其他工艺与实施例1完全相同,制备的复合材料添加到半钢及全轮胎胎面胶配方,经过性能测试,测试结果与实施例1进行比较,比较结果见表1
表1胎面胶性能测试结果
表1数据显示,石墨烯炭化后胶料性能明显提升,经炭化后石墨烯表面附着的分散剂被炭化分解,使其石墨烯表面片层厚度变薄,石墨烯导电、导热性能得到明显提升。
对比例2
仅仅将炭黑添加到胎面胶中,对该胎面胶进行性能测试作为对照项;将实施中的偶联剂去除,其他工艺与实施例1完全相同,制备的复合材料添加到半钢及全轮胎胎面胶配方中,与实施例1-4的胎面胶作性能测试比较,比较结果见表2。
表2不同的偶联剂得到的胎面胶性能测试结果
表2数据显示,复合材料经偶联剂接枝处理后,复合材料的胶料其磨耗量降低25%左右,说明本发明提供的制备方法得到的多相纳米级复合碳材料与胶料混合,得到的胎面胶具有高耐磨的特性;表2中复合材料的胶料其体积电阻率下降近3个数量级,导电性能明显提高,在一些特殊车辆用轮胎的导电性要求良好,比如油罐车的车胎对车胎的导电性要求比较严格,油罐车等特殊车辆需要抗静电作用良好,以防止车辆事故的发生;复合材料的胶料其生热降低8%,导热系数提高30%,说明本发明提供的制备方法得到的多相纳米级复合碳材料与胶料混合,得到的胎面胶具有低生热的特性。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (6)
1.一种多相纳米级复合碳材料的制备方法,其特征在于,具体包括以下步骤:
(1.1)将石墨粉体分散在质量浓度为0.1-3%的聚氧乙烯型非离子表面活性剂或氨基酸型离子表面活性剂水溶液中混合,所述石墨粉体和表面活性剂的质量比为1:50-1:150,将混合液放入球磨罐中球磨,静置后倾出上层黑色溶液,将其洗涤抽滤后得到固体,将所述固体放入马弗炉中,升温到100-1200℃,保温至残留表面活性剂炭化,得到比表面积大、片层厚度薄,层数小于10层的石墨烯粉体;
(1.2)将所述石墨烯粉体和炭黑放入接枝反应器中,然后通入质量浓度为0.5-30%偶联剂水溶液进行原位接枝反应得到接枝反应物;
(1.3)将所述接枝反应物搅拌均匀并加热至0-150℃或超声混合,然后将所得料浆雾化、干燥制得微粒状多相纳米级复合碳材料。
2.如权利要求1所述的制备方法,其特征在于,所述表面活性剂选自烷基酚聚氧乙烯醚、萘酚聚氧乙烯醚、辛基酚聚氧乙烯醚、双十二烷基二甲基溴化铵、十二烷基苯磺酸钠、十二烷基硫酸钠、十二烷基氨基丙酸钠、十六烷基三甲基溴化铵\聚乙二醇对异辛基苯基醚或月桂酰基谷氨酸钠中的一种。
3.如权利要求1所述的制备方法,其特征在于,所述球磨机以200-1000rpm转速球磨10-30h。
4.如权利要求1所述的制备方法,其特征在于,所述偶联剂选自对苯酚磺酸、烯烃基多硫化物、硅硼偶联剂、3-氯丙基三甲氧基硅烷、顺丁烯二酸二丁酯、三甲氧基硅烷基甲硫醇、4,4'-偶氮二(4-氰基戊酸)聚乙二醇酯、(N,N-二甲胺基乙基)丙烯酸酯、氨基磺酸、双-(γ-三乙氧基硅丙基)四硫化物、N-氨乙基-3-氨丙基甲基二甲氧基硅烷、γ-氨丙基三乙氧基硅烷、3-氨基丙基三乙氧基硅烷一种或几种。
5.如权利要求1所述的制备方法,其特征在于,所述接枝反应的反应温度为0-150℃,反应压力为0-5kg/cm2,反应时间为1-10h;所述石墨烯粉体、炭黑和偶联剂的质量比为1:5-50:1-20。
6.如权利要求1所述的制备方法,其特征在于,所述步骤(1.3)中的超声混合的超声频率为20-130KHz,超声功率≥300W,超声时间为0.5-5h。
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