CN107428953A - 碳纳米结构预共混物及其应用 - Google Patents
碳纳米结构预共混物及其应用 Download PDFInfo
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- CN107428953A CN107428953A CN201680018767.4A CN201680018767A CN107428953A CN 107428953 A CN107428953 A CN 107428953A CN 201680018767 A CN201680018767 A CN 201680018767A CN 107428953 A CN107428953 A CN 107428953A
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Classifications
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- C08J3/223—Packed additives
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/152—Fullerenes
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
一种制备纳米结构的碳,例如纳米管,富勒烯,或石墨烯和粒子固体,例如炭黑,石墨材料或玻璃状碳的“预共混物”的方法,该方法牵涉湿式混合,和接着任选地干燥,以除去液体介质。该预共混物可以是芯‑壳粉末材料形式,其中纳米结构的碳作为在粒子固体芯上的壳。该预共混物可提供单壁纳米管在乙烯‑α‑烯烃弹性体组合物内尤其改进的分散,从而导致来自纳米管的改进的增强。改进的弹性体组合物可显示出模量和断裂伸长率二者的同时改进。该弹性体组合物可形成为有用的橡胶制品。
Description
发明背景
1.发明领域
本发明一般地涉及在聚合物内分散诸如纳米管之类的碳纳米结构,例如以制造弹性体组合物的方法,形成用于它的碳纳米结构预共混物的方法,和所得预共混物和组合物的应用。
2.现有技术的说明
由于以缠结的纤维束形式生产碳纳米管("CNT"),因此使它们在聚合物内分散是其用作增强添加剂的关键步骤。使用了许多方法,以获得具有分散碳纳米管的聚合物。这些方法是在热塑性树脂内熔体共混CNT,在CNT存在下聚合,高剪切混合,化学改性CNT和使用表面活性剂。
关于在橡胶或弹性体聚合物内混合碳纳米管,非常难以在与大多数弹性体或橡胶一样高粘度的基质材料内分散CNT。施加热量没有显著足够地降低聚合物的粘度,就如同它在塑料内熔体共混一样。需要改进在橡胶内CNT分散性的方法。
美国专利No.7,785,701B2公开了一种碳纤维复合材料,它包括弹性体和在该弹性体内分散的碳纳米纤维,其中该弹性体具有不饱和键或者对碳纳米纤维具有亲和性的基团。当弹性体对纳米纤维的亲和性高时,据报道通过混合剪切力,例如在开炼机上容易分散。据报道对于诸如EPDM之类的非极性弹性体,分散并不容易。相对于不具有纳米纤维的组合物,所得开炼机混合的组合物显示出增加的模量和强度,但伸长率下降,这是许多增强填料的典型特征。
EP2,138,535 Bl公开了一种可硫化组合物,其含有特定氢化的羧化腈类橡胶(HXNBR),交联剂和碳纳米管,和这种组合物的制备方法。该文中报道了溶剂混合,熔体混合和喷雾干燥工艺用作加工方法,以制备一些橡胶/CNT复合材料。在密炼机和双辊磨内在HXNBR中常规地混合多壁碳纳米管("MWCNT")的实例。所得组合物显示出增加的模量和强度,但伸长率基本上相同。
参考2014年4月2日提交的,标题为Method for Rubber Reinforced With CarbonNanotubes的申请人的未决美国专利申请序列No.14/243,634。
发明概述
本发明涉及通过形成含碳纳米结构的预共混物组合物,在弹性体内分散诸如纳米管之类的碳纳米结构的改进方法,和所得弹性体组合物以及由其制造的制品。
通过在溶剂内悬浮或溶解CNT,或其他碳纳米结构材料,并与载体材料,例如炭黑共混,接着干燥,可在载体材料内和周围分散CNT,或者贯穿CNT网络,分散载体材料。已发现,这一预共混物辅助CNT在橡胶,特别地非极性弹性体,例如乙烯-α-烯烃弹性体内分散。结果,可实现模量,伸长率和剪切的改进。CNT可增加模量,同时增加断裂伸长率和撕裂性能的事实认为是新的且有利的结果。使用炭黑作为载体粒子固体可容易地掺入到已有的橡胶工艺中且可以是成本合算的。
本发明涉及一种方法,该方法包括下述步骤:通过在液体介质内分散碳纳米结构,形成碳预共混物,与粒子固体,例如炭黑混合,并干燥,以除去液体,导致纳米结构和材料的预共混物,例如CNT和炭黑的预共混物。然后可在聚合物基质,例如弹性体基质内分散预共混物。本发明还涉及所得聚合物或弹性体或橡胶组合物和由该组合物制造的制品,例如轮胎,传动带,运输带或软管。
本发明的方法可包括在溶剂内悬浮或溶解CNT和载体粒子,例如炭黑二者,混合和最后干燥它们。本发明的方法可导致本发明的CNT-涂覆的粒子或者用其他碳纳米结构材料涂覆的粒子,以形成预共混物。
取决于CNT和载体粒子二者的尺寸和用量,可形成由粒子在其内分散的CNT网络组成的结构替代CNT-涂覆的粒子。
CNT/炭黑预共混物可提供单壁碳纳米管("SWCNT")在乙烯-α-烯烃橡胶组合物内特别改进的分散,从而导致来自SWCNT的改进分散。
在本发明的弹性体组合物内CNT或其他纳米结构碳的用量可以是从0.5,1或2wt%一直到2,3,4或5wt%。在预共混物内的CNT用量可以是从1%,或5%,或7%一直到约20%,或一直到30%,或一直到50wt%,基于预共混物的重量。
可将本发明的弹性体组合物形成为有用的橡胶制品,例如轮胎,皮带,软管或振动控制组件。传动带没有限制地包括V-带,多楔带,同步带,平带,和类似物。
含有一定量CNT预共混物的改进的弹性体组合物可显示出模量和断裂伸长率二者的同时改进。该组合物也可显示出撕裂强度,割口或裂纹生长速率和抗疲劳性的改进。
前面相当广义地概述了本发明的特征和技术优点,以便可更好地理解随后本发明的详细说明。下文将描述本发明的额外特征和优点,它们形成本发明权利要求的主题。本领域技术人员应当理解,作为改性或设计实施本发明相同目的的其他结构的基础,可容易地实现所公开的概念和具体实施方案。本领域技术人员还应当意识到,这种等价的结构没有脱离所附权利要求列出的本发明范围。认为当结合附图考虑时,根据下述说明,将更好地理解就其组织和操作方法二者来说,属于本发明特性的新型特征,连同进一步的目的和优点。然而,要清楚地理解,仅仅为了阐述和说明目的来提供每一附图且并不意欲作为限制本发明的定义。
附图简述
将附图引入说明书并形成说明书的一部分,其中相同的数字表示相同的部件,所述附图阐述了本发明的实施方案,且与说明书一起,起到解释本发明原理的作用。
图1是本发明方法的一个实施方案的流程图。
图2是由在乙醇内以13:1的比值混合N550炭黑和SWCNT组成的预共混物材料在785nm下测量的拉曼光谱。
图3A是由在乙醇内以13:1的比值混合N550炭黑和SWCNT组成,接着过滤,和在60℃下干燥过夜的预共混物材料放大2,500倍的扫描电镜(SEM)图像。
图3B是图3A的材料放大35,000倍的SEM;
图3C是图3A的材料放大120,000倍的SEM;和
图3D是根据本发明的一个实施方案,图3A的材料放大l20,000倍的另一SEM。
图4是根据本发明的一个实施方案用单壁碳纳米管涂覆的聚合物珠粒的SEM。
图5是仅仅炭黑加入到橡胶中的对照橡胶胶料放大35,000倍的FE-SEM图像。
图6是通过单独地添加N550炭黑和SWCNT到橡胶中制造的对照橡胶胶料放大35,000倍的FE-SEM图像。
图7是根据本发明的一个实施方案,具有在乙醇内湿式混合并加入到橡胶中的N550炭黑/SWCNT预共混物的橡胶胶料放大35,000倍的FE-SEM图像。
图8是通过在o-二氯苯内混合N220炭黑/SWCNT(5:1)制备的炭黑/SWCNT预共混物放大40,000倍的SEM图像。
图9是通过在o-二氯苯内混合N220炭黑/SWCNT(7:1)制备的炭黑/SWCNT预共混物放大40,000倍的SEM图像。
图10A是通过在o-二氯苯内混合N550炭黑/SWCNT(5:1)制备的炭黑/SWCNT预共混物放大25,000倍的SEM图像。
图10B是图10A的预共混物放大70,000倍的SEM图像。
图11A是通过在o-二氯苯内混合N550炭黑/SWCNT(7:1)制备的炭黑/SWCNT预共混物放大25,000倍的SEM图像。
图11B是图11A的预共混物放大70,000倍的SEM图像。
详细说明
本发明的方法和弹性体组合物包括形成碳纳米结构,例如CNT,与粒子固体,例如炭黑的预共混物的方法,和在弹性体内分散该预共混物的进一步的方法。碳纳米结构是至少一个尺寸为至少1至数纳米数量级的碳-基材料。它们包括,但不限于,结构化纳米碳,例如单壁,双壁,很少-壁(few-walled)或多壁碳纳米管,石墨烯,很少-壁的石墨烯,氧化石墨烯,富勒烯和结构化碳的形式及其化学衍生物。它们包括富勒烯分子,例如C60,C70,C84等,和在富勒烯笼内部或外部含有另一个原子或多个原子或者含有一个或多个官能团的富勒烯分子。其他碳纳米结构包括具有明显富勒烯特征的由弧形碳片或层构成的碳的球状体或小球体。在六元和有时七元环当中,通过存在导致弧形碳片的五元碳环,记录(note)富勒烯特征。碳纳米结构的化学衍生物包括以上所述的任何碳-基材料,它们被官能化,即具有添加的基团,例如通过加成反应。此外,碳纳米结构包括以上所述的任何结构化纳米碳的结构化链段。预共混物是在另一混合工艺,例如橡胶组合物混合工艺之前制造的材料的混合物。预共混物因此与其他所需的成分一起混合到弹性体内,制造可用于弹性体制品的适合于模塑的弹性体组合物。图1示出了根据本发明一个实施方案的方法的流程图。预共混物有时也称为“预分散体”或简单地“共混物”。
在图1中,方法100包括共混112,混合120,和制造制品124的步骤。共混步骤112包括载体材料102,例如炭黑,碳纳米管104,载体液体介质106和任选地其他添加剂105作为输入物。湿共混112步骤可包括各种顺序的添加和/或混合。在一个优选的实施方案中,CNT104首先分散在液体介质106中,接着添加粒子固体102。在另一实施方案中,CNT 104和粒子固体106各自分散在单独的液体介质106中,然后结合这两种分散体。湿共混112后接着干燥118。在共混和干燥步骤之后,可将所得CNT预共混物119与所需的聚合物或橡胶成分122一起引入到混合步骤120中,获得适合于制造制品124的橡胶胶料。混合步骤120可任选地包括多个混合工艺步骤和/或多个成分的添加。在其他实施方案中,在图1中的CNT可被以上定义的一些其他碳纳米结构或其混合物替代。
碳纳米管(CNT)是横跨纤维具有小尺寸和合理地大的L/D比的非常结实的分子纤维。若干合成方法是可能的,其中在所使用的比较常见的方法中,例如在美国专利No.7,887,775和美国专利No.7,396,520中公开的化学蒸汽沉积(CVD),电弧放电(EAD)和燃烧。尺寸取决于制造工艺。单壁碳纳米管(SWCNT)的直径范围可以是0.5至6纳米(nm),长度范围可以是0.1至5微米(μm),优选长度为0.5至5μm。由折叠成圆柱体的单片石墨烯形成单壁碳纳米管。多壁碳纳米管(MWCNT)的直径范围为2至110nm,和长度为0.1至1000μm,优选0.1至50μm,且由在自身上卷起形成管道形状的多层石墨烯组成。这些尺寸变化取决于工艺和制造者。可在本发明的方法和组合物中使用单壁碳纳米管或者多壁碳纳米管,但优选单壁碳纳米管。
碳纳米管预共混物包括碳纳米管和粒子固体,例如炭黑。特别有用的粒子固体是在聚合物或弹性体组合物中常用作增强填料或者非-增强填料的那些,其中包括氧化硅,炭黑,粘土,白垩粉(whiting),各种金属氧化物和氢氧化物,和类似物。优选炭黑,因为它宽泛地在橡胶中使用且它与碳纳米管化学相容。适合于在本发明的方法中使用的炭黑的类型包括在ASTM D1765中确定的那些。两种合适的实例包括N550和N220,正如以下看到的。
在预共混物内CNT的用量可以是从1%,或5%,或7%一直到约50%,或一直到30%,或一直到20wt%,基于预共混物的重量。在预共混物内CNT的用量可以表达为材料对碳纳米管之比,和该比值可以是以重量计,约4:1至99:1或到20:1,或从6:1至15:1,或约9:1至约14:1。根据本文描述的方法,CNT可容易地与炭黑共混,和CNT/炭黑预共混物与乙烯-α-烯烃弹性体,例如EPDM非常相容。
术语“载体液体”或“液体载体”是指碳纳米管可在其内溶解,分散或悬浮的液体。可通过蒸发或干燥,除去载体液体,从而留下涂覆于炭黑上或者与炭黑混合的纳米管。合适的载体液体包括水或有机溶剂,其中包括醇,氯化脂族或芳族溶剂,酮,其他含氧或含卤素的烃液体,取代芳烃分子,烷基取代的芳烃,卤化取代分子,卤化烷烃,部分氢化的芳烃,烷基胺,环醚,o-二氯苯,甲苯,二甲苯,苯,二甲基甲酰胺("DMF"),氯化乙烯,氯仿,1,2,4-三甲基苯,1,2,3,4-四甲基苯,四氢呋喃,1,2-二溴苯,1,1,2,2-四氯乙烷,1,2,3,4-四氢萘,十八烷基胺,丙酮。可使用的其他液体包括例如基于通过表面活性剂稳定的水的体系,其中这种表面活性剂是选自胆酸钠,("NaDDBS",C12H25C6H4SO3Na),辛基苯磺酸钠(NaOBS;C8H17C6H4SO3Na),丁基苯磺酸钠("NaBBS";C4H9C6H4SO3Na),苯甲酸钠(C6H5CO2Na),十二烷基硫酸钠("SDS";CH3(CH2)11-OSO3Na),Triton(Dow Chemical Co.的商标)X-100("TX100";C8H17C6H4(OCH2CH2)n-OH;n为约10),十二烷基三甲基溴化铵("DTAB";CH3(CH2)11N(CH3)3Br),糊精,和聚苯乙烯-聚氧化乙烯二嵌段共聚物("PS-PEO")中的至少一种成员。其他非离子分散助剂,例如在国际申请No.PCT/US2010/045391和美国专利申请序列No.13/725,080中概述的那些可在水或溶剂-基体系中使用。也可在水或溶剂-基体系中使用温度调节剂,以便提高分散或溶液性能。以下看到的两种合适的实例包括乙醇和o-二氯苯。
术语聚合物包括热塑性,弹性体和热固性聚合物材料。术语橡胶和弹性体可以有时互换使用,但一般地橡胶暗含交联的弹性体材料,而某些弹性体一般地可以是热塑性或者可以交联。在本文中使用术语“橡胶”和“弹性体”是指形成弹性或橡胶状材料中的主要弹性成分的弹性或橡胶聚合物,而使用术语“橡胶组合物”和“弹性体组合物”指代主要的弹性成分和一种或多种其他配混成分,例如填料,纤维,抗降解剂,加工助剂,固化剂,固化促进剂,助剂(coagent),软化剂,增量剂和类似物的混合物。可使用任何合适的弹性体,其中没有限制地包括天然橡胶(NR),环氧化天然橡胶(ENR),异戊二烯橡胶(IR),苯乙烯-丁二烯橡胶(SBR),腈类橡胶(NBR),氢化腈类橡胶(HNBR),氯丁二烯橡胶(CR),乙烯-α-烯烃弹性体,例如乙烯丙烯橡胶(EPM或EPDM),乙烯丁烯橡胶(EBM)或乙烯辛烯橡胶(EOM),丁基橡胶(IIR),氯丁橡胶(CI IR),丙烯酸橡胶(ACM),硅橡胶(Q),氟橡胶(FKM),丁二烯橡胶(BR),环氧化丁二烯橡胶(EBR),表氯醇橡胶(ECO),浇铸聚氨酯弹性体(PU)或聚硫化物橡胶(T);热塑性弹性体,例如烯烃-基弹性体(TPO),聚氯乙烯-基弹性体(TPVC),聚酯-基弹性体(TPEE),聚氨酯-基弹性体(TPU),聚酰胺-基弹性体(TPEA)或苯乙烯-基弹性体(SBS),和类似物。可使用这些弹性体的混合物。该方法的实施方案尤其可用于乙烯-α-烯烃弹性体,其中包括难以分散的非极性弹性体,例如EPM或EPDM,EBM,或EOM。
制造CNT/炭黑预共混物的方法是在合适的液体内湿式混合它们。可在任何合适的混合器内或者采用任何合适的混合器进行混合,不管分批还是连续,例如密炼机,条状-刀片分批混合器,高-剪切分批混合器,单螺杆挤出机和双螺杆挤出机。然后可使用任何合适的干燥设备,干燥混合物,不管分批还是连续,例如喷雾干燥器,真空干燥器,转鼓式干燥器,带式干燥器,和类似物。可在干燥加工中包括过滤,以浓缩固体。
可根据配混聚合物,橡胶和弹性体的已知方法,将预共混物形式的预共混的碳纳米结构加入到聚合物或弹性体组合物中。例如,可使用分批密炼机,单螺杆挤出机,双螺杆挤出机,双辊磨,或类似物,将橡胶和它的各种成分与预共混物配混。可在各段中或者所有一次性添加各种成分。优选地,在多段中混合胶料,如果在分批混合器内的话。
除了掺入这种预共混物到弹性体或其他聚合物内以外,也可在许多其他应用中使用含例如碳纳米管,炭黑,石墨碳粒和或玻璃状碳粒的预共混碳纳米结构。这种扩展的应用尤其包括在电池组电极,特别地锂电池组电极,电池电解质组合物和在超级电容器中使用该预共混物。
以上描述的碳预共混物可在二次电池中以与活性材料和粘合剂的各种比例用作导电材料作为电池组电极的一部分。可与碳预共混物结合使用的普通的活性材料的实例是LiCoO2,LiNiO2,LiFeO2,LiMnO2,LiVO2,或组合,其中给定的过渡金属离子(Co,Ni,Fe,Mn和V)被其他过渡金属离子部分取代。
在没有受到粘合剂选择的情况下,可考虑的普通粘合剂尤其包括聚四氟乙烯,聚偏氟乙烯,聚乙烯,聚丙烯和合成橡胶。
为了混合碳预共混物的干燥形式与其他种类的导电,活性或电解质材料以供例如在电池组电解质组合物中使用,可使用宽范围的溶剂。例如,碳酸亚丙酯,碳酸亚乙酯,碳酸亚丁酯,碳酸二乙酯,碳酸二甲酯,碳酸甲乙酯和乙腈可单独或者与其他溶剂结合使用,形成浆液。
可使用一个范围的沉积技术,其中包括刮涂,印刷,棒涂或喷涂,在挠性聚合物基底或纸张上形成厚膜电极。
利用大表面积的CNT,也可使用本发明的碳预共混物例如作为电双层电容器(常常称为超级电容器)的一部分,其中包括与其他形式的碳,导电材料,电解质,溶剂和盐结合用作电解质。可与碳预共混物一起使用的电解质的一种示意性实例是单独或者与诸如四乙基四氟硼酸铵(C2H5)4NBF4结合使用的乙腈。
作为在本说明书通篇中各种详细地描述的使用碳的预共混物形式的另一实例,可将预共混物组合物以油漆,涂层或浆液形式施加到各种基底上,或者用作油漆,涂层或浆液的一种组分。
实施例
在第一实施例中,制备含N550炭黑和SWCNT的预共混物,评价CNT的预共混物是否随后可在EPDM弹性体组合物内辅助分散CNT。由Nano-C,Inc.of Westwood,Massachusetts提供单壁碳纳米管(SWCNT)。关于SWCNT的尺寸,直径范围为0.8至1.9nm,且较高丰度介于0.8至1.3nm。关于SWCNT束的长度,其范围为0.4至2微米,最大丰度为0.5至1微米。本文中提及的所有其他成分获自商业零售商且以提供时的形式使用。
单壁碳纳米管与N550炭黑的第一共混物实例具有7.18wt%的SWCNT含量,或13:1的炭黑对CNT比值。通过首先在乙醇内混合SWCNT(在35ml乙醇内1g SWCNT)和超声化15分钟,制备这一共混物。此外,在乙醇中以约30gm/l分散炭黑,并与IKA T25分散剂(以IKA商品名由IKA Works Inc.销售)混合15分钟。然后将CNT溶液加入到适量炭黑溶液中并与IKAT25分散剂混合另外15分钟。然后通过过滤除去溶剂,并分离碳预共混物材料,和在60℃烘箱内干燥过夜。然后评估所得产物的均化程度和同一性(identity),表征这一材料。
拉曼光谱结果(如图2所示)证明在共混物内存在这两种成分,且对于每一材料来说,显示出峰非常小的改性。RBM-(≈200至300cm-1)和G-(约1600cm-1)模式源自于SWCNT,而D-带(≈1300至1400cm-1)反映存在炭黑。由于这一观察结果单独仅仅表明该共混物含有这两种材料,而没有详细的形貌,随后通过SEM显微术检验该共混物。在图3中示出了由比值为13:1的N550炭黑和SWCNT组成的预共混物材料的SEM图像,其中包括放大(图3A)2500x,(图3B)35,000x和(图3C)与(图3D)120,000x。图3A-3D示出了具有独特形貌的预共混物材料,其中这两种成分材料紧密地混合。由于本文中使用的炭黑材料比纳米管的宽度大得多,因此,新材料由围绕炭黑材料的纳米管网络组成,或者换句话说,具有在其内分散的炭黑材料的纳米管网络。发现证据:这一独特预共混物结构提供随后纳米管在弹性体组合物内分散的改进。
由石墨,玻璃状或较小-结构(structure-less)碳组成的其他碳-基材料可用作载体粒子固体或其混合物来替代炭黑或者除了炭黑以外,使用它们。载体的材料形状可以是规则或不规则的。
可使用其他富勒烯或纳米结构的碳材料,例如球体富勒烯(C60,C70,...,C84,..),石墨烯,不管官能化与否,来替代碳纳米管。
当碳-基载体材料大于它们与其混合的材料的宽度和长度时,形成纳米管或其他富勒烯材料(“壳”)覆盖石墨,玻璃状或较小-结构“芯”的独特芯-壳材料。覆盖率可以是最多50%或50至100%。
碳-基或其他粒状芯材料的直径可以是20nm至20μm,而纳米炭壳材料的最长尺寸可以是0.7nm至2.0μm。
在图4中给出了用碳纳米管作为壳覆盖的芯的示意图,其中示出了用单壁碳纳米管涂覆的直径约1μm的聚合物珠粒。
预共混材料的一种最后的分析是测量共混物的电阻率。检查本体材料的电阻率并且该预共混物与纯纳米管本身几乎一样导电,尽管在该预共混物内纳米管的水平低。这一令人惊奇的结果表明,在没有使纳米管网络断裂的情况下,纳米管网络可通过相互分散的较大炭黑材料扩展。
本文中的橡胶配混使用内部体积为1571ml的常规B-本伯里氏实验室混合器。在第一系列的橡胶配混实施例中,如表1所示,对照弹性体组合物是100重量份以该商品名由Exxon Chemicals销售的Vis talon 706(EPM);相对于100份弹性体("phr"),60份N550炭黑,和5phr过氧化物固化剂(Vul-Cup 40KE)。该组合物还包括0.3phr延迟剂和1phr抗氧剂。混合这一组合物(对比例1)作为对照例(即,不具有CNT)。混合第二对比实例(对比例2)与一起加入到混合器内,但不是作为预共混物的50phr N550和3.87phr CNT。使用53.87phr7.18%前述SWCNT和炭黑的预共混物,混合本发明的实施例(实施例3),从而导致1.25体积%的CNT负载。在标准橡胶移动模具流变仪(moving die rheometer)("MDR")上,在170℃下进行固化研究(根据ASTM D-5289)。根据ASTM D-412,在室温和125℃下进行拉伸试验。所报道的结果包括“10%模量”,它是在10%应变下的应力,单位N/mm2。试验在室温("RT")下和在顺纹("w/g")方向上,除非另外指明。横纹试验表示为"x/g"。在表1中示出了配方和结果。可看出将SWCNT混合到橡胶组合物内产生下述结果。
对于具有炭黑和纳米管的两个样品来说,在170℃下观察到的MDR最大扭矩(MH)较低。与此同时,对于具有纳米管的两个样品来说,在这一温度下的最小扭矩(ML)高于对照例。在表1中通过t90表示在这些胶料上的固化速率信息。具有纳米管的胶料的固化时间显著小于对照胶料。这一趋势与针对前面在美国专利申请序列No.14/243,634中评价的蜡/碳纳米管分散体观察到的一致。
在添加碳纳米管情况下,这些胶料的门尼粘度(ML/132℃)(在比MDR低的温度下)显示出小的增加。对于掺入纳米管的任意路线来说,粘度实质上没有差别。
根据ASTM D-6601,在175℃下,在橡胶加工分析仪(RPA)上测定具有纳米管的两种胶料的动态模量。表1示出了对于采用MDR观察到的含纳米管的胶料来说相同的较低模量(G')。此处当纳米管与炭黑预共混时,所得材料比简单地单独添加两种材料略硬。这是使用炭黑/纳米管共混物的纳米管分散体的一定改进的指示。采用预共混这两种材料观察到的模量小幅增加伴随着滞后(tanδ)增加,但仅仅最多达到对照例的水平。
室温10%模量表明引入纳米管到胶料内模量增加,和这随着在配混之前,预共混两种材料而进一步增加。在每一情况下,最大增加是在顺纹方向上和在横纹方向上非常轻微。在高温下,模量增加微小,从而遵照由RPA和MDR数据表示的趋势。在高温下与对照例相比,不存在模量的显著下降,这在前面的蜡/CNT预分散体的研究中观察到。因此,预共混CNT和炭黑的方法提供比另一方法更好的温度稳定性。
断裂伸长率表明引入CNT到胶料内值得注意的增加,和当预共混CNT和炭黑时,额外的增加。这一趋势与来自加工的顺纹或横纹取向一致。在高温(125℃)下,该趋势相同,但在室温下增加全部较小。通过CNT还改进韧度。
撕裂性能(根据ASTM D-624的口型-C(die-C)撕裂强度)表明在添加CNT情况下稳定增加,和采用预共混进一步增加。此外,引入CNT的情况下,各向异性略微增加。在增加的温度下与对照例相比,撕裂也轻微增加。
这些胶料的肖氏A硬度实质上相同。
根据ASTM D-813,采用穿刺的样品,进行DeMattia试验。割口生长速率报道为达到1英寸割口宽度的外推兆周值,即Mcycles/in。DeMattia裂纹生长速率表明突出的改进,而与胶料内CNT的取向无关,如果有的话。这在125℃下评价,和尽管胶料劲度具有某些增加的事实,但发生了改进。
使用两个探针的单元,评价胶料的电性能。在胶料内具有CNT的两个样品表明改进的导电率,但两个样品之间不存在区分度。
最后,对这一系列的橡胶样品拍摄场-发射SEM(FE-SEM)显微照片。图5-7表明三个橡胶胶料在30,000x下的FE-SEM照片:图5示出了仅仅炭黑加入到橡胶中的对照例;图6示出了单独添加炭黑和SWCNT到橡胶中;和图7示出了在Nano-C下在液体中制备并加入到橡胶中的炭黑/SWCNT预共混物。具有仅仅炭黑的样品(图5)在表面上显示出炭黑。具有CNT的两个样品(图6-7)表明与橡胶相互作用并产生网状表面特征的碳纳米管。基于这些照片,认为与对比例2相比,实施例3的材料的纳米管的分散较好。
该实施例表明与炭黑预共混的CNT可改进橡胶的物理性能,例如断裂伸长率,模量,抗裂纹生长性和导电率,同时其他性能未受影响或者得到略微改进。
表1
1Ν 550;
21000 CPM,0.18°应变,175℃。
在第二系列的实施例中,如表2所示,使用与第一实施例相同的SWCNT。然而,在这一实施例中,使用不同的液体介质,制备不同比值的两种预共混物。使用o-二氯苯作为有机液体,制造CNT和炭黑的这些预共混物。通过使用IKA T25混合器,首先在o-二氯苯中以约30g SWCNT/L溶剂的浓度,混合SWCNT 15分钟,制备共混物。然后在o-二氯苯中在约20-30g/L溶剂的浓度下混合炭黑25分钟。最后,采用IKA T25混合器,结合适量的两种混合物并搅拌1小时。然后通过过滤,除去溶剂,并在70℃下真空干燥残留的湿共混物48小时。在这一系列中,研究共混物比值和炭黑类型的影响。在橡胶配方中使用两种共混物比值:5:1和13:1炭黑比CNT。使用两类炭黑N550和N220,它们主要是粒度不同。在图8-11中给出了在其于橡胶配方中使用之前,所得预共混物的SEM图像。图8和图9示出了分别在5:1和7:1比值下,在40,000倍放大下的N220炭黑/SWCNT预共混物。图10和图11示出了分别在5:1和7:1比值下的N550炭黑/SWCNT预共混物,其中图10A和11A在25,000倍放大下,和图10B与11B在70,000倍放大下。基础EPM弹性体组合物,橡胶混合和测试与针对第一系列的相同。在下表2中示出了所使用的橡胶配方和结果。
与图3A-3D和图8-11的SEM图像的检查一致,在湿共混工艺中,使用o-二氯苯似乎提供比使用乙醇更好的最终结果。这可例如通过比较表2中实施例6,7和10与前面表1中的实施例3的断裂伸长率看出。o-二氯苯共混物得到较高的伸长率,从而暗含比较坚韧的胶料。炭黑对CNT的较高比值与较低比值相比,似乎得到更好的性能,从而表明在弹性体内更好地分散,这可能是由于CNT网络通过炭黑更多地扩展导致的。DeMattia裂纹生长数据也表明o-二氯苯共混物得到比乙醇共混物甚至更好的结果。
表2
应当注意,对于实施例的胶料来说,断裂伸长率增加和10%模量的显著改进与文献中观察到的趋势相反。例如,实施例6和7显示出10%模量增加约20%,伴随着断裂伸长率增加60%。CB/SWCNT的组合还显示出在DeMattia试验中撕裂强度,割口生长速率的改进,和抗疲劳性的改进。认为模量和伸长率的同时改进归因于CNT在弹性体组合物内改进的分散,这非常难以量化。因此,本发明可通过相对于不具有CNT的相同组合物,模量(例如10%模量)和断裂伸长率的同时增加来表征。优选地,一种或两种性能的增加范围为至少20%,或至少30%,或至少50%。
也可注意到,橡胶的导电率似乎没有依赖于CNT的分散方法,仅仅依赖于它们足量的存在和所使用的炭黑类型。当所使用的炭黑并不非常导电时,我们观察到导电率的差异,从而与简单地添加SWCNT相比,有利于溶液共混CB/SWCNT。当炭黑非常导电,即为N220时,我们观察到小得多的差异。
因此,本发明在弹性体内使用炭黑/CNT预共混物来分散CNT的方法导致与现有技术的方法相比,改进的分散,从而导致在所得弹性体组合物内模量和伸长率同时增加。可使用本发明的弹性体组合物制造各种橡胶制品,例如皮带,软管,振动控制组件,轮胎,片状物品和类似物。
尽管详细地描述了本发明及其优点,但应当理解,可在没有脱离所附权利要求定义的本发明范围的情况下,在本文中做出各种变化,替代,和改变。而且,本申请的范围并不打算限制到说明书中描述的工艺,设备,制造,物质组合物,方式,方法和步骤的特定实施方案上。因为根据本发明的公开内容,本领域普通技术人员容易理解,可根据本发明实现目前已有或者随后开发的行使与本文描述的相应事实上方案基本上相同功能或实现基本上相同结果的工艺,设备,制造,物质组合物,方式,方法或步骤。因此,所附权利要求打算包括这种工艺,设备,制造,物质组合物,方式,方法或步骤在其范围内。可在不存在本文没有具体地公开的任何要素情况下,合适地实践本文公开的发明。
Claims (44)
1.在聚合物内分散碳纳米结构的方法,该方法包括:
在液体介质内湿式混合含有所述碳纳米结构和粒子固体的共混物;
干燥所述共混物,形成碳纳米结构和粒子的预共混物以便在常规的配混过程中加入到聚合物内。
2.权利要求1的方法,其中所述液体介质是有机液体。
3.权利要求1的方法,其中所述液体介质包括取代的芳烃分子,烷基取代的芳烃,卤化取代的分子,卤化烷烃,部分氢化的芳烃,烷基胺,环醚,o-二氯苯,二甲苯,苯,二甲基甲酰胺,氯化乙烯,氯仿,1,2,4-三甲基苯,1,2,3,4-四甲基苯,四氢呋喃,1,2-二溴苯,1,1,2,2-四氯乙烷,1,2,3,4-四氢化萘,十八烷基胺,丙酮及其混合物。
4.权利要求1的方法,其中所述液体介质是水或者通过表面活性剂稳定的水,其中这种表面活性剂是选自胆酸钠,辛基苯磺酸钠,丁基苯磺酸钠,苯甲酸钠,十二烷基硫酸钠,C8H17C6H4(OCH2CH2)n-OH,其中n为约10,十二烷基三甲基溴化铵,糊精,和聚苯乙烯-聚氧化乙烯二嵌段共聚物中的至少一种成员。
5.权利要求1的方法,其中所述粒子固体是炭黑。
6.权利要求1的方法,其中纳米结构的碳包括碳纳米管("CNT"),且其中所述预共混物包括与所述CNT的网络混合的粒子固体的材料。
7.权利要求6的方法,其中所述CNT是单壁碳纳米管。
8.权利要求6的方法,其中所述CNT是多壁碳纳米管。
9.权利要求1的方法,进一步包括混合所述预共混物到聚合物组合物内。
10.权利要求9的方法,其中在聚合物组合物内的主要聚合物是乙烯-α-烯烃弹性体。
11.权利要求10的方法,其中乙烯-α-烯烃弹性体中的α-烯烃是丙烯,丁烯或辛烯。
12.权利要求9的方法,进一步包括制造含有所述聚合物组合物的橡胶制品。
13.权利要求12的方法,其中所述橡胶制品是皮带,软管,轮胎或振动控制组件。
14.一种在弹性体内分散碳纳米管("CNT")的方法,该方法包括:
获得通过在液体介质中湿式混合CNT和炭黑、接着干燥而形成的CNT和炭黑的预共混物;
在所述弹性体内混合所述预共混物与其他成分,以形成弹性体组合物。
15.权利要求14的方法,进一步包括制造含有所述弹性体组合物的弹性体制品。
16.权利要求15的方法,其中所述弹性体制品是皮带,软管,轮胎或振动控制组件。
17.权利要求15的方法,其中所述弹性体制品是传动带。
18.权利要求14的方法,其中在该预共混物内炭黑对CNT的重量比范围为4:1至20:1。
19.权利要求14的方法,其中该预共混物包括在CNT网络内混合的炭黑材料。
20.权利要求14的方法,其中该预共混物包括具有在其内分散的炭黑材料的纳米管网络。
21.一种预共混物组合物,它包括通过在液体基质中湿式混合而制备的碳纳米结构和粒子固体。
22.权利要求21的预共混物组合物,其中该预共混物包括具有在其内分散的炭黑材料的纳米管网络。
23.权利要求21的预共混物组合物,其中该预共混物包括用纳米管涂覆的炭黑材料。
24.权利要求21的预共混物组合物,其中该预共混物包括用碳纳米结构涂覆的石墨碳材料。
25.权利要求21的预共混物组合物,其中该预共混物包括用碳纳米结构的壳涂覆的固体芯材料,从而形成芯-壳材料。
26.权利要求25的预共混物组合物,其中芯材料的形状规则或不规则,且就其平均最长尺寸来说,尺寸范围为20nm至20μm。
27.权利要求25的预共混物组合物,其中芯材料是石墨,玻璃状或无定形的碳。
28.权利要求25的预共混物组合物,其中碳纳米结构由选自富勒烯,单壁碳纳米管,多壁碳纳米管,及其化学衍生物中的一种或多种组成。
29.权利要求25的预共混物组合物,其中在芯材料上的壳涂层覆盖芯材料总表面积的50-100%范围的表面积。
30.一种预共混物组合物,它包括通过在液体介质中湿式混合接着干燥该固体组合物而制备的碳纳米结构和粒子固体。
31.权利要求30的预共混物组合物,其中该预共混物包括具有在其内分散的炭黑的纳米管网络。
32.权利要求30的预共混物组合物,其中该预共混物包括用纳米管涂覆的炭黑材料。
33.权利要求30的预共混物组合物,其中该预共混物包括用碳纳米结构涂覆的石墨碳材料。
34.权利要求30的预共混物组合物,其中该预共混物包括用碳纳米结构的壳涂覆的固体芯材料,从而形成芯-壳材料。
35.权利要求34的芯-壳材料,其中芯材料的形状规则或不规则,且就其平均最长尺寸来说,尺寸范围为20nm至20μm。
36.权利要求34的组合物,其中芯材料是石墨,玻璃状或无定形的碳。
37.权利要求34的组合物,其中碳纳米结构由选自富勒烯,单壁碳纳米管,多壁碳纳米管,及其化学衍生物中的一种或多种组成。
38.权利要求34的芯壳材料,其中在芯材料上的壳涂层覆盖芯材料总表面积的50-100%范围的表面积。
39.一种方法,它包括:
在液体介质内分散碳纳米结构,形成分散体;
共混该分散体与粒子固体,形成共混物。
40.权利要求39的方法,进一步包括干燥所述共混物,形成预共混物。
41.权利要求40的方法,其中该预共混物包括芯-壳材料,所述芯-壳材料包括用所述碳纳米结构的壳涂覆的所述固体材料的芯。
42.权利要求40的方法,进一步包括在配混过程中添加该预共混物到聚合物中。
43.权利要求40的方法,进一步包括使用该预共混物作为电池电极的一部分或者作为超级电容器内电解质介质的一部分。
44.权利要求39的方法,进一步包括在电解质介质,油漆,涂层或浆液中使用该预共混物。
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CN108020572B (zh) * | 2016-10-31 | 2020-07-10 | 清华大学 | 碳纳米管的表征方法 |
JP6805863B2 (ja) * | 2017-02-13 | 2020-12-23 | 住友ゴム工業株式会社 | タイヤ用ゴム組成物及び空気入りタイヤ |
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WO2020061988A1 (en) | 2018-09-28 | 2020-04-02 | Dow Silicones Corporation | Liquid silicone rubber composition |
JPWO2020137936A1 (ja) * | 2018-12-27 | 2021-11-18 | 昭和電工株式会社 | 樹脂添加組成物及びその製造方法、樹脂組成物及びその製造方法 |
WO2020246190A1 (ja) * | 2019-06-07 | 2020-12-10 | バンドー化学株式会社 | 伝動ベルト |
KR102524378B1 (ko) * | 2019-09-27 | 2023-04-20 | 주식회사 엘지화학 | 딥 성형용 라텍스 조성물, 이의 제조방법 및 이로부터 성형된 성형품 |
CN111607296A (zh) * | 2020-06-02 | 2020-09-01 | 上海金狮化工有限公司 | 一种功能性石墨烯改性水性皮革色浆及其制备方法 |
WO2024005669A1 (ru) * | 2022-06-27 | 2024-01-04 | Общество С Ограниченной Ответственностью "Ампертекс" | Электропроводящее композитное волокно и способ его получения и применения |
JP7230269B1 (ja) | 2022-07-29 | 2023-02-28 | 大日精化工業株式会社 | カーボン材料分散液及びその使用 |
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US9550907B2 (en) | 2017-01-24 |
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KR101996071B1 (ko) | 2019-07-05 |
JP2018518541A (ja) | 2018-07-12 |
EP3262105B1 (en) | 2023-11-08 |
EP4286465A2 (en) | 2023-12-06 |
KR20170125363A (ko) | 2017-11-14 |
US20180223052A1 (en) | 2018-08-09 |
EP4286465A3 (en) | 2024-02-28 |
WO2016138024A1 (en) | 2016-09-01 |
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