CN115916695A - 碳材料分散液 - Google Patents
碳材料分散液 Download PDFInfo
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- CN115916695A CN115916695A CN202180048782.4A CN202180048782A CN115916695A CN 115916695 A CN115916695 A CN 115916695A CN 202180048782 A CN202180048782 A CN 202180048782A CN 115916695 A CN115916695 A CN 115916695A
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 30
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Classifications
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Abstract
提供一种碳材料分散液,其能够构成即使碳材料为高浓度也难以再聚集而稳定地分散在包含有机溶剂的液体介质中的、可以形成导电性优异的涂膜的油墨等各种制品。碳材料分散液含有碳材料、有机溶剂、和高分子分散剂,高分子分散剂为具有3~55质量%下述通式(1)(R表示氢原子等,A表示O或NH,B表示亚乙基等,R1和R2相互独立地表示甲基等,Ar表示苯基等,X表示氯原子等,p表示任意的重复单元数)所示的结构单元(1)的聚合物,高分子分散剂的胺值为100mgKOH/g以下,数均分子量为5000~20000。
Description
技术领域
本发明涉及碳材料分散液。
背景技术
碳黑、碳纤维、碳纳米管、石墨烯、石墨等碳材料(也记为“纳米碳材料”)具有通过碳原子的共价键形成的六元环石墨结构。这些碳材料是具有导电性或传热性等特性的材料,因此在很多领域中正在研究利用这些特性的使用方法。例如,关注碳材料的电特性、热特性和作为填料的性质等,迄今为止提出了作为防静电剂、导电材料和塑料增强材料的使用方法。进一步地,正在进行作为用于构成半导体、燃料电池电极、显示器的阴极线等的材料的开发。
这些用途通常以使碳材料分散在有机溶剂等液体介质中的碳材料分散液的状态使用。并且,对于这种碳材料分散液,要求碳材料均匀且稳定地分散在液体介质中,即所谓的分散性优异。进一步地,还要求这种分散性长期稳定地维持。不过,纳米尺寸的碳材料的表面能量高,由于强范德华力发挥作用,具有容易聚集的性质。因此,存在即使分散,也会马上聚集的问题。
为了解决这种问题,使碳材料在液体介质中稳定地分散,有时使用分散剂。例如,提出了使用烷醇胺盐等阳离子性表面活性剂、苯乙烯-丙烯酸系树脂等高分子分散剂作为分散剂,使碳纳米管等碳材料分散在液体介质中(专利文献1和2)。
现有技术文献
专利文献
专利文献1:日本特开2010-174084号公报
专利文献2:日本特表2013-537570号公报
发明内容
发明要解决的问题
通过使用专利文献1和2中提出的分散剂,可以使碳材料在液体介质中一定程度分散。但是,由于分散性不充分、或者分散后容易再聚集,因此分散性能未必充分,存在进一步改良的余地。
本发明是鉴于现有技术存在的这样的问题而完成的,其要解决的技术问题在于提供一种碳材料分散液,其能够构成即使碳材料为高浓度也难以再聚集而稳定地分散在包含有机溶剂的液体介质中的、可以形成导电性优异的涂膜的油墨等各种制品。
用于解决问题的方案
即,根据本发明,可以提供下述的碳材料分散液。
[1]一种碳材料分散液,其含有:选自由碳黑、碳纤维、碳纳米管、石墨和石墨烯组成的组中的至少1种的碳材料;有机溶剂;和高分子分散剂,所述高分子分散剂为具有3~55质量%下述通式(1)所示的结构单元(1)、45~90质量%下述通式(3)所示的结构单元(3)、和0.5~20质量%与这些结构单元连接的其他结构单元(4)(其中,所有结构单元的总和设为100质量%)的聚合物,所述高分子分散剂的胺值为100mgKOH/g以下、数均分子量为5000~20000。
(所述通式(1)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、或双(九氟丁烷磺酰)亚胺,p表示任意的重复数)
(所述通式(3)中,R表示氢原子或甲基,A表示O或NH,Q表示亚乙基或甲基亚乙基,Y表示O、NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基,r表示任意的重复数)
[2]根据上述[1]所述的碳材料分散液,其中,所述高分子分散剂为进一步具有下述通式(2)所示的结构单元(2)的聚合物。
(所述通式(2)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基,q表示任意的重复数)
[3]根据上述[2]所述的碳材料分散液,其中,所述结构单元(1)、所述结构单元(2)和所述结构单元(3)分别由下述通式(1-1)、下述通式(2-1)和下述通式(3-1)表示,所述结构单元(4)包含源自α-甲基苯乙烯的结构单元。
(所述通式(1-1)中,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、双(九氟丁烷磺酰)亚胺,p表示任意的重复数)
(所述通式(2-1)中,R1和R2相互独立地表示甲基或乙基,q表示任意的重复数)
(所述通式(3-1)中,Y表示NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基,r表示任意的重复数)
[4]根据上述[1]~[3]中任一项所述的碳材料分散液,其中,所述碳材料的含量为15质量%以下,相对于100质量份所述碳材料,所述高分子分散剂的含量为10~200质量份。
发明的效果
根据本发明,可以提供一种碳材料分散液,其能够构成即使碳材料为高浓度也难以再聚集而稳定地分散在包含有机溶剂的液体介质中的、可以形成导电性优异的涂膜的油墨等各种制品。
具体实施方式
<碳材料分散液>
以下,对本发明的实施方式进行说明,但本发明并不限于下述的实施方式。本发明的碳材料分散液含有碳材料、有机溶剂和高分子分散剂。使碳材料分散在包含有机溶剂的液体介质中的高分子分散剂为具有下述通式(1)所示的结构单元(1)、下述通式(3)所示的结构单元(3)、和与这些结构单元连接的其他结构单元(4)的聚合物。并且,该高分子分散剂的胺值为100mgKOH/g以下,数均分子量(Mn)为5000~20000。以下,对本发明的碳材料分散液的具体内容进行说明。
(碳材料)
碳材料为选自由碳黑、碳纤维、碳纳米管、石墨和石墨烯组成的组中的至少1种。作为碳黑,可以使用乙炔黑、炉黑、乙炔黑、热炭黑、科琴黑等现有公知的各种碳黑。
作为碳纤维,可以列举出以聚丙烯腈为原料的PAN系碳纤维、以沥青类为原料的沥青系碳纤维、和它们的再生品等。其中,优选纤维直径为纳米尺寸、具有将六元环石墨结构卷绕成筒状的形状的所谓碳纳米纤维、纤维直径为单纳米尺寸的碳纳米管。碳纳米纤维和碳纳米管可以是多层(多壁)和单层(单壁)中的任一者。
碳材料中也可以掺杂铂、钯等金属或金属盐。进一步地,碳材料也可以通过氧化处理、等离子体处理、辐射线处理、电晕处理、偶联处理等进行表面改性。
(有机溶剂)
作为有机溶剂,可以使用现有公知的有机溶剂。需要说明的是,也可以和有机溶剂一起使用水。作为有机溶剂,可以列举出己烷、甲苯、二甲苯等烃类溶剂;甲醇、乙醇、异丙醇、丁醇、十二醇等醇类溶剂;丙酮、甲乙酮、二乙基酮、异丁基甲基酮等酮类溶剂;乙酸乙酯、乙酸丁酯、乙酸戊酯、琥珀酸二甲酯、己二酸二甲酯、乳酸甲酯、乳酸二甲酯等酯类溶剂;二丙醚、四氢呋喃、二恶烷等醚类溶剂;碳酸二甲酯、碳酸亚乙酯、碳酸亚丙酯等碳酸酯类溶剂;N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、吡咯烷酮、N-甲基吡咯烷酮、3-甲氧基-N,N-二甲基丙酰胺、3-丁氧基-N,N-二甲基丙酰胺等酰胺类溶剂;四甲基脲、二甲基咪唑啉酮等脲类溶剂;二甲基亚砜等亚砜类溶剂;乙二醇、丙二醇、二乙二醇、乙二醇甲醚、乙二醇丁基醚、二乙二醇甲醚、二乙二醇单丁醚、三乙二醇单丁醚、丙二醇单甲醚、丙二醇单丙醚、丙二醇单丁醚、二丙二醇单甲醚等二醇单醚类溶剂;乙二醇二甲醚、二乙二醇二甲醚、二乙二醇二乙醚、二丙二醇二甲醚等二醇二醚类溶剂;乙二醇单甲醚乙酸酯、二乙二醇单甲醚乙酸酯、丙二醇单甲醚乙酸酯、丙二醇单丁醚乙酸酯等二醇醚单醚酯类溶剂等。
另外,可以使用(甲基)丙烯酸类单体、乙烯基醚类单体、环氧化合物、氧杂环丁烷化合物等反应性单体作为有机溶剂。通过使用这样的反应性单体作为有机溶剂,可以制成能够制备紫外线·电子射线固化性油墨、紫外线·电子射线固化性涂布剂等的碳材料分散液。
(高分子分散剂)
高分子分散剂为具有3~55质量%通式(1)所示的结构单元(1),45~90质量%通式(3)所示的结构单元(3)、和0.5~20质量%与这些结构单元连接的其他结构单元(4)(其中,所有结构单元的总和设为100质量%)的聚合物。
(所述通式(1)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、或双(九氟丁烷磺酰)亚胺,p表示任意的重复数)
(所述通式(3)中,R表示氢原子或甲基,A表示O或NH,Q表示亚乙基或甲基亚乙基,Y表示O、NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基,r表示任意的重复数)
[结构单元(1)]
结构单元(1)是具有季铵盐基的结构单元。作为能够构成结构单元(1)的单体(单体1),例如,可以列举出下述通式(1a)所示的单体。认为通过结构单元(1)中的季铵盐基吸附在碳材料上,有助于提高碳材料在包含有机溶剂的液体介质中的分散性。另外,与季铵盐基的氮原子结合的取代基之一为芳基甲基(-CH2-Ar)。认为该芳基甲基的芳香族环与碳材料亲和,从而提高碳材料的分散性。通式(1)中的R1和R2的碳原子数过多时,芳基甲基因位阻而变得不稳定,难以形成季铵盐基。因此,通式(1)中的R1和R2需要相互独立地为甲基或乙基。
(所述通式(1a)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、或双(九氟丁烷磺酰)亚胺)
由于季铵盐基是离子性的官能团,因此具有包含该季铵盐基的结构单元(1)的聚合物(高分子分散剂)有望通过水分吸附或离子导电而显示导电性。即,通过将具有结构单元(1)的聚合物用作高分子分散剂,有望制成可以形成抑制了导电性下降的涂膜的碳材料分散液。
结构单元(1)优选由下述通式(1-1)表示。
(所述通式(1-1)中,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、双(九氟丁烷磺酰)亚胺,p表示任意的重复数)
通式(1-1)所示的结构单元例如由下述通式(1a-1)所示的单体构成。
(所述通式(1a-1)中,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子,溴原子、双(三氟甲基)磺酰亚胺,双(九氟丁烷磺酰)亚胺)
作为能够构成通式(1-1)所示的结构单元的单体的具体例,可以列举出二甲基萘基甲基铵乙基甲基丙烯酸酯氯化物、二甲基萘基甲基铵乙基甲基丙烯酸酯溴化物、二甲基萘基甲基铵乙基甲基丙烯酸酯双(三氟甲基)磺酰亚胺、二甲基萘基甲基铵乙基甲基丙烯酸酯双(九氟丁烷磺酰)亚胺、二乙基萘基甲基铵乙基甲基丙烯酸酯氯化物、二乙基萘基甲基铵乙基甲基丙烯酸酯溴化物、二乙基萘基甲基铵乙基甲基丙烯酸酯双(三氟甲基)磺酰亚胺、二乙基萘基甲基铵乙基甲基丙烯酸酯双(九氟丁烷磺酰)亚胺、蒽基甲基二甲基甲基铵乙基甲基丙烯酸酯氯化物、蒽基甲基二甲基甲基铵乙基甲基丙烯酸酯溴化物、蒽基二甲基甲基铵乙基甲基丙烯酸酯双(三氟甲基)磺酰亚胺、蒽基二甲基萘基铵乙基甲基丙烯酸酯双(九氟丁烷磺酰)亚胺、二乙基乙烯基甲基铵乙基甲基丙烯酸酯氯化物、二乙基乙烯基甲基铵乙基甲基丙烯酸酯溴化物、二乙基乙烯基甲基铵乙基甲基丙烯酸酯双(三氟甲基)磺酰亚胺、二乙基乙烯基甲基铵乙基甲基丙烯酸酯双(九氟丁烷磺酰)亚胺等。
[结构单元(2)]
高分子分散剂优选为进一步具有下述通式(2)所示的结构单元(2)的聚合物。通过使用进一步具有结构单元(2)的聚合物作为高分子分散剂,可以进一步提高碳材料的分散性。需要说明的是,通过使结构单元(2)中的氨基季盐化,可以形成结构单元(1)中的季铵盐基。
(所述通式(2)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基,q表示任意的重复数)
作为能够构成结构单元(2)的单体(单体2),例如,可以列举出下述通式(2a)所示的单体。
(所述通式(2a)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基)
结构单元(2)具有作为碱性基团的氨基。因此,认为通过氧化等形成在碳材料的表面上的羧基或酚性羟基与结构单元(2)中的氨基离子键合,高分子分散剂容易吸附在碳材料上,可以进一步提高碳材料的分散性。进一步地,认为通过与结构单元(1)中的季铵盐基、构成季铵盐基的多环芳香族基团在碳材料上的吸附的协同效果,可以进一步提高碳材料的分散性。
结构单元(2)优选由下述通式(2-1)表示。
(所述通式(2-1)中,R1和R2相互独立地表示甲基或乙基,q表示任意的重复数)
通式(2-1)所示的结构单元例如由下述通式(2a-1)所示的单体构成。
(所述通式(2a-1)中,R1和R2相互独立地表示甲基或乙基。)
作为能够构成通式(2-1)所示的结构单元的单体的具体例,可以列举出甲基丙烯酸二甲基氨基乙酯、甲基丙烯酸二乙基氨基乙酯等。
[结构单元(3)]
结构单元(3)是具有聚亚烷基二醇链的结构单元。具有该结构单元(3)的高分子分散剂是具有聚亚烷基二醇链接枝的结构的聚合物。并且,聚亚烷基二醇链是可以溶解在作为分散介质的有机溶剂中的分子链。通式(3)中,Y表示的氨基甲酸酯键(NHCOO)、脲键(NHCONH)与构成通过改性在碳材料的表面生成的羟基等的氢原子氢键合。因此,高分子分散剂中,作为接枝链的聚亚烷基二醇链溶解在作为分散介质的有机溶剂中,同时包括结构单元(3)中的氨基甲酸酯键(NHCOO)或脲键(NHCONH)和结构单元(1)的主链吸附在碳材料上。并且,溶解的聚亚烷基二醇链在颗粒状的碳材料之间形成位阻而排斥,能够使碳材料在液体介质中长期良好且稳定地分散。
通式(3)中,m为亚丙基氧基(-CH(CH3)CH2O-)的平均重复单元数,n为亚乙基氧基(-CH2CH2O-)的平均重复单元数。并且,m和n相互独立地为0以上的数值,m+n=20~100,优选为m+n=35~100。即,聚亚烷基二醇链的分子量优选为880~5800,进一步优选为1540~5800。需要说明的是,通式(3)中,R3所示的碳原子数1~18的烷基优选为甲基、乙基、丙基、丁基、十二烷基、硬脂基、苯基、萘基或壬基苯基。
作为能够构成结构单元(3)的单体(单体3),例如,可以列举出下述通式(3a)所示的单体(大分子单体)。
(所述通式(3a)中,R表示氢原子或甲基,A表示O或NH,Q表示亚乙基或甲基亚乙基,Y表示O、NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基)
结构单元(3)优选由下述通式(3-1)表示。
(所述通式(3-1)中,Y表示NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基,r表示任意的重复数)
通式(3-1)所示的结构单元例如由下述通式(3a-1)所示的单体构成。
(所述通式(3a-1)中,Y表示NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基)
作为能够构成通式(3-1)所示的结构单元的单体,可以列举出使甲基丙烯酰氧基乙基异氰酸酯与聚乙二醇单甲醚、聚乙二醇聚丙二醇单丁醚、聚丙二醇单甲醚、聚乙二醇单十二烷基醚等二醇醚单烷基醚反应而得到的、Y为氨基甲酸酯键(NHCOO)的大分子单体;使甲基丙烯酰氧基乙基异氰酸酯与聚乙二醇聚丙二醇单胺等单醚单胺反应而得到的、Y为脲键(NHCONH)的大分子单体等。
通式(3)、(3a)、(3-1)和(3a-1)中,Y优选为使异氰酸酯与胺反应时不需要催化剂的脲键(NHCONH)。另外,通式(3)、(3a)、(3-1)和(3a-1)中的聚亚烷基二醇链优选为环氧丙烷与环氧乙烷的无规共聚物。进一步地,通式(3)、(3a)、(3-1)和(3a-1)中,R3优选为甲基。需要说明的是,聚亚烷基二醇链的分子量优选为2000~4000,优选m+n=36~90。
[结构单元(4)]
结构单元(4)是可以与上述结构单元连接的其他结构单元。作为能够构成结构单元(4)的单体(单体4),例如,可以列举出(甲基)丙烯酸、(甲基)丙烯酸酯等(甲基)丙烯酸类单体;苯乙烯、乙烯基甲苯、乙烯基吡啶、乙烯基己内酯、乙烯基咪唑、α-甲基苯乙烯、乙酸乙烯酯等乙烯基单体等。其中,从分子量的控制变得容易的角度出发,优选为α-甲基苯乙烯。
(高分子分散剂的组成、物性)
高分子分散剂(聚合物)中,结构单元(1)占所有结构单元的总和的比例为3~55质量%,优选为5~50质量%。结构单元(1)的比例小于3质量%时,在碳材料上的吸附变得不充分。另一方面,结构单元(1)的比例大于55质量%时,在有机溶剂中的溶解性变得不充分。
聚合物中,结构单元(2)占所有结构单元的总和的比例优选为30质量%以下,进一步优选为2~25质量%。需要说明的是,聚合物的胺值为100mgKOH/g以下,优选为3~90mgKOH/g。结构单元(2)的比例大于30质量%时,聚合物可能发生着色。
聚合物中,结构单元(3)占所有结构单元的总和的比例为45~90质量%,优选为50~85质量%。即,结构单元(3)是在聚合物中较多含有的结构单元。通过较多含有结构单元(3),聚亚烷基二醇链会被致密配置。因此,若作为高分子分散剂的聚合物吸附在碳材料上,则致密配置的聚亚烷基二醇链成为位阻,阻碍碳材料之间的接近,能够使碳材料稳定地分散。
聚合物中的结构单元(3)的比例小于45质量%时,不会形成充分的位阻,难以提高分散性。另一方面,结构单元(3)的比例大于90质量%时,由于构成结构单元(3)的大分子单体的反应性稍差,因此,有时不聚合而残留。
聚合物中,结构单元(4)占所有结构单元的总和的比例为0.5~20质量%,优选为0.6~16质量%。结构单元(4)的比例大于0.5质量%时,其他结构单元的含量会相对减少,因此作为分散剂的功能会下降。
结构单元(1)、结构单元(2)和结构单元(3)分别由通式(1-1)、通式(2-1)和通式(3-1)所示,结构单元(4)含有源自α-甲基苯乙烯的结构单元由于可以制成即使碳材料为高浓度也更难以再聚集,更稳定地分散的碳材料分散液,因而优选。
用作高分子分散剂的聚合物的、通过凝胶渗透色谱(GPC)测定的聚苯乙烯换算的数均分子量(Mw)为5000~20000,优选为10000~15000。聚合物的数均分子量小于5000时,源自大分子单体的结构单元(3)的导入量少,无法得到充分的分散稳定性。另一方面,聚合物的数均分子量大于20000时,使碳材料分散所需的高分子分散剂的量会变得过多,同时得到的碳材料分散液的粘度会变得过高。
(高分子分散剂的合成方法)
作为高分子分散剂的聚合物可以通过现有公知的方法合成。例如,可以通过现有公知的自由基聚合法;使用硫醇等链转移剂调整分子量的聚合法、原子转移自由基聚合法(ATRP法)、可逆加成断裂链转移聚合法(RAFT法)、氮氧稳定自由基聚合法(NMP法)、有机碲自由基聚合法(TERP法)、碘转移聚合法(ITP法)、可逆链转移催化聚合法(RTCP法)、可逆络合自由基聚合法(RCMP法)等活性自由基聚合法来合成。其中,由于可以使主链的分子量更均匀地一致,同时通过添加方法形成A-B嵌段共聚物,因此优选活性自由基聚合法。
聚合可以是热聚合和光聚合中的任一种,也可以将偶氮系自由基引发剂、过氧化物系自由基引发剂、光敏剂等添加到聚合反应系中。聚合形式可以是无溶剂聚合、溶液聚合和乳液聚合中的任一种,其中优选溶液聚合。通过在溶液聚合时使用与碳材料分散液中使用的有机溶剂相同的有机溶剂,可以将聚合反应后的聚合物直接用于碳材料分散液,因而优选。
例如,通过将上述各单体进行溶液聚合,能够得到目标聚合物(高分子分散剂)。需要说明的是,通过向将构成结构单元(2)的单体、构成结构单元(3)的单体、和构成结构单元(4)的单体聚合而得到的反应溶液中添加氯化苄、萘基甲基氯化物、炔基甲基氯化物、芘基甲基氯化物、萘基甲基溴化物等卤代烷基,可以使结构单元(2)中的氨基季铵盐化,将结构单元(2)转换为结构单元(1)。进一步地,通过添加双(三氟甲基砜)酰亚胺锂盐,双(七氟丁基砜)酰亚胺锂盐等,可以对构成季铵盐的阴离子(Cl-、Br-)进行离子交换。
(碳材料分散液)
碳材料分散液中的碳材料的含量优选设为15质量%以下,进一步优选设为0.5~12质量%。另外,高分子分散剂相对于100质量份碳材料的含量优选为10~200质量份,进一步优选为20~150质量份,特别优选为30~100质量份。高分子分散剂的量相对于碳材料过少时,分散性有时会变得稍不充分。另一方面,高分子分散剂的量相对于碳材料过多时,碳材料的比率相对降低,得到的碳材料分散液会变得容易增粘。
也可以使碳材料分散液中含有除高分子分散剂以外的树脂或添加剂等。作为除高分子分散剂以外的树脂,例如,可以列举出聚烯烃树脂、聚卤代烯烃树脂、聚酯树脂、聚酰胺树脂、聚酰亚胺树脂、聚醚树脂、聚乙烯基树脂、聚苯乙烯树脂、聚乙烯醇树脂、聚甲基丙烯酸酯树脂、聚氨酯树脂、聚环氧树脂、多酚树脂、聚脲树脂、聚醚砜树脂等。作为添加剂,可以列举出油溶性染料、颜料、紫外线吸收剂、光稳定剂、抗氧化剂、流平剂、消泡剂、防腐剂、防霉剂、光聚合引发剂、其它颜料分散剂等。
(碳材料分散液的制造方法)
通过使用作为高分子分散剂的聚合物使碳材料分散在包含有机溶剂的液体介质中,能够得到目标碳材料分散液。作为使用高分子分散剂对碳材料进行分散处理的方法,可以采用现有公知的方法。具体而言,可以采用分散机搅拌、三辊磨的混炼、超声波分散、珠磨机分散、使用乳化装置、高压均质机等的分散等分散方法。其中,由于分散效果好,因此优选珠磨机分散、超声波分散、使用高压均质机的分散。
(碳材料的分散性的评价方法)
作为评价碳材料分散液中的碳材料的分散性的方法,有如下所示的使用分光光度计的吸光度测定法。首先,制备以极低浓度含有碳材料的浓度已知的多个分散液,并且测定这些分散液在特定波长的吸光度,制作相对于碳材料的浓度描绘吸光度的校准曲线。接着,混合碳材料、有机溶剂和高分子分散剂,以适当的方法进行分散处理。其后,通过离心分离处理使未完全分散的碳材料沉降而分离除去,得到上清液。将得到的上清液稀释至可以测定吸光度的浓度后测定吸光度,根据校准曲线算出碳材料的浓度。并且,通过比较算出的分散液中的碳材料的浓度与碳材料的加入量,可以评价碳材料的分散性。
另外,通过长时间静置离心分离处理后的碳材料分散液,确认有无聚集物的方法也可以评价碳材料的分散性。进一步地,也可以将碳材料分散液滴加到玻璃板等上,使用电子显微镜等评价分散状态,也可以测定涂布并干燥碳材料分散液而形成的涂膜的电导率,根据是否达到规定的电导率来评价分散状态。
<碳材料分散液的使用>
上述的碳材料分散液可以作为碳材料以分散状态被包含的涂料、油墨、塑料制品等材料使用,期待其作为导电性材料、热导电性材料、防静电材料的用途。碳材料以分散的状态被包含的涂料或油墨例如可以通过以成为规定的涂料组成或油墨组成的方式,将溶剂、树脂和添加物等添加到碳材料分散液中进行涂料化或油墨化的方法来制备。另外,也可以通过向市售的涂料或油墨中添加碳材料分散液的方法来制备目标涂料或油墨。碳材料以分散的状态被包含的塑料制品例如可以通过向熔融状态的塑料材料中添加碳材料分散液并混合后,除去溶剂的方法来制造。另外,也可以通过向微粉末状态的塑料材料中添加碳材料分散液并混合后,除去溶剂,或使碳材料析出的方法来制造期望的塑料制品。
实施例
以下,基于实施例对本发明进行具体说明,但本发明并不限于这些实施例。需要说明的是,除非特别限定,实施例、比较例中的“份”和“%”都为质量基准。
<高分子分散剂(聚合物)的合成>
(合成例1:高分子分散剂D-1)
向安装有搅拌机、回流冷凝器、温度计和滴液漏斗的反应装置中加入单末端氨基化聚丙二醇聚乙二醇单甲醚(商品名“JEFFAMIN M2005”,Huntsman Corporation制,m+n=35(m=29,n=6),实测胺值28.05mgKOH/g)(M2005)100份(0.05mol)、丙二醇单甲醚乙酸酯(PGMAc)100份,在室温下搅拌10分钟使其均匀化。向另外的容器中加入甲基丙烯酸2-异氰酸根合乙酯(商品名“Karenz MOI”,昭和电工株式会社制)(MOI)7.75份(0.05mol)和PGMAc7.75份并混合,制备混合液。将制备的混合液用30分钟滴加到反应装置内使其反应。取样一部分反应溶液进行IR测定,确认了源自MOI的异氰酸酯基的消失和脲键的生成。另外,使用电位差自动滴定装置,使用0.1mol/L2-丙醇性盐酸溶液测定的产物的胺值为0.1mgKOH/g。由此,确认了氨基与异氰酸酯基的反应基本完成。得到的产物是在聚丙二醇聚乙二醇单甲醚(PPG/PEG)的单末端结合有甲基丙烯酰基的大分子单体(MCR-1)。使用水分计测定的MCR-1溶液的固体成分为50.0%。另外,通过以四氢呋喃(THF)为展开溶液的凝胶渗透色谱(GPC)测定的MCR-1的聚苯乙烯换算的数均分子量(Mn)为3400。
向安装有搅拌机、回流冷凝器、温度计和氮气导入管的反应装置中加入PGMAc49.6份、MCR-1溶液215.5份、α-甲基苯乙烯(αMS)1.8份、苯乙烯(St)25.1份、和甲基丙烯酸2-(N,N-二甲基氨基)乙酯(DMAEMA)19.2份(0.122mol),一边使氮气鼓泡一边加热。在内温达到70℃时,添加2,2’-偶氮二异丁酸二甲酯(商品名“V-601”,富士胶片和光纯药株式会社制)(V-601)3.0份,加热至75℃聚合4小时。添加V-601 0.5份,在75℃下进一步聚合4小时。取样一部分反应溶液测定的产物的Mn为8500,分散度(PDI)为1.65,峰顶分子量(PT)为14000,几乎没有观察到源自MCR-1的峰。反应溶液的固体成分为50.1%。另外,产物的胺值(以树脂纯度换算)为44.6mgKOH/g。
在室温条件下用30分钟滴加PGMAc7.8份和氯化苄(BzCl)7.8份(0.0616mol)的溶液。滴加后,加热至80℃维持5小时,得到含有高分子分散剂D-1的液体。高分子分散剂D-1的Mn为8700,PDI为1.66,PT为14400。含有高分子分散剂D-1的液体的固体成分为50.0%。高分子分散剂D-1的胺值(以树脂纯度换算)为21.0mgKOH/g,确认了反应几乎定量进行。得到的高分子分散剂D-1是以BzCl季盐化了50%的源自DMAEMA的氨基的树脂。
(合成例2~5:高分子分散剂D-2~D-5)
除了采用表1所示的配方以外,与上述合成例1同样地得到高分子分散剂D-2~D-5。表1中的缩略符号的含义如下。
·M41:单末端氨基化聚丙二醇聚乙二醇甲醚(商品名“Genamin M41/2000”,Clariant Corporation制,m+n=41(m=9,n=32))
·DMQ:甲基丙烯酸2-(N,N-二甲基氨基乙基)的苄基氯盐
·MMA:甲基丙烯酸甲酯
以合成例1为例说明表1中的DMQ的组成的计算方法。聚合物中的DMAEMA(Mw157.1)19.2份(0.122mol)与添加的BzCl(Mw126.6)7.8份(0.0616mol)定量反应。因此,生成了DMQ(Mw283.6)为0.0616mol×283.6=17.5份。以下,考虑季盐化率,同样地算出聚合物中的DMQ的组成。
以合成例1为例说明聚合物的胺值的理论值的计算方法。聚合物中的DMAEMA19.2份(0.122mol)的一半(0.0616mol)与BzCl反应而消失,因此残留在聚合物中的DMAEMA为0.122×0.5×157.1=9.6份。1g聚合物中含有9.6/(100+7.75+17.5+9.6+1.8+25.1)×100=0.059g的DMAEMA。因此,可以算出胺值为0.059/157.1×56.1×1000=21.1mgKOH/g。
表1:由合成例1~5得到的聚合物的组成和物性
(合成例6:高分子分散剂D-6)
向安装有搅拌机、回流冷凝器、温度计和氮气导入管的反应装置中加入PGMAc49.5份、MCR-1溶液216份、αMS1.8份、甲基丙烯酸苄基酯(BzMA)12.5份、和DMAEMA31.7份(0.202mol),一边使氮气鼓泡一边加热。在内温达到70℃时,添加V-601 3.0份,加热至75℃聚合4小时。添加V-601 0.5份,在75℃下进一步聚合4小时。取样一部分反应溶液测定的产物的Mn为10600,PDI为1.89,PT为20200,几乎没有观察到源自MCR-1的峰。反应溶液的固体成分为50.1%。另外,产物的胺值(以树脂纯度换算)为113.2mgKOH/g。
除了使用1-氯甲基萘(CMN)17.8份(0.101mol)代替BzCl以外,与上述合成例1同样地进行季盐化反应,得到含有高分子分散剂D-6的液体。高分子分散剂D-6的Mn为10900,PDI为1.88,PT为20300。含有高分子分散剂D-6的液体的固体成分为50.0%。高分子分散剂D-6的胺值(以树脂纯度换算)为32.8mgKOH/g。得到的高分子分散剂D-6是以CMN季盐化了50%源自DMAEMA的氨基的树脂。
(合成例7和8:高分子分散剂D-7和D-8)
除了采用表2所示的配方以外,与上述合成例6同样地得到高分子分散剂D-7和D-8。表2中的缩略符号的含义如下。
·CMA:9-氯甲基蒽
·CMP:1-氯甲基芘
·PME-4000:甲基丙烯酸末端甲氧基聚乙二醇(商品名“BLEMMER PME-4000”,日油株式会社制,m=0,n=90)
·NQ:甲基丙烯酸2-(N,N-二甲基氨基乙基)的1-氯甲基萘盐
·AQ:甲基丙烯酸2-(N,N-二甲基氨基乙基)的9-氯甲基蒽盐
·PQ:甲基丙烯酸2-(N,N-二甲基氨基乙基)的1-氯甲基芘盐
表2:由合成例6~8得到的聚合物的组成和物性
(合成例9:高分子分散剂D-9)
向安装有搅拌机、回流冷凝器和温度计的反应装置中加入含有高分子分散剂D-2的液体100.0份(固体成分50.0%)和PGMAc150.0份,搅拌而制成均匀的溶液。添加双(三氟甲烷磺酰基)酰亚胺锂(TFSILi)5.04份(0.0176mol,相对于DMQ为30%)并使其溶解。由此,生成以双(三氟甲烷磺酰基)酰亚胺阴离子(TFSI)为抗衡离子的季铵盐,得到含有高分子分散剂D-9的液体。含有高分子分散剂D-9的液体的固体成分为21.5%。高分子分散剂D-9的胺值(以树脂纯度换算)为21.8mgKOH/g。想要通过GPC测定高分子分散剂D-6的Mn时,强烈地吸附在色谱柱上,未能准确测定。TFSILi与等摩尔的DMQ反应时,生成等摩尔的LiCl(Mw42.4)。因此,通过TFSILi与DMQ的反应生成了季盐的量可以如下算出。
0.0176mol×(283.7+287.1)-0.0176mol×42.4=9.30份
(合成例10和11:高分子分散剂D-10和D-11)
除了采用表3所示的配方以外,与上述合成例9同样地得到高分子分散剂D-10和D-11。表3中的缩略符号的含义如下。
·DMTFSI:DMQ的氯化物离子盐交换成双三氟甲烷磺酰亚胺的季盐
·DMNFSI:DMQ的氯化物离子盐交换成双九氟丁烷磺酰亚胺的季盐
·NTFSI:NQ的氯化物离子盐交换成双三氟甲烷磺酰亚胺的季盐
表3:由合成例9~11得到的聚合物的组成和物性
(比较合成例1:高分子分散剂HD-1)
除了采用表4所示的配方,和使用滴液漏斗用1小时滴加αMS和St以外,与上述合成例1同样地进行聚合。取样一部分反应溶液测定的产物的Mn为18900,PDI为1.85,PT为34300。反应溶液的固体成分为50.5%。另外,产物的胺值(以树脂纯度换算)为28.5mgKOH/g。
在室温条件下用30分钟滴加PGMAc7.8份和BzCl7.8份(0.0616mol)的溶液。滴加后,加热至80℃维持5小时,得到含有高分子分散剂HD-1的液体。高分子分散剂HD-1的Mn为19500,PDI为1.84,PT为34800。含有高分子分散剂HD-1的液体的固体成分为50.4%。高分子分散剂HD-1的胺值(以树脂纯度换算)为13.1mgKOH/g。
(比较合成例2和3:高分子分散剂HD-2和HD-3)
除了采用表4所示的配方以外,与上述比较合成例1同样地得到高分子分散剂HD-2和HD-3。表4中的缩略符号的含义如下。
·M600:单末端氨基化聚丙二醇聚乙二醇单甲醚,商品名“JEFFAMINM600”,Huntsman Corporation制,m+n=9(m=9,n=0)
·NaBF4:四氟硼酸钠
·DMBF:DMQ的氯化物离子盐交换成四氟硼酸根离子的季盐
表4:由比较合成例1~3得到的聚合物的组成和物性
※:在NaBF4与DMQ进行盐交换反应时稀释的PGMAc的量
<碳纳米管分散液的制造>
(实施例1:CNT分散液-1)
向树脂制容器中加入碳纳米管(CNT)(平均直径:15nm,平均长度:3.0μm,MWNT)2.0份、PGMAc94.01份、和含有高分子分散剂D-1的液体(固体成分:50.1%)3.99份。CNT虽然被有机溶剂湿润,但是保持原来的形状沉入容器的底部的状态,上清液是透明的。向容器中加入搅拌子,通过磁力搅拌器搅拌,同时,使用超声波分散机照射60分钟超声波(功率300W)。通过照射超声波,液体均匀地变黑,成为CNT的聚集状态解除的状态。通过离心分离处理使未充分分散的固体物质沉降而分离除去,得到CNT分散液-1。
(实施例2:CNT分散液-2)
向树脂制容器中加入CNT2.0份、PGMAc94.00份、和含有高分子分散剂D-2的液体(固体成分:50.0%)4.00份。CNT虽然被有机溶剂湿润,但是保持原来的形状沉入容器的底部的状态,上清液是透明的。使用均质机以8000rpm搅拌60分钟。通过使用均质机搅拌,液体均匀地变黑,成为CNT的聚集状态解除的状态。通过离心分离处理使未充分分散的固体物质沉降而分离除去,得到CNT分散液-2。
(实施例3:CNT分散液-3)
向树脂制容器中加入CNT2.0份、PGMAc94.02份、含有高分子分散剂D-3的液体(50.2%)3.98份、和直径的氧化锆珠150份。CNT虽然被有机溶剂湿润,但是保持原来的形状沉入容器的底部的状态,上清液是透明的。使用Scandex分散处理60分钟。通过使用Scandex进行分散处理,液体均匀地变黑,成为CNT的聚集状态解除的状态。通过离心分离处理使未充分分散的固体物质沉降而分离除去,得到CNT分散液-3。
(实施例4~11、比较例1~3:CNT分散液-4~14)
除了使用表5所示的配方,同时使用表5所示的分散机进行分散处理以外,与上述实施例1~3同样地,得到CNT分散液-4~14。
表5:CNT分散液的制备
※:含有高分子分散剂的液体的量
<评价(1):CNT分散液的评价>
使用E型粘度计,测定刚分散后的CNT分散液在25℃下的粘度。另外,对CNT分散液进行离心分离处理。并且,使用分光光度计测定和算出离心分离后的CNT分散液的CNT浓度。需要说明的是,计算CNT浓度时,使用测定浓度已知的样品的吸光度而制作的校准曲线。进一步地,算出分散稳定度(离心分离后的CNT浓度/设计时的CNT浓度(%))。另外,将离心分离处理后的CNT分散液静置7天,目视确认静置后的CNT分散液的状态。将结果示于表6中。
表6:CNT分散液的评价结果
<纳米石墨烯分散液的制造>
(实施例12:NGR分散液-1)
向树脂制容器中加入纳米石墨烯(NGR)(平均直径:5μm,平均厚度:6~8nm)5.0份、PGMAc85.02份、和含有高分子分散剂D-1的液体(固体成分:50.1%)9.98份。向容器中加入搅拌子,通过磁力搅拌器搅拌,同时,使用超声波分散机照射60分钟超声波(功率300W),得到作为粘性液体的NGR分散液-1。
(实施例13和14,比较例4和5:NGR分散液-2~5)
除了采用表7所示的配方,同时使用表7所示的分散机进行分散处理以外,与上述实施例12同样地,得到NGR分散液-2~5。
表7:NGR分散液的制备
※:含有高分子分散剂的液体的量
<评价(2):NGR分散液的评价>
使用E型粘度计,测定NGR分散液在25℃下的粘度。另外,使用动态光散射式粒度分布装置,测定NGR分散液中的颗粒的中值直径(D50)。进一步地,使用动态光散射式粒度分布装置,测定NGR分散液中的颗粒的粒度分布,确认了有无聚集物。将结果示于表8中。
表8:NGR分散液的评价结果
<碳纳米纤维分散液的制造>
(实施例15:CNF分散液-1)
向树脂制容器中加入碳纳米纤维(CNF)(商品名“VGCF-H”,昭和电工株式会社制,平均直径:150nm,平均长度:6.0μm)2.0份、二乙二醇二乙醚(DEDG)(商品名“DEDG”,日本乳化剂株式会社制)94.01份、高分子分散剂D-1(固体成分:50.1%)3.99份、和直径的氧化锆珠150份。CNF虽然被有机溶剂湿润,但是保持原来的形状沉入容器的底部的状态,上清液是透明的。使用超声波分散机分散处理60分钟。通过超声波分散机进行分散处理,液体均匀地变黑,成为CNF的聚集状态解除的状态。通过离心分离处理使未充分分散的固体物质沉降而分离除去,得到CNF分散液-1。
(实施例16和17、比较例6:CNF分散液-2~4)
除了采用表9所示的配方,同时使用表9所示的分散机进行分散处理以外,与上述实施例15同样地得到CNF分散液-2~4。
表9:CNF分散液的制备
※:含有高分子分散剂的液体的量
<评价(3):CNF分散液的评价>
使用E型粘度计,测定刚分散后的CNF分散液在25℃下的粘度。另外,离心分离处理CNF分散液。并且,使用分光光度计测定和算出离心分离后的CNF分散液的CNF浓度。需要说明的是,计算CNF浓度时,使用测定浓度已知的样品的吸光度而制作的校准曲线。进一步地,算出分散稳定度(离心分离后的CNF浓度/设计时的CNF浓度(%))。另外,将离心分离处理后的CNF分散液静置7天,目视确认静置后的CNF分散液的状态。将结果示于表10中。
表10:CNF分散液的评价结果
<碳黑分散液的制造>
(实施例18:CB分散液-1)
向树脂制容器中加入碳黑(CB)(商品名“#1000”,三菱化学株式会社制)20份、PGMAc68.02份、含有高分子分散剂D-1的液体(固体成分:50.1%)11.98份、增效剂(铜酞菁衍生物,商品名“Solsperse 12000”,Lubrizol Corporation制)1.0份、和直径的氧化锆珠150份。使用超声波分散机分散处理30分钟,得到CB分散液-1。
(实施例19和20、比较例7:CB分散液-2~4)
除了采用表11所示的配方,并且使用表11所示的分散机进行分散处理以外,与上述实施例18同样地得到CB分散液-2~4。
表11:CB分散液的制备
※:含有高分子分散剂的液体的量
<评价(4):CB分散液的评价>
使用E型粘度计,测定刚分散后的CB分散液在25℃下的粘度。另外,使用动态光散射式粒度分布装置,测定CB分散液中的颗粒的中值直径(D50)。进一步地,使用E型粘度计,测定在45℃下保存7天后的CB分散液在25℃下的粘度。将结果示于表12中。
表12:CB分散液的评价结果
<CNT分散油墨涂膜的制造和评价>
(应用例1)
向实施例1中得到的CNT分散液-1中,添加相对100份CNT而言丙烯酸树脂的量为100份的量的丙烯酸树脂溶液(甲基丙烯酸苄基酯/甲基丙烯酸共聚物,Mn:7500,酸值:100mgKOH/g,PGMAc溶液,固体成分:40%)。以CNT浓度为1%的方式添加PGMAc进行稀释,得到CNT分散油墨-1。在厚度100μm的PET薄膜的表面上使用棒涂机将所得油墨以平均膜厚成为5μm的方式涂布后,在130℃下干燥30分钟,形成导电性的涂膜。使用电阻率计(商品名“Hiresta”,NITTOSEIKO ANALYTECH公司制)测定涂膜的表面电阻值。将结果示于表13中。
(应用例2~4、比较应用例1)
除了使用表13所示种类的CNT分散液以外,与上述应用例1同样地分别制备CNT分散油墨-2~5。并且,分别使用制备的CNT分散油墨,与上述应用例1同样地形成导电性的涂膜,测定表面电阻值。将结果示于表13中。
表13:CNT分散油墨涂膜的特性
<NGR分散油墨涂膜的制造>
(应用例6)
向实施例12中得到的NGR分散液-1中,添加相对于100份NGR而言丙烯酸树脂的量为100份的量的丙烯酸树脂溶液(甲基丙烯酸苄基酯/甲基丙烯酸共聚物,Mn:7500,酸值:100mgKOH/g,PGMAc溶液,固体成分:40%)。以NGR浓度为3%的方式添加PGMAc进行稀释,得到NGR分散油墨-1。在厚度100μm的PET薄膜的表面上使用棒涂机将所得油墨以平均膜厚成为5μm的方式涂布后,在130℃下干燥30分钟,形成导电性的涂膜。使用电阻率计(商品名“Hiresta”,NITTOSEIKO ANALYTECH公司制)测定涂膜的表面电阻值。将结果示于表14中。
(应用例7和8、比较应用例2)
除了使用表14所示种类的NGR分散液以外,与上述应用例6同样地分别制备NGR分散油墨-2~4。并且,分别使用制备的NGR分散油墨,与上述应用例6同样地形成导电性的涂膜,测定表面电阻值。将结果示于表14中。
表14:NGR分散油墨涂膜的特性
<将CNF混炼至树脂中>
(应用例9)
向烧杯中加入溶剂(甲醇/水=1/1)3000份。一边用分散器搅拌,一边缓缓加入实施例15中得到的CNF分散液-1,使被高分子分散剂被覆的CNF(树脂被覆CNF)析出。过滤析出的树脂被覆CNF后,使用甲醇和水清洗。使用干燥机干燥,得到树脂被覆CNF(固体成分99.5%)。
混合橡胶改性聚苯乙烯树脂、和相对于100份橡胶改性聚苯乙烯树脂为2份的树脂被覆CNF。使用安装有T型模的Labo Plastomill(东洋精机制作所制)挤出成形,制造厚度约0.5mm、宽度100mm的片状的评价用样品。对制造的评价用样品进行冲压,制作厚度约20μm的片材。使用光学显微镜观察制作的片材,结果未观察到CNF的聚集物。进一步地,测定制作的片材的表面电阻值,结果为5.26×108Ω/□。
(比较应用例3)
除了使用比较例6中得到的CNF分散液-4代替CNF分散液-1以外,与上述应用例9同样地制造片状的评价用样品。进一步地,对制造的评价用样品进行冲压,制作厚度约20μm的片材。使用光学显微镜观察制作的片材,结果观察到存在很多CNF的聚集物。进一步地,测定制作的片材的表面电阻值,结果为8.38×1010Ω/□。
产业上的可利用性
本发明的碳材料分散液除了涂料、油墨、塑料制品以外,还可以作为用于制造电池材料、电子部件托盘、IC芯片用罩、电磁波屏蔽器、汽车用构件、机器人用部件等各种制品的材料。
Claims (4)
1.一种碳材料分散液,其含有:选自由碳黑、碳纤维、碳纳米管、石墨和石墨烯组成的组中的至少1种的碳材料;有机溶剂;和高分子分散剂,
所述高分子分散剂为具有3~55质量%下述通式(1)所示的结构单元(1)、45~90质量%下述通式(3)所示的结构单元(3)、和0.5~20质量%与这些结构单元连接的其他结构单元(4)的聚合物,其中,所有结构单元的总和设为100质量%,
所述高分子分散剂的胺值为100mgKOH/g以下,数均分子量为5000~20000,
所述通式(1)中,R表示氢原子或甲基,A表示O或NH,B表示亚乙基或亚丙基,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、或双(九氟丁烷磺酰)亚胺,p表示任意的重复数;
所述通式(3)中,R表示氢原子或甲基,A表示O或NH,Q表示亚乙基或甲基亚乙基,Y表示O、NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基,r表示任意的重复数。
3.根据权利要求2所述的碳材料分散液,其中,所述结构单元(1)、所述结构单元(2)和所述结构单元(3)分别由下述通式(1-1)、下述通式(2-1)和下述通式(3-1)表示,
所述结构单元(4)包含源自α-甲基苯乙烯的结构单元,
所述通式(1-1)中,R1和R2相互独立地表示甲基或乙基,Ar表示苯基、萘基、蒽基或芘基,X表示氯原子、溴原子、双(三氟甲基)磺酰亚胺、双(九氟丁烷磺酰)亚胺,p表示任意的重复数;
所述通式(2-1)中,R1和R2相互独立地表示甲基或乙基,q表示任意的重复数;
所述通式(3-1)中,Y表示NHCOO或NHCONH,m和n相互独立地表示0以上的平均重复单元数、并且m+n=20~100,R3表示碳原子数1~18的烷基、芳基或烷基芳基,r表示任意的重复数。
4.根据权利要求1~3中任一项所述的碳材料分散液,其中,所述碳材料的含量为15质量%以下,
相对于100质量份所述碳材料,所述高分子分散剂的含量为10~200质量份。
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