CN104822762B - 添加剂组合物及包含其的组合物和制品 - Google Patents
添加剂组合物及包含其的组合物和制品 Download PDFInfo
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- CN104822762B CN104822762B CN201380062775.5A CN201380062775A CN104822762B CN 104822762 B CN104822762 B CN 104822762B CN 201380062775 A CN201380062775 A CN 201380062775A CN 104822762 B CN104822762 B CN 104822762B
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Abstract
本发明公开了一种包含含氟聚合物、增效剂和脂肪酸金属盐的添加剂组合物。
Description
背景技术
加工助剂可降低混合橡胶诸如腈基丁二烯橡胶(NBR)、天然橡胶(NR)和乙烯丙烯二烯单体(EPDM)期间所消耗的时间和能量,从而允许昂贵混合器械的最大程度使用。通常采用的加工助剂(包括石蜡、矿物油、极性表面活性剂和石油树脂)例如由于有限的相容性而充当外部或内部润滑剂。由于已知加工助剂的局限性,仍然需要新型且可用的橡胶加工助剂。
发明内容
本发明提供了一种包含含氟聚合物、增效剂和脂肪酸金属盐的添加剂组合物。
本发明还公开了包含所公开的添加剂组合物和橡胶的组合物。
本发明还公开了由所公开的组合物形成的制品。
上述发明内容并非意图描述本发明的每个所公开实施例或每种实施方式。以下描述更具体地例示了示例性实施例。在本专利申请全文的若干地方,通过实例列表提供指导,实例可用于多种组合中。在每一种情形下,列表的列表仅仅作为代表性群组,而不应被理解为排他性列表。
具体实施方式
本文中,“室温”或“RT”是指20℃至30℃或优选地20℃至25℃的温度。
当术语“包括”和其变型在说明书和权利要求书中出现时,这些术语并不具有限制性含义。“包括”、“包含”或类似术语意指涵盖但不限于,即,包括且不排除。
在本专利申请中,诸如“一个”、“一种”和“所述”之类的术语并非旨在仅指单一实体,而是包括一般类别,其具体实例可用于举例说明。术语“一个”、“一种”和“所述”可与术语“至少一个”互换使用。其后跟随列举的短语“至少一个”和“包含至少一个”是指列表中项目的任何一个以及列表中两个或更多个项目的任何组合。
如本文中所用,术语“或”通常按其通常的意义使用,包括“和/或”,除非上下文清楚地指出并非如此。术语“和/或”意指所列要素的一个或全部,或所列要素的任何两个或更多个的组合。
同样在本文中,所有的数字在本文中均假定由术语“约”修饰并优选由术语“精确地”修饰。如本文中所用,关于测得的量,术语“约”指测得的量中如进行测量并一定程度地小心的技术人员将预期的与测量的目标和所用测量设备的精度的偏差。
另外,本文中通过端点表述的数值范围包括该范围内包含的所有数值以及端值(例如,1至5包括1、1.5、2、2.75、3、3.80、4、5等)。
本发明总体上提供可用作用于橡胶的加工助剂的组合物。所公开的组合物可提供分散填料、其他添加剂或两者的优点,以及充当润滑剂以便于加工。所公开的组合物一般可包含含氟聚合物、增效剂和脂肪酸金属盐。所公开的组合物可包含一种或不只一种含氟聚合物、一种或不只一种增效剂,以及一种或不只一种脂肪酸金属盐。
所公开的组合物包含至少一种含氟聚合物。该至少一种含氟聚合物可提供润滑剂作用以降低摩擦系数并且在聚合物-金属界面处形成低表面能涂层以产生滑移并降低设备中橡胶的粘着。可用于所公开的组合物的含氟聚合物可包含弹性体含氟聚合物(即,含氟弹性体或无定形含氟聚合物)和热塑性含氟聚合物(即,半结晶含氟聚合物)。可用的含氟聚合物可包含氟化烯烃的均聚物和/或共聚物。在一些实施例中,均聚物或共聚物可具有至少1:2,在一些实施例中至少1:1的氟原子与碳原子之比;和/或至少1:1.5的氟原子与氢原子之比。或者,可用于所公开的组合物的含氟聚合物也可被描述为在室温及以上处于流体状态,即Tg值低于室温并且在室温下很少或没有表现出结晶度的含氟聚合物。
可使用的示例性均聚物是衍生自例如偏二氟乙烯和氟乙烯的那些。可使用的氟化烯烃的示例性共聚物是衍生自例如偏二氟乙烯和一种或多种另外的烯烃的那些,该一种或多种另外的烯烃可以是或可以不是氟化的(氟化烯烃的实例为六氟丙烯,并且非氟化烯烃的实例为丙烯)。
在一些实施例中,可使用的示例性含氟聚合物包括偏二氟乙烯与在每个双键碳原子上包含至少一个氟原子的至少一种末端不饱和的含氟单烯烃的共聚物,所述含氟单烯烃的每个碳原子仅被氟、氯、溴、氢或低级含氟烷基基团(例如,具有1至4个碳原子的全氟烷基)或含氟烷氧基(例如,具有1至4个碳原子的全氟烷氧基)取代。可与偏二氟乙烯一起使用的示例性具体共聚单体包括全氟丙烯、四氟乙烯、三氟氯乙烯和五氟丙烯。在一些实施例中,可使用由偏二氟乙烯、六氟丙烯、三氟氯乙烯、四氟乙烯、全氟烷基全氟乙烯醚或它们的组合所聚合的含氟聚合物。可采用的含氟弹性体的具体实例包括偏二氟乙烯与选自六氟丙烯、三氟氯乙烯、1-氢五氟丙烯和2-氢五氟丙烯的共聚单体的共聚物;偏二氟乙烯、四氟乙烯与六氟丙烯或1-或2-氢五氟丙烯的共聚物;以及四氟乙烯、丙烯和任选地偏二氟乙烯的共聚物,所有这些共聚物是本领域已知的。在一些实施例中,可使用通过使全氟丙烯与偏二氟乙烯共聚而获得的含氟聚合物。此类具体含氟聚合物在例如美国专利No.3,051,677(Rexford)和3,318,854(Honn等人)中有所描述。在一些实施例中,可使用通过使全氟丙烯、偏二氟乙烯和四氟乙烯共聚而获得的含氟聚合物。此类具体含氟聚合物在例如美国专利No.2,968,649(Pailthorp等人)中有所描述。在一些实施例中,可使用由六氟丙烯与偏二氟乙烯聚合的含氟聚合物或者六氟丙烯与偏二氟乙烯的共聚物。六氟丙烯与偏二氟乙烯的示例性共聚物可以DynamarTM FX 9613和FX 9614商购获得(可从美国明尼苏达州的3M公司(3M,Minnesota,USA)商购获得)。
可用于所公开的组合物的半结晶含氟聚合物包括但不限于聚(偏二氟乙烯)、四氟乙烯的均聚物和共聚物(诸如FEP氟碳树脂,以及四氟乙烯、丙烯和任选地偏二氟乙烯的共聚物)。多峰含氟聚合物(诸如国际专利公布WO 00/69967中所公开的那些)也可用作所公开的组合物中的含氟聚合物。如本文中所用,“多峰”意指具有离散且不同的分子量的至少两种组分的含氟聚合物。两种组分均可为无定形或半结晶的,或一种组分可为无定形的并且另一种组分为半结晶的。
所公开的组合物还包含至少一种增效剂。增效剂可充当组合物的各组分的分散剂并充当橡胶的外部润滑剂。增效剂一般为具有极性主链的低粘度聚合物或极性化合物。此类增效剂的实例包括i)硅氧烷-聚醚共聚物;ii)脂族聚酯,诸如聚(己二酸丁二醇酯)、聚(乳酸)和聚己内酯聚酯;iii)芳族聚酯,诸如邻苯二甲酸二异丁基酯;iv)聚醚多元醇,诸如聚(四亚甲基醚乙二醇);v)胺氧化物,诸如辛基二甲基氧化胺;vi)羧酸,诸如羟基-丁二酸;vii)脂肪酸酯,诸如脱水山梨糖醇单月桂酸酯和三甘油酯;以及vii)聚(氧化烯)聚合物。
在一些实施例中,增效剂可为聚(氧化烯)聚合物。示例性聚(氧化烯)聚合物可包括聚(氧化烯)多元醇及其衍生物。具体示例性聚(氧化烯)聚合物由下式I表示:
A[(OR1)xOR2]y (I)
在式I中,A可为具有多个活性氢原子(例如,2或3个)的低分子量引发剂有机化合物的无活性氢的残基,该低分子量引发剂有机化合物诸如为多羟基烷烃或聚醚多元醇,例如乙二醇、甘油、1,1,1,-三羟甲基丙烷和聚(氧丙烯)二醇。
在式I中,y可为2或3。
在式I中,(OR1)x可为具有多个氧化亚烷基基团(OR1)的聚(氧化烯)链,其中R1基可为相同或不同的,并且选自C1至C5亚烷基;并且x为氧化亚烷基单元的数量。在一些实施例中,R1基可为相同或不同的,并且选自C2和C3亚烷基。所述聚(氧化烯)链可为均聚物链,例如聚(氧乙烯)或聚(氧丙烯),或者可以为无规分布的(即异种混合物)氧化亚烷基基团的链,例如--OC2H4--和--OC3H6--单元的共聚物,或者可以为具有重复的氧化亚烷基基团的交替嵌段或主链链段的链,例如包含
和
嵌段的聚合物,其中a+b=x,为约5至约500并且在一些实施例中为约10至300。R2为H或有机基,诸如烷基、芳基或其组合如芳烷基或烷芳基,并且可包含杂原子,诸如O或N。例如,R2可为甲基、丁基、苯基、苄基和酰基基团,诸如乙酰基(CH3CO-)、苯甲酰基(C6H5CO-)和硬脂酰基(C17H35CO-)。
可用于本文中的具体聚(氧化烯)聚合物衍生物可包括例如聚(氧化烯)多元醇衍生物,其中末端羟基基团已被部分或完全转化为醚衍生物,例如甲氧基基团,或者酯衍生物,例如硬脂酸酯基团(C17H35COO-)。其他可用的聚(氧化烯)衍生物包括(例如)由二羧酸和聚(氧化烯)二醇制备的聚酯。在一些实施例中,聚(氧化烯)聚合物衍生物按重量计的主要部分是重复的氧化亚烷基基团(OR)。所述聚(氧化烯)多元醇及其衍生物在室温下可为液体或固体,并且可具有至少200的分子量,并且在一些实施例中约400至20,000的分子量或在一些实施例中甚至更高,例如200,000或更大。
可用于所公开的组合物的具体聚(氧化烯)多元醇可包括以商标CARBOWAX诸如CARBOWAXTM 3350,H(OC2H4)nOH(其中n为约76)及CARBOWAXTM 8000(美国密歇根州米德兰的陶氏化学公司(Dow Chemicals,Midland MI USA))出售的那些,以及以商标PLURONIC例如PLURONICTM F-77,H(OC2H4)d[OCH(CH3)CH2]e(OC2H4)f)H出售的那些,其中d+f为约108,并且e为约35。
在一些实施例中,聚(氧化烯)聚合物可为聚(氧乙烯)二醇,通常称为聚乙二醇(或“PEG”)。在一些实施例中,可使用分子量为约1000至20,000的PEG。
在一些实施例中,增效剂可为脂族聚酯。可用于所公开的组合物的示例性脂族聚酯可包括聚己内酯。在一些实施例中,可使用数均分子量在1000至32000范围内的聚己内酯。在一些实施例中,可使用数均分子量在2000至10000范围内的聚己内酯。在一些实施例中,可使用数均分子量在2000至4000范围内的聚己内酯。可用作所公开的组合物中的增效剂的聚己内酯的具体实例具有约4000的分子量并且可以商品名CAPA 2402(英国柴郡沃灵顿的柏斯托英国公司,邮编WA46HA(Perstorp UK Ltd,Warrington,Cheshire,WA46HA,UK))获得。
所公开的组合物还包含至少一种脂肪酸金属盐。脂肪酸金属盐可起到提供扭矩降低以及在加工机器(例如,混合器或铣床)中混合时使组合物热稳定的作用。
脂肪酸金属盐一般包括脂肪酸组分和金属阳离子组分。在一些实施例中,脂肪酸组分和金属阳离子可离子键合在一起以形成化合物,然后将其引入组合物中。
脂肪酸可一般描述为具有脂族尾部的羧酸。脂族尾部可为饱和或不饱和的。在一些实施例中,脂肪酸可具有约八(C8)至约三十(C30)的碳数。在一些实施例中,脂肪酸可具有约八(C8)至约二十六(C26)的碳数。具有八至二十六个碳数的脂肪酸的常用名称是:辛酸(C8)、癸酸(C10)、月桂酸(C12)、肉豆蔻酸(C14)、棕榈酸(C16)、硬脂酸(C18)、花生酸(C20)、山嵛酸(C22)、木蜡酸(C24)和蜡酸(C26)。脂肪酸金属盐中的脂肪酸组分一般不含羧酸的氢,并且可一般涉及从名称末尾移除…“酸”并替换为“酸盐”。例如因此,脂肪酸金属盐的示例性脂肪酸组分可包括辛酸盐、癸酸盐、月桂酸盐、肉豆蔻酸盐、棕榈酸盐、硬脂酸盐、花生酸盐、山嵛酸盐、木蜡酸盐和蜡酸盐。
脂肪酸金属盐还包含金属阳离子。金属阳离子与脂肪酸组分离子键合,从而取代羧酸的氢离子。示例性金属阳离子可包括铝(Al)、钙(Ca)、镁(Mg)和锌(Zn)。
可用于所公开的组合物的脂肪酸金属盐可涉及金属阳离子与脂肪酸的组合,例如,硬脂酸锌。例如,硬脂酸锌可以商品名FINALUX SS(印度孟买的精细有机物公司(FineOrganics,Mumbai,India))商购获得。可形成可用于所公开的组合物的脂肪酸金属盐,然后加入所公开的组合物中,或者可另选地在该组合物中形成。在其中脂肪酸金属盐在组合物中形成的实施例中,可将包含金属阳离子的第一组分和包含脂肪酸的第二组分均加入组合物中。这种实施例的实例包括将氧化锌和硬脂酸加入组合物中以形成脂肪酸金属盐硬脂酸锌。
可以各种类型的配方配制和利用所公开的组合物。第一种类型的组合物在本文中可称为添加剂组合物或三元添加剂组合物。所公开的添加剂组合物可包含至少一种含氟聚合物、至少一种增效剂和至少一种脂肪酸金属盐。例如,添加剂组合物可用作加入橡胶和/或其他组分中的添加剂以有助于加工橡胶。所公开的添加剂组合物可包含各种量的这三种组分。各种组分的量可通过组分相对于这三种组分的总重量的重量百分比来描述。在一些实施例中,添加剂组合物可包含约90重量%至10重量%:90重量%至10重量%:80重量%至5重量%的含氟聚合物:增效剂:脂肪酸金属盐的量。在一些实施例中,添加剂组合物可包含约70重量%至30重量%:45重量%至5重量%:45重量%至5重量%的含氟聚合物:增效剂:脂肪酸金属盐的量。在一些实施例中,添加剂组合物可包含约60重量%至40重量%:35重量%至15重量%:35重量%至15重量%的含氟聚合物:增效剂:脂肪酸金属盐的量。在某些示例性实施例中,所公开的添加剂组合物可包含约50重量%:25重量%:25重量%的含氟聚合物:增效剂:脂肪酸金属盐的量。在某些其他示例性实施例中,所公开的添加剂组合物可包含约25重量%:25重量%:50重量%的含氟聚合物:增效剂:脂肪酸金属盐的量。在某些其他示例性实施例中,所公开的添加剂组合物可包含约15重量%:15重量%:70重量%的含氟聚合物:增效剂:脂肪酸金属盐的量。
第二种类型的组合物可称为包含橡胶的组合物。包含橡胶的组合物可包含要在添加极少或不添加另外的组分的情况下加工成制品的最终组合物;以及母料组合物,在将母料组合物加工成制品之前要向母料组合物中加入另外的组分,包括另外的橡胶。
所公开的包含橡胶的组合物包含橡胶。可用于本文中的橡胶的示例性类型可包括例如天然橡胶、乙烯丙烯二烯单体(EPDM)橡胶、腈基丁二烯橡胶(NBR)、丁二烯/苯乙烯橡胶、丁二烯/丙烯腈橡胶、硅橡胶或它们的组合。在一些实施例中,包含橡胶的组合物可包含EPDM、NBR或天然橡胶。
当与“纯”组合物(即,基本上只包含这三种组分的组合物)相比时,母料组合物可使得利用所公开的组合物更容易。例如,可将母料组合物加入另外的橡胶中(或反之亦然,可将另外的橡胶加入母料组合物中)以形成要加工成制品的最终组合物。母料可被描述为混合物,或更具体地例如为添加剂组合物(即,含氟聚合物、增效剂和脂肪酸金属盐)与橡胶的分散体。
要用作母料组合物的包含橡胶的组合物可通过橡胶相对于按橡胶和添加剂组合物的重量计的总量的量来表征。在一些实施例中,母料组合物可包含例如至少约60重量%的橡胶。在一些实施例中,母料组合物可包含例如约60重量%至约95重量%的橡胶。母料组合物也可通过其中所含的添加剂组合物的量来描述。在一些实施例中,母料组合物可包含约30重量%或更少的添加剂组合物。在一些实施例中,母料组合物可包含约5重量%至约30重量%的添加剂组合物。
可通过将适当量的添加剂组合物和橡胶在混合器例如混合器中混合来制备母料组合物。可在高于一种或多种组分的熔点的温度下混合母料以有助于组分的混合。
要用作待加工成制品的最终组合物的包含橡胶的组合物(本文中称为“可加工组合物”)一般可包含一定量的添加剂组合物、橡胶和任选的其他成分。可包含于可加工组合物中的橡胶的具体种类与以上讨论的那些相同。应当指出的是,可通过将所需量的添加剂组合物与橡胶组合、通过将另外的橡胶与母料组合物组合,或它们的组合来形成可加工组合物。
可加工组合物可一般通过各种组分的量来表征。在一些实施例中,可加工组合物可通过其中包含的添加剂组合物相对于可加工组合物的全部重量(全部重量将包括添加剂组合物、橡胶和任何其他任选组分的重量)的量来表征。例如,在一些实施例中,可加工组合物可包含约0.1重量%至约3重量%的添加剂组合物。在一些实施例中,可加工组合物可包含约0.5重量%至约2.5重量%的添加剂组合物。在一些实施例中,可加工组合物可包含约2重量%的添加剂组合物。
可加工组合物还可包含填料。示例性填料可包括例如炭黑、二氧化硅、钙金属硅酸盐、碳酸钙、粘土和硫酸钡。本文中所公开的添加剂组合物可有助于掺入填料,即使在相对较高水平。在一些实施例中,可加工组合物可包含约30重量%至约60重量%的填料。
本文中所公开的可加工组合物可提供许多益处和/或优点。所公开的可加工组合物可得益于缩短的混合时间和因此减少的能量消耗,因为填料由于添加剂组合物的存在可更易于分散。可通过组成组合物的集料的平均尺寸来定量地监测填料分散。在一些实施例中,可加工组合物可具有小于约10微米的平均集料尺寸。可使用已知方法测量集料尺寸,该方法包括例如反射光显微镜法或SEM。
表征集料尺寸的一种示例性方法是通过使用可以商品名“disperGRADER”从美国俄亥俄州阿克伦的阿尔法科技公司(Alpha Technologies,Akron,Ohio)商购获得的反射光显微镜。该分析所得的结果可包括白色区域的表征。“白色区域”由不分散的附聚物引起。由于附聚物比聚合物基体更硬,在切下样品后它们返回到表面,从而在表面上形成隆起,这在照片上显示为白色区域。白色区域%越低,组合物就越分散并且不分散的填料%极少。该仪器还提供X和Y评级。X评级基于1-10标度的附聚物尺寸分布。如果分散较好,则附聚物尺寸将为低的并且评级将为高的。Y值取决于高于23微米的附聚物的量。如果具有较少的高于23微米的附聚物,则Y评级将较高,从而指示较好的分散。当比较使用相同类型的填料例如相同等级的炭黑制备的试样时,也可使用附聚物尺寸的平均附聚物尺寸和标准偏差。
所公开的可加工组合物也可具有更好的流动性质,从而使得加工更容易。一旦所公开的可加工组合物沉积在模具中,就可增强脱模,尤其是在具有复杂外形的模具中脱模。更好的脱模也可引起更少的模具结垢,从而减少模具清洁所需的时间和精力。更好的脱模使部件的粘着最小化并且模具清洁耗时更短。清洁时间最小化可使台板温度降低的程度最小化。如果台板温度降低,可能需要再次加热模具,从而浪费了制品模制期间的时间和能量。
使用所公开的可加工组合物制备的制品也可具有优异的性质。例如,由可加工组合物形成的制品可具有增强的机械性质,诸如拉伸强度和断裂伸长率。由可加工组合物形成的制品也可具有改善的光泽度和总体上改善的外观。
实例
以下具体的、但非限制性的实例用于示出本发明。在这些实例中,所有的量均表示为重量份,或重量份/100重量份橡胶(phr)。缩写包括克缩写为g,分钟缩写为min,小时缩写为hrs,每分钟转数缩写为rpm。
测试方法
分散测试
使用以商品名“disperGRADER”得自美国俄亥俄州阿克伦的阿尔法科技公司的商用仪器进行分散测试。该仪器是使用反射光的反射光显微镜,其被设计为测量橡胶化合物的填料分散。用剃刀刀片切下硫化橡胶样品,并且以切割面面向光圈的方式放在光圈的前方。光以30度角反射到样品上。光被反射远离表面的平滑部分,而入射到附聚物上的光被反射到相机中。ISO 11345方法B是用于限定橡胶的分散特性的测量的规范。该规范为分散测试以及限定标准测试条件给出了良好背景。“disperGRADER”基准标度基于ISO 11345方法B,该方法利用了这样的事实,弹性体和填料充分分散于其中的化合物在反射光中将显示平滑无疵质地。不适当分散的成分的存在通过呈现表面上的“隆起”的形式的不规则部分来显示,从而指示配混成分的较差分散。这些不规则部分的尺寸和频率用于判断化合物达不到最佳分散的程度。为disperGRADER中的每种不同基准标度建立一组十个图像标准。为这些基准图像中的每一个指定数值评级1-10(“X”值)。
测试结果以1-10范围内的两种数值标度表示。X值是相对于实际橡胶类型的图像基准标度的评级。这是填料分布的量度。如果分散较好,则附聚物尺寸将为低的并且评级将为高的。Y值基于引起从表面不规则部分反射的附聚物的尺寸和数量。在100x放大倍率中忽略低于23微米的尺寸。该值与大附聚物的发生率相关。如果具有较少数量的高于23微米的附聚物,则Y评级将为高的,从而指示较好的分散。
该方案提供了评价橡胶化合物中的分散的方式并且为分散程度指定数值标号。
处于100x放大倍率的“disperGRADER”测量并定量从3至57微米尺寸范围内的表面不规则部分的反射。通过较高放大倍率,增强了较高质量橡胶的分辨率,其中主要部分的附聚物处于3至57微米的范围内。被分析的区域等于1/10用30x仪器分析的区域。由于测试区域较小,如果附聚物在测试表面上的分布非常不均匀,则可增加扫描数量以实现较大测试区域。对于具有100x放大倍率的“disperGRADER”而言,当前可用的不同标度和方法使用“CB(x,y)方法”。具有非常高且均匀程度的炭黑分散的应用要求增加100x放大倍率的分辨率。CB(x,y)方法是用于所有类型的炭黑的一般方法。除了放大倍率外,该方法具有与国际标准ISO 11345方法B相同的测试规范。该方法也对大附聚物的存在进行评级。测试工序意味着对测试样品没有特殊要求。适用于流变仪测试的样品适用于“disperGRADER”。用样品切割器将一小片橡胶切片,以露出新的平坦表面。
亨特立(Hunter Lab)色度计测试
使用美国弗吉尼亚州雷斯顿的亨特立公司(Hunter Lab(Reston,VA))便携式反射色分光光度计(EZ)根据ASTM D6290来测量平坦、不透明样品的反射率。
配置软件以读取:CIE L a*b*的颜色标度、作为发光体的D65光源以及处于10度角的观察者。通过如下方式使仪器标准化:首先使用黑玻璃或光阱设定标度的最低点。确保黑玻璃与端口紧密接触,或光阱完全覆盖端口。使用经校准的白色标准完成标准化。将橡胶样品(2mm厚度的10×10cm片材)以待测量的侧面面朝上的方式放在台面顶或其他平坦表面上。将仪器端口放在样品的顶部上,确保其被待测量的区域完全覆盖并且平靠着该区域。取样品的单个颜色读数。将样品旋转90°并且对其再读取至少一次。对表示其颜色的单个颜色测量值的多个颜色读数进行平均。对各读数间旋转所得的多个读数进行平均,使得与方向性相关联的测量变化最小化。记录L、a*、b*的平均颜色值。
光泽度
使用可从美国特拉华州纽卡斯尔的检测设备公司(Testing Machines,Inc,NewCastle,DE,USA)以商品名“NOVOGLOSS LITE60°”商购获得的光泽计,根据ASTM D523进行如表4中所示的光泽度测量。指示均质性的模制部件的光泽度在三元共混物中优于任何比较例。
SEM成像
使用日本东京的日本电子株式会社(JEOL(Tokyo,JP))“JSM-6510LV”扫描电子显微镜(SEM)来表征配混的样品并且结果列于表2中。用超薄切片机将样品切成厚度为1-2mm的5mm×5mm正方形。然后将样品放入试样夹持器中,并且在“JEOL JFC-1600”自动精细离子溅射仪(auto fine coater)中在小于5托的真空下将铂溅镀在试样上持续80秒。将溅镀的样品置于SEM仪器内部的试样安装室上,并且使样品暴露于高真空和10kV的HT光束。通过扫描4次改善图像的分辨率,并且捕获反向散射电子图像,以在对对比度和亮度自动调节的情况下得到清晰的SEM图像。“JSM-6510LV”在30kV下具有3.0nm的分辨率。在5kV或10kV下以100x至900x拍摄SEM图像以查看粒度、退化黑点、附聚以及表面处的浸出或起霜。
力学测试
按照ASTM D 412-C类测量拉伸强度和断裂伸长率。
配混、混合和固化工序
使用(混合器类型WN 350E)进行所有预固化配混和混合。该型号允许使用测力计测量样品材料对旋转叶片的阻力。为每种样品材料记录随时间变化的扭矩和储存温度。在测量期间所测量的数据以表格方式数字地和/或以图表方式图形地显示在监视器上,并且可打印并保存。结果在表4中示出。
对于所有试验,混合器温度保持在135℃,使用凸轮型转子叶片“N”,旋转速度保持在50rpm并且批重固定在250克。已证实,混合器在混合开始之前达到设定温度。
将橡胶(EPDM或NBR)装入BRABENDER混合器中并温热1分钟。在1分钟内一步加入实例1至3和比较例A至Q的预共混物和添加剂。EPDM样品的预共混物为105phr炭黑1、25phrRPO、5phr ZnO和0.9phr硬脂酸。NBR样品的预共混物为5phr ZnO、1phr硬脂酸、35phr炭黑2、35phr炭黑3和7phr的邻苯二甲酸二辛酯。一旦混合器装满,就推下混合器上的启动按钮,记录随时间变化的扭矩、熔融时间、比能量和熔融温度。所有批次的混合时间设定为6分钟。6分钟结束时,转子自动停止。将橡胶化合物从混合器和转子完全清除,并且使用3M SCOTCH-BRITE擦洗垫将任何残余材料从转子和混合容器的表面移除。最后,在开始下一批次之前使混合器冷却到设定温度。
然后对于EPDM样品,将所制备的“绿色化合物”与1.8phr硫、1phr MBTS、0.8phrTMT和1phr ZNBC的固化包装在双辊开炼机中混合5-10分钟,最后辗平成3-4mm厚的片材。NBR样品的固化包装为1phr硫、1.5phr CBS、1phr TMT。然后在20-25kg/cm2和170℃的温度下将掺入的固化橡胶化合物在压塑机(商号:印度孟买的桑托什橡胶机械公司(M/SSantosh Rubber Machineries,Mumbai,India),50T压制硫化压机(50T CompressionCuring Press))中固化10-15分钟。使用振荡盘式流变仪(商号:美国德普科技公司(TechPro,USA),MDR 2000)在177℃下测试固化的片材6分钟,结果示于表3中,以及机械性质的结果示于表2中。
比较例
这些比较例使用如表1中所示的橡胶加工助剂的必需的3种成分中的0、1或2种。数据示于表2中。
实例
这些实例使用配混到橡胶(EPDM或NBR)中的橡胶加工助剂(无定形含氟聚合物FX-9614)、增效剂(PEG或PCL)和脂肪酸金属盐(硬脂酸锌)的所有三种必需成分,如表1中所示。数据示于表2中。
表1:材料
表2:用于绿色化合物制备的基于每一百份橡胶的份数(phr)计的配方
*所有比较例和实例使用105phr炭黑(FEF N550)、25phr RPO、5phr ZnO、0.9phr硬脂酸、1.8phr硫、1phr MBTS、0.8phr TMT和1phr ZNBC。
表3:分散体、色度计、SEM和机械测试结果
*SEM说明:
SP、MP、LP=小、中或大粒子
DDS=退化黑点
A=附聚
B=起霜或表面浸出
大粒子=30-40微米,中粒子=10-20微米,小粒子=1-5微米
表4:固化流变性
ML:以dNm为单位的最小扭矩水平
MH:以dNm为单位的最大扭矩水平
Δ扭矩:最大扭矩(MH)与最小扭矩(ML)之间的差值
ts2:达到2dNm升高的分钟数
t’50:达到50%的Δ扭矩的分钟数(50%固化时间)
t’90:达到90%的Δ扭矩的分钟数(90%固化时间)
示例性实施例包括如下:
实施例1.一种添加剂组合物,其包含:
含氟聚合物;
增效剂;和
脂肪酸金属盐。
实施例2.根据实施例1所述的添加剂组合物,其中所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量%计的量可在90-10%:90-10%:80-5%的范围内。
实施例3.根据实施例1所述的添加剂组合物,其中所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量可在60-40%:35-15%:35-15%的范围内。
实施例4.根据实施例1所述的添加剂组合物,其中所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量为约50%:25%:25%。
实施例5.根据实施例1所述的添加剂组合物,其中所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量为约25%:25%:50%。
实施例6.根据实施例1所述的添加剂组合物,其中所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量为约15%:15%:70%。
实施例7.根据实施例1至6中任一项所述的添加剂组合物,其中所述含氟聚合物由偏二氟乙烯、六氟丙烯、三氟氯乙烯、四氟乙烯、全氟烷基全氟乙烯醚或它们的组合聚合而成。
实施例8.根据实施例1至6中任一项所述的添加剂组合物,其中所述含氟聚合物为六氟丙烯与偏二氟乙烯的共聚物。
实施例9.根据实施例1至8中任一项所述的添加剂组合物,其中所述增效剂包括聚(氧化烯)聚合物、聚己内酯或它们的组合。
实施例10.根据实施例1至9中任一项所述的添加剂组合物,其中所述脂肪酸金属盐包含锌(Zn)、钙(Ca)、镁(Mg)、铝(Al)或它们的组合。
实施例11.根据实施例1至10中任一项所述的添加剂组合物,其中所述脂肪酸金属盐包含C8至C26脂肪酸的混合物。
实施例12.一种组合物,包含:
根据实施例1-11中任一项所述的添加剂组合物;和
橡胶。
实施例13.根据实施例12中任一项所述的组合物,其中所述橡胶包括天然橡胶、乙烯丙烯二烯单体(EPDM)橡胶、腈基丁二烯橡胶(NBR)、丁二烯/苯乙烯橡胶、丁二烯/丙烯腈橡胶、硅橡胶或它们的组合。
实施例14.根据实施例12或13所述的组合物,其中所述橡胶包括EPDM、NBR或天然橡胶。
实施例15.根据实施例12至14中任一项所述的组合物,其包含至少约70重量%的橡胶。
实施例16.根据实施例12至14中任一项所述的组合物,其包含约60重量%至约95重量%的橡胶。
实施例17.根据实施例12至14中任一项所述的组合物,其中所述组合物包含约0.1至约3重量%的添加剂组合物。
实施例18.根据实施例12至14中任一项所述的组合物,其中所述组合物包含约0.5重量%至约2.5重量%的添加剂组合物。
实施例19.根据实施例12至14中任一项所述的组合物,其中所述组合物包含约2重量%的添加剂组合物。
实施例20.根据实施例17至19中任一项所述的组合物,其中所述组合物还包含约30重量%至约60重量%的填料。
实施例21.一种由根据实施例17至20中任一项所述的组合物形成的制品。
实施例22.根据实施例21所述的制品,其中所述制品具有改善的光泽度。
Claims (18)
1.一种组合物,该组合物包含:
橡胶,其中所述橡胶包括天然橡胶、腈基丁二烯橡胶(NBR)、丁二烯/苯乙烯橡胶、硅橡胶或它们的组合,
30重量%至60重量%的填料,和
添加剂组合物,该添加剂组合物包含:
含氟聚合物;
增效剂,其中所述增效剂包括聚(氧化烯)聚合物、聚己内酯或它们的组合;和
脂肪酸金属盐。
2.根据权利要求1所述的组合物,其中基于所述添加剂组合物的总重量,所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量在90-10%:90-10%:80-5%的范围内,其中各组分的百分比之和为100%。
3.根据权利要求1所述的组合物,其中基于所述添加剂组合物的总重量,所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量在60-40%:35-15%:35-15%的范围内。
4.根据权利要求1所述的组合物,其中基于所述添加剂组合物的总重量,所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量为50%:25%:25%。
5.根据权利要求1所述的组合物,其中基于所述添加剂组合物的总重量,所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量为25%:25%:50%。
6.根据权利要求1所述的组合物,其中基于所述添加剂组合物的总重量,所述含氟聚合物、所述增效剂和所述脂肪酸金属盐的按重量计的量为15%:15%:70%。
7.根据权利要求1至6中任一项所述的组合物,其中所述含氟聚合物由偏二氟乙烯、六氟丙烯、三氟氯乙烯、四氟乙烯、全氟烷基全氟乙烯醚或它们的组合聚合而成。
8.根据权利要求1至6中任一项所述的组合物,其中所述含氟聚合物为六氟丙烯与偏二氟乙烯的共聚物。
9.根据权利要求1至6中任一项所述的组合物,其中所述脂肪酸金属盐的金属阳离子包含锌(Zn)、钙(Ca)、镁(Mg)、铝(Al)或它们的组合。
10.根据权利要求1至6中任一项所述的组合物,其中所述脂肪酸金属盐包含C8至C26脂肪酸盐的混合物。
11.根据权利要求1至6中任一项所述的组合物,其中所述橡胶包括NBR或天然橡胶。
12.根据权利要求1至6中任一项所述的组合物,其包含60重量%至95重量%的橡胶,其中各组分的百分比之和为100%。
13.根据权利要求1至6中任一项所述的组合物,其中所述组合物包含0.1至3重量%的所述添加剂组合物。
14.根据权利要求1至6中任一项所述的组合物,其中所述组合物包含0.5重量%至2.5重量%的所述添加剂组合物。
15.根据权利要求1至6中任一项所述的组合物,其中所述组合物包含2重量%的所述添加剂组合物。
16.根据权利要求1至6中任一项所述的组合物,其中所述填料包括炭黑。
17.一种由根据权利要求1所述的组合物形成的制品。
18.一种由根据权利要求13所述的组合物形成的制品。
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- 2013-11-18 WO PCT/US2013/070570 patent/WO2014085126A1/en active Application Filing
- 2013-11-18 CN CN201380062775.5A patent/CN104822762B/zh not_active Expired - Fee Related
- 2013-11-18 US US14/648,199 patent/US9938402B2/en active Active
- 2013-11-18 EP EP13858823.1A patent/EP2925815B1/en active Active
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Also Published As
Publication number | Publication date |
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EP2925815A1 (en) | 2015-10-07 |
US20150299444A1 (en) | 2015-10-22 |
EP2925815A4 (en) | 2016-06-29 |
EP2925815B1 (en) | 2020-08-05 |
CN104822762A (zh) | 2015-08-05 |
WO2014085126A1 (en) | 2014-06-05 |
US9938402B2 (en) | 2018-04-10 |
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