CN109310179A - 鞋底、组合物及其制造方法 - Google Patents
鞋底、组合物及其制造方法 Download PDFInfo
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- CN109310179A CN109310179A CN201780027430.4A CN201780027430A CN109310179A CN 109310179 A CN109310179 A CN 109310179A CN 201780027430 A CN201780027430 A CN 201780027430A CN 109310179 A CN109310179 A CN 109310179A
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- polyolefin
- sole
- weight
- silane
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- BWSZXUOMATYHHI-UHFFFAOYSA-N tert-butyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(C)(C)C BWSZXUOMATYHHI-UHFFFAOYSA-N 0.000 description 1
- CFWAESPQSRZDQT-UHFFFAOYSA-N tert-butyl-dimethoxy-propylsilane Chemical compound CCC[Si](OC)(OC)C(C)(C)C CFWAESPQSRZDQT-UHFFFAOYSA-N 0.000 description 1
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
提供了鞋底组合物和制造鞋底的方法。所述鞋底包括一种组合物,该组合物包含密度小于0.50g/cm3的发泡的硅烷交联的聚烯烃弹性体。所述鞋底具有约5.0%至约20.0%的压缩变定,根据ASTM D 395测量(6小时,50℃)。所述发泡的硅烷交联的聚烯烃弹性体可以由包括密度小于0.86g/cm3的第一聚烯烃、结晶度小于40%的第二聚烯烃、硅烷交联剂、接枝引发剂、缩合催化剂和发泡剂的共混物制备。
Description
发明领域
本发明总体上涉及可用于形成鞋底的聚合物组合物,更具体地说,涉及用于形成中底和/或大底的发泡的硅烷交联的聚烯烃弹性体组合物以及用于制造这些鞋底和组合物的方法。
背景技术
鞋底传统上由天然和合成橡胶制成。海绵鞋底的使用一直在增加,以跟上对轻质和功能性运动鞋和正装鞋的日益增长的需求。用于海绵鞋底的许多不同的合成材料是已知的,包括乙烯醋酸乙烯酯(EVA)、聚氨酯(PU)和丁腈橡胶。如今,EVA海绵占据了海绵鞋底材料的最大市场份额,所述海绵鞋底材料被用于使用包括压制发泡和注射发泡方法在内的技术形成中底、大底和售后市场鞋垫。
对于成功地用在鞋底中的材料来说,基于其最终用途鞋应用,该材料需要满足的各种材料性能要求,例如密度、回弹、在各种类型表面上的抓持力、耐磨性、可加工性和/或冲击吸收性。从运动鞋到老年鞋,鞋底必须提供优异的舒适性、牵引力和耐久性。
考虑到对鞋底的材料性能要求,制造商需要开发新的聚合物组合物和制造鞋底的方法,所述鞋底是多功能的,更易于生产的,重量更轻的,并且在更长的时间段内具有优异的耐久性。
发明概述
根据本公开的一个方面,公开了具有一种组合物的鞋底,该组合物包含密度小于0.50g/cm3的发泡的硅烷交联的聚烯烃弹性体。所述鞋底具有约5.0%至约35.0%的压缩变定,根据ASTM D 395测量(6小时,50℃)。
根据本公开的另一方面,提供了制造鞋底的方法。该方法包括:将密度小于0.86g/cm3的第一聚烯烃、第二聚烯烃、硅烷交联剂和自由基引发剂一起挤出,以形成硅烷接枝的聚烯烃共混物;将所述硅烷接枝的聚烯烃共混物、发泡剂和缩合催化剂一起挤出,以形成可交联的聚烯烃共混物;将所述可交联的聚烯烃共混物注射成型成鞋底部件;和在大于150℃的温度和环境湿度下交联所述可交联的聚烯烃共混物,以形成密度小于0.50g/cm3的鞋底。
根据本公开的另一方面,提供了制造鞋底的方法。该方法包括:将密度小于0.86g/cm3的第一聚烯烃、第二聚烯烃、硅烷交联剂和自由基引发剂一起挤出,以形成硅烷接枝的聚烯烃共混物;将所述硅烷接枝的聚烯烃共混物、发泡剂和缩合催化剂一起挤出,以形成可交联的聚烯烃共混物;将所述可交联的聚烯烃共混物模压成型成鞋底部件;和在大于150℃的温度和环境湿度下交联所述可交联的聚烯烃共混物,以形成密度小于0.50g/cm3的鞋底。
在研究以下说明书、权利要求书和附图后,本领域技术人员将理解和领会本发明的这些和其它方面、目的和特征。
附图的简要说明
在附图中:
图1是根据本公开的一些方面的鞋的透视图;
图2是根据本公开的一些方面的、图1中描绘的鞋的横截面透视图;
图3是用于按照本发明一些方面生产硅烷交联的聚烯烃弹性体的示意性反应途径;
图4是按照本发明的一些方面使用两步Sioplas方法用所形成的硅烷交联的聚烯烃弹性体制造中底的方法的流程图;
图5A是按照本发明的一些方面的反应性双螺杆挤出机的示意性剖视图;
图5B是按照本发明的一些方面的单螺杆挤出机的示意性剖视图;
图6是按照本发明的一些方面使用一步Monosil工艺用所形成的硅烷交联的聚烯烃弹性体制造中底的方法的流程图;
图7是按照本发明一些方面的反应性单螺杆挤出机的示意性剖视图;
图8是根据本公开的一些方面的压缩模具的示意性剖视图;
图9是根据本公开的一些方面的注射模具的示意性剖视图;
图10是根据本公开的一些方面的注射压缩模具的示意性剖视图;
图11是根据本公开的一些方面的、配备有超临界流体注射器的挤出机的示意性横截面图;
图12是根据本公开的一些方面使用超临界流体方法形成的横截中底的显微照片;
图13是根据本公开的一些方面使用化学发泡剂形成的横截中底的显微照片;和
图14是根据本公开的一些方面使用化学发泡剂形成的横截中底的显微照片。
优选实施方案的详细描述
就这里的描述而言,术语“上”、“下”、“右”、“左”、“后”、“前”、“垂直”、“水平”及它们的派生词应涉及图1中所示的鞋中取向的本发明的鞋底。然而,应该理解所述鞋底、组合物和方法可以采用各种替代的取向和步骤顺序,除非明确地相反指出。还应理解,附图中图解说明和在以下说明书中描述的具体装置和方法仅是所附权利要求书中限定的发明构思的示例性实施方案。因此,与本文中公开的实施方案相关的具体尺寸和其它物理特性不应被视为限制,除非权利要求书明确地另外说明。
本文中公开的所有范围包括所述及的端点并且是可独立地组合的(例如,“从2到10”的范围包括端点2和10以及所有中间值)。本文中公开的范围的端点和任何值不限于所述精确的范围或值;它们充分不精确以包括靠近这些范围和/或值的值。
由一个或多个术语如“约”和“基本上”修饰的值可以不限于所指定的精确值。所述近似语言可以相应于用于测量所述值的仪器的精度。修饰语“约”也应被视为公开了由两个端点的绝对值定义的范围。例如,表述“约2至约4”也公开了“2至4”的范围。
当用在两个或更多个项目的列表中时,本文中使用的术语“和/或”意味着所列出的项目中的任何一个可以被单独使用,或者所列出的项目中的两个或更多个的任何组合可以被采用。例如,如果组合物被描述为含有组分A、B和/或C,则该组合物可以仅含有A;仅含有B;仅含有C;含有A和B的组合;含有A和C的组合;含有B和C的组合;或含有A、B和C的组合。
参考图1-2,公开了一种鞋底。本公开的鞋底通常包括一种组合物,该组合物具有密度小于0.50g/cm3的发泡的硅烷交联的聚烯烃弹性体。按照ASTM D 395测量(6小时,50℃),所述鞋底具有约5.0%至约35.0%的压缩变定。所述发泡的硅烷交联的聚烯烃弹性体可以由一种共混物制备,该共混物包括密度小于0.86g/cm3的第一聚烯烃、结晶度小于40%的第二聚烯烃、硅烷交联剂、接枝引发剂、缩合催化剂和发泡剂。
现在参考图1,提供了鞋10的透视图。鞋10包括连接到中底18的大底14,其中中底18直接位于大底14上方。脚趾盒22与鞋头26组合构成鞋10的前部。脚趾盒22和鞋头26被定位以支撑并包围脚的脚趾。鞋舌30与鞋帮34组合工作以支撑脚的顶部。鞋口38和鞋跟支撑架42定位在鞋10的后部并且一起工作以舒适地定位和保持鞋10中的鞋跟。尽管图1中描绘的鞋是跑鞋,所述鞋10不意味着是限制性的,并且鞋10可以另外包括例如其它运动鞋、凉鞋、登山鞋、冬靴、正装鞋和医用矫形鞋。
现在参考图2,提供了图1中所描绘的鞋10的剖视图。该剖视图提供了与中底18相比的大底14的相应厚度。中底18是鞋10的一部分,其被夹在大底14和内衬46之间,内衬46提供缓冲和回弹,同时帮助保护脚以免感受到硬物或尖锐物体。足部与帮里50接触,帮里50定位在内衬46上作为顶层,同时在鞋10内部的脚的位置由脚趾盒22、鞋舌30和鞋帮34保持。
中底18为脚提供稳定性,使得用于制造中底18的材料被设计成能够容忍鞋通常所遇到的所有类型的挑战-即地形、使用者的体重和在行走或跑步期间产生的压力源等成为必要。用于制造中底的最常见材料是乙烯醋酸乙烯酯(EVA)的膨胀泡沫橡胶形式。与大多数橡胶一样,EVA是柔软的,但由于其热塑性性能,它在各种各样制品(包括中底)的制造中还是易于加工和操作的。虽然因为它的“低温”韧性、抗应力开裂性、防水性和抗紫外线辐射性使得EVA通常被选择作为生产中底的理想的材料,但对EVA的最大批评是其短的寿命。随着时间的推移,EVA往往压缩,并且使用者(特别是跑步者)说他们觉得他们的鞋在一段时间后变平。目前,避免EVA中底的这种变平的唯一方法是每3到6个月更换一次鞋子。
作为EVA的替代物,本文中公开的是一族发泡的硅烷交联的聚烯烃弹性体。本公开的弹性体提供了许多与EVA相同的优点,但它们还提供许多改进的材料性能,包括例如密度、回弹、压缩变定和耐久性。所述发泡的硅烷交联的聚烯烃弹性体以及用于模塑本文中公开的中底18的各种技术产生含有很多微小气泡的轻质材料,这些气泡为使用者提供了缓冲和减震。使所公开的发泡的硅烷交联的聚烯烃弹性体比EVA和其它常规鞋底材料好的性能之一是这些弹性体的相对轻盈性。所述发泡的硅烷交联的聚烯烃弹性体具有低的密度,使它们成为用于重量是问题的鞋类的理想材料。
本文中的公开内容集中于所述组合物、制备所述组合物的方法和用于制备中底18的所述发泡的硅烷交联的聚烯烃弹性体的相应材料性能。所述中底18由硅烷接枝的聚烯烃形成,其中可以向所述硅烷接枝的聚烯烃中加入催化剂以形成可硅烷交联的聚烯烃弹性体。该可硅烷交联的聚烯烃然后可以在暴露于湿气和/或热后被交联以形成最终的发泡的硅烷交联的聚烯烃弹性体或共混物。在一些方面,所述发泡的硅烷交联的聚烯烃弹性体或共混物包括密度小于0.90g/cm3的第一聚烯烃、结晶度小于40%的第二聚烯烃、硅烷交联剂、接枝引发剂、缩合催化剂和发泡剂。
第一聚烯烃
第一聚烯烃可以是聚烯烃弹性体,包括烯烃嵌段共聚物,乙烯/α-烯烃共聚物,丙烯/α-烯烃共聚物,EPDM,EPM,或这些材料中任何两种或更多种的混合物。示例性的嵌段共聚物包括以商品名INFUSETM(烯烃嵌段共聚物,the Dow Chemical Company)和SEPTONTMV-SERIES(苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物,Kuraray Co.,LTD.)销售的那些。示例性的乙烯/α-烯烃共聚物包括以商品名TAFMERTM(例如TAFMER DF710)(Mitsui Chemicals,Inc.)和ENGAGETM(例如ENGAGE 8150)(the Dow Chemical Company)销售的那些。示例性的丙烯/α-烯烃共聚物包括以商品名VISTAMAXXTM6102牌号(Exxon Mobil Chemical Company)、TAFMERTMXM(Mitsui Chemical Company)和VERSIFYTM(Dow Chemical Company)销售的那些。EPDM可以具有约0.5至约10重量%的二烯含量。EPM可以具有45重量%至75重量%的乙烯含量。
术语“共聚单体”是指适合与烯烃单体如乙烯或丙烯单体聚合的烯烃共聚单体。共聚单体可以包括但不限于脂肪族C2-C20α-烯烃。合适的脂肪族C2-C20α-烯烃的实例包括乙烯,丙烯,1-丁烯,4-甲基-1-戊烯,1-己烯,1-辛烯,1-癸烯,1-十二碳烯,1-十四碳烯,1-十六碳烯,1-十八碳烯和1-二十碳烯。在一个实施方案中,共聚单体是乙酸乙烯酯。术语“共聚物”是指通过在同一聚合物链中连接超过一种类型的单体制备的聚合物。术语“均聚物”是指通过在不存在共聚单体的情况下连接烯烃单体制备的聚合物。在一些实施方案中,基于聚烯烃的重量计,共聚单体的量可以为从大于0重量%至约12重量%,包括从大于0重量%至约9重量%和从大于0重量%至约7重量%。在一些实施方案中,共聚单体含量大于最终聚合物的约2mol%,包括大于约3mol%和大于约6mol%。共聚单体含量可以小于或等于约30mol%。共聚物可以是无规或嵌段(多相)共聚物。在一些实施方案中,所述聚烯烃是丙烯和乙烯的无规共聚物。
在一些方面,第一聚烯烃选自以下物质组成的组:烯烃均聚物,均聚物的共混物,使用两种或更多种烯烃制备的共聚物,各自使用两种或更多种烯烃制备的共聚物的共混物,和烯烃均聚物与使用两种或更多种烯烃制备的共聚物共混的组合。所述烯烃可以选自乙烯,丙烯,1-丁烯,1-丙烯,1-己烯,1-辛烯和其它高级1-烯烃。第一聚烯烃可以使用许多不同的方法(例如使用气相和溶液基的茂金属催化和齐格勒-纳塔催化)和任选地使用适合于聚合乙烯和/或α-烯烃的催化剂合成。在一些方面,茂金属催化剂可用于生产低密度乙烯/α-烯烃聚合物。
在一些方面,用于第一聚烯烃的聚乙烯可以被分类成几种类型,包括但不限于LDPE(低密度聚乙烯)、LLDPE(线性低密度聚乙烯)和HDPE(高密度聚乙烯)。在其它方面,所述聚乙烯可以被分类成超高分子量(UHMW)、高分子量(HMW)、中分子量(MMW)和低分子量(LMW)。在其它方面,所述聚乙烯可以是超低密度乙烯弹性体。
在一些方面,第一聚烯烃可以包括LDPE/硅烷共聚物或共混物。在其它方面,第一聚烯烃可以是聚乙烯,其可以使用任何本领域已知的催化剂制备,所述催化剂包括但不限于铬催化剂、齐格勒-纳塔催化剂、茂金属催化剂或后茂金属催化剂。
在一些方面,第一聚烯烃可以具有小于或等于约5,小于或等于约4,约1至约3.5,或约1至约3的分子量分布Mw/Mn。
第一聚烯烃可以以基于组合物计大于0重量%至约100重量%的量存在。在一些实施方案中,聚烯烃弹性体的量为约30重量%至约70重量%。在一些方面,进料至挤出机的第一聚烯烃可以包括约50重量%至约80重量%的乙烯/α-烯烃共聚物,包括约60重量%至约75重量%和约62重量%至约72重量%。
第一聚烯烃可以具有约2,000cP至约50,000cP范围内的熔体粘度,使用Brookfield粘度计在约177℃的温度下测量。在一些实施方案中,熔体粘度为约4,000cP至约40,000cP,包括约5,000cP至约30,000cP和约6,000cP至约18,000cP。
第一聚烯烃可以具有约20.0g/10min至约3,500g/10min(包括约250g/10min至约1,900g/10min和约300g/10min至约1,500g/10min)的熔体指数(T2),在190℃和2.16kg载荷下测量。在一些方面,第一聚烯烃具有0.5g/10min至约3,500g/10min的分数熔体指数。
在一些方面,第一聚烯烃的密度小于0.90g/cm3,小于约0.89g/cm3,小于约0.88g/cm3,小于约0.87g/cm3,小于约0.86g/cm3,小于约0.85g/cm3,小于约0.84g/cm3,小于约0.83g/cm3,小于约0.82g/cm3,小于约0.81g/cm3,或小于约0.80g/cm3。在其它方面,第一聚烯烃的密度可以为约0.85g/cm3至约0.89g/cm3,约0.85g/cm3至约0.88g/cm3,约0.84g/cm3至约0.88g/cm3,或约0.83g/cm3至约0.87g/cm3。在其它方面,所述密度为约0.84g/cm3,约0.85g/cm3,约0.86g/cm3,约0.87g/cm3,约0.88g/cm3,或约0.89g/cm3。
第一聚烯烃的百分结晶度可以小于约60%,小于约50%,小于约40%,小于约35%,小于约30%,小于约25%,或小于约20%。所述百分结晶度可以为至少约10%。在一些方面,结晶度在约2%至约60%的范围内。
第二聚烯烃
第二聚烯烃可以是聚烯烃弹性体,包括烯烃嵌段共聚物,乙烯/α-烯烃共聚物,丙烯/α-烯烃共聚物,EPDM,EPM,或这些材料中任何两种或更多种的混合物。示例性的嵌段共聚物包括以商品名INFUSETM(the Dow Chemical Company)和SEPTONTMV-SERIES(KurarayCo.,LTD.)销售的那些。示例性的乙烯/α-烯烃共聚物包括以商品名TAFMERTM(例如TAFMERDF710)(Mitsui Chemicals,Inc.)和ENGAGETM(例如ENGAGE 8150)(the Dow ChemicalCompany)销售的那些。示例性的丙烯/α-烯烃共聚物包括以商品名TAFMERTMXM牌号(MitsuiChemical Company)和VISTAMAXXTM(例如VISTAMAXX 6102)(Exxon Mobil ChemicalCompany)销售的那些。所述EPDM可以具有约0.5至约10重量%的二烯含量。所述EPM可以具有45重量%至75重量%的乙烯含量。
在一些方面,第二聚烯烃选自由以下物质组成的组:烯烃均聚物,均聚物的共混物,使用两种或更多种烯烃制备的共聚物,各自使用两种或更多种烯烃制备的共聚物的共混物,和烯烃均聚物与使用两种或更多种烯烃制备的共聚物的共混物。所述烯烃可以选自乙烯,丙烯,1-丁烯,1-丙烯,1-己烯,1-辛烯和其它高级1-烯烃。第一聚烯烃可以使用许多不同的方法(例如使用气相和溶液基的茂金属催化和齐格勒-纳塔催化)和任选地使用适合于聚合乙烯和/或α-烯烃的催化剂合成。在一些方面,茂金属催化剂可用于生产低密度乙烯/α-烯烃聚合物。
在一些方面,第二聚烯烃可以包括聚丙烯均聚物,聚丙烯共聚物,乙烯-丙烯共聚物,或它们的混合物。合适的聚丙烯包括但不限于通过丙烯的均聚或丙烯与α-烯烃共聚单体的共聚获得的聚丙烯。在一些方面,第二聚烯烃可以具有比第一聚烯烃高的分子量和/或高的密度。
在一些实施方案中,第二聚烯烃可以具有小于或等于约5,小于或等于约4,约1至约3.5,或约1至约3的分子量分布Mw/Mn。
第二聚烯烃可以以基于组合物计从大于0重量%至约100重量%的量存在。在一些实施方案中,聚烯烃弹性体的量为约30重量%至约70重量%。在一些实施方案中,进料至挤出机的第二聚烯烃可以包括约10重量%至约50重量%的聚丙烯,约20重量%至约40重量%的聚丙烯,或约25重量%至约35重量%的聚丙烯。所述聚丙烯可以是均聚物或共聚物。
第二聚烯烃可以具有约2,000cP至约50,000cP范围内的熔体粘度,使用Brookfield粘度计在约177℃的温度下测量。在一些实施方案中,所述熔体粘度为约4,000cP至约40,000cP,包括约5,000cP至约30,000cP和约6,000cP至约18,000cP。
第二聚烯烃可以具有约20.0g/10min至约3,500g/10min(包括约250g/10min至约1,900g/10min和约300g/10min至约1,500g/10min)的熔体指数(T2),在190℃和2.16kg载荷下测量。在一些实施方案中,聚烯烃具有0.5g/10min至约3,500g/10min的分数熔体指数。
在一些方面,第二聚烯烃的密度小于约0.90g/cm3,小于约0.89g/cm3,小于约0.88g/cm3,小于约0.87g/cm3,小于约0.86g/cm3,小于约0.85g/cm3,小于约0.84g/cm3,小于约0.83g/cm3,小于约0.82g/cm3,小于约0.81g/cm3,或小于约0.80g/cm3。在其它方面,第一聚烯烃的密度可以为约0.85g/cm3至约0.89g/cm3,约0.85g/cm3至约0.88g/cm3,约0.84g/cm3至约0.88g/cm3,或约0.83g/cm3至约0.87g/cm3。在其它方面,所述密度为约0.84g/cm3,约0.85g/cm3,约0.86g/cm3,约0.87g/cm3,约0.88g/cm3,或约0.89g/cm3。
第二聚烯烃的百分结晶度可以小于约60%,小于约50%,小于约40%,小于约35%,小于约30%,小于约25%,或小于约20%。所述百分结晶度可以为至少约10%。在一些方面,所述第二聚烯烃的结晶度在约2%至约60%的范围内。
如上所述,所述发泡的硅烷交联的聚烯烃弹性体或共混物,例如在中底18(参见图1-2)中使用的那些,包括所述第一聚烯烃和所述第二聚烯烃。所述第二聚烯烃通常被用于改变所述密度小于0.90g/cm3的第一聚烯烃的硬度和/或可加工性。在一些方面,不仅仅所述第一和第二聚烯烃可用于形成所述发泡的硅烷交联的聚烯烃弹性体或共混物。例如,在一些方面,一种、两种、三种、四种或更多种密度小于0.90g/cm3、小于0.89g/cm3、小于0.88g/cm3、小于0.87g/cm3、小于0.86g/cm3或小于0.85g/cm3的不同的聚烯烃可以代替和/或用于第一聚烯烃。在一些方面,一种、两种、三种、四种或更多种不同的聚烯烃、乙烯-丙烯共聚物可以代替和/或用于第二聚烯烃。
在一些方面,第一和第二聚烯烃可以进一步包括一种或多种具有或不具有硅烷接枝结构部分的TPV和/或EPDM,其中所述TPV和/或EPDM聚合物以所述硅烷交联的聚烯烃弹性体/共混物的至多20重量%的量存在。
接枝引发剂
接枝引发剂(在本公开中也称为“自由基引发剂”)可以被用在至少第一和第二聚烯烃的接枝过程中,所述接枝引发剂与各聚烯烃反应以形成能够与硅烷交联剂分子反应和/或偶联的反应性物种。接枝引发剂可以包括卤素分子,偶氮化合物(例如偶氮二异丁基),过羧酸,过氧化酯,过氧缩酮和过氧化物(例如烷基过氧化氢、二烷基过氧化物和二酰基过氧化物)。在一些实施方案中,接枝引发剂是选自下组的有机过氧化物:过氧化二叔丁基,叔丁基枯基过氧化物,过氧化二枯基,2,5-二甲基-2,5-二(叔丁基过氧)己炔-3,1,3-双(叔丁基过氧异丙基)苯,4,4-双(叔丁基过氧)戊酸正丁酯,过氧化苯甲酰,过氧苯甲酸叔丁酯,叔丁基过氧异丙基碳酸酯和过苯甲酸叔丁酯,以及双(2-甲基苯甲酰基)过氧化物,双(4-甲基苯甲酰基)过氧化物,过辛酸叔丁酯,氢过氧化枯烯,过氧化甲乙酮,月桂基过氧化物,过乙酸叔丁酯,过氧化二叔戊基,过氧苯甲酸叔戊酯,1,1-双(叔丁基过氧)-3,3,5-三甲基环己烷,α,α’-双(叔丁基过氧)-1,3-二异丙基苯,α,α’-双(叔丁基过氧)-1,4-二异丙基苯,2,5-双(叔丁基过氧)-2,5-二甲基己烷,2,5-双(叔丁基过氧)-2,5-二甲基-3-己炔和2,4-二氯苯甲酰过氧化物。示例性的过氧化物包括以商品名LUPEROXTM销售的那些(可从Arkema,Inc.获得)。
在一些方面,接枝引发剂以从大于0重量%至约2重量%(包括从约0.15重量%至约1.2重量%)的量存在,基于组合物计。引发剂和硅烷的用量可以影响硅烷接枝聚合物的最终结构(例如接枝聚合物中的接枝度和硫化聚合物中的交联度)。在一些方面,反应性组合物含有至少100ppm的引发剂,或至少300ppm的引发剂。引发剂可以以300ppm至1500ppm或300ppm至2000ppm的量存在。硅烷:引发剂重量比可以为约20:1至约400:1,包括约30:1至约400:1,约48:1至约350:1,和约55:1至约333:1。
接枝反应可以在优化在共聚体主链上的接枝并同时使副反应(例如接枝剂的均聚)最小化的条件下进行。接枝反应可以在熔体中、在溶液中、在固态和/或在溶胀态进行。硅烷化可以在各种各样的设备(例如双螺杆挤出机、单螺杆挤出机、Brabenders、密闭式混合机如班伯里密炼机和间歇式反应器)中进行。在一些实施方案中,所述聚烯烃、硅烷和引发剂被在挤出机的第一段中混合。熔融温度(即聚合物开始熔化和开始流动的温度)可以为约120℃至约260℃,包括约130℃至约250℃。
硅烷交联剂
硅烷交联剂可以被用于将硅烷结构部分共价接枝到所述第一和第二聚烯烃上,并且所述硅烷交联剂可以包括烷氧基硅烷,硅氮烷,硅氧烷或它们的组合。各种潜在的硅烷交联剂或硅烷交联剂分子的接枝和/或偶联由与相应硅烷交联剂反应的接枝引发剂形成的反应性物种促进。
在一些方面,所述硅烷交联剂是硅氮烷,其中所述硅氮烷可以包括例如六甲基二硅氮烷(HMDS)或双(三甲基甲硅烷基)胺。在一些方面,所述硅烷交联剂是硅氧烷,其中所述硅氧烷可以包括例如聚二甲基硅氧烷(PDMS)和八甲基环四硅氧烷。
在一些方面,所述硅烷交联剂是烷氧基硅烷。本文中使用的术语“烷氧基硅烷”是指包含硅原子、至少一个烷氧基和至少一个其它有机基团的化合物,其中所述硅原子通过共价键与所述有机基团键合。在一些方面,所述烷氧基硅烷选自包含以下物质的组:烷基硅烷;基于丙烯酰基的硅烷;基于乙烯基的硅烷;芳族硅烷;基于环氧基的硅烷;基于氨基的硅烷和具有-NH2、-NHCH3或-N(CH3)2的胺;基于脲的硅烷;基于巯基的硅烷;和具有羟基(即-OH)的烷氧基硅烷。基于丙烯酰基的硅烷可以选自包含以下物质的组:β-丙烯酰氧基乙基三甲氧基硅烷;β-丙烯酰氧基丙基三甲氧基硅烷;γ-丙烯酰氧基乙基三甲氧基硅烷;γ-丙烯酰氧基丙基三甲氧基硅烷;β-丙烯酰氧基乙基三乙氧基硅烷;β-丙烯酰氧基丙基三乙氧基硅烷;γ-丙烯酰氧基乙基三乙氧基硅烷;γ-丙烯酰氧基丙基三乙氧基硅烷;β-甲基丙烯酰氧基乙基三甲氧基硅烷;β-甲基丙烯酰氧基丙基三甲氧基硅烷;γ-甲基丙烯酰氧基乙基三甲氧基硅烷;γ-甲基丙烯酰氧基丙基三甲氧基硅烷;β-甲基丙烯酰氧基乙基三乙氧基硅烷;β-甲基丙烯酰氧基丙基三乙氧基硅烷;γ-甲基丙烯酰氧基乙基三乙氧基硅烷;γ-甲基丙烯酰氧基丙基三乙氧基硅烷;3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷。基于乙烯基的硅烷可以选自包含以下物质的组:乙烯基三甲氧基硅烷;乙烯基三乙氧基硅烷;对苯乙烯基三甲氧基硅烷,甲基乙烯基二甲氧基硅烷,乙烯基二甲基甲氧基硅烷,二乙烯基二甲氧基硅烷,乙烯基三(2-甲氧基乙氧基)硅烷,和乙烯基苄基亚乙基二氨基丙基三甲氧基硅烷。芳族硅烷可以选自苯基三甲氧基硅烷和苯基三乙氧基硅烷。基于环氧基的硅烷可以选自包含以下物质的组:3-环氧丙氧基丙基三甲氧基硅烷;3-环氧丙氧基丙基甲基二乙氧基硅烷;3-环氧丙氧基丙基三乙氧基硅烷;2-(3,4-环氧环己基)乙基三甲氧基硅烷和环氧丙氧基丙基甲基二甲氧基硅烷。基于氨基的硅烷可以选自包含以下物质的组:3-氨基丙基三乙氧基硅烷;3-氨基丙基三甲氧基硅烷;3-氨基丙基二甲基乙氧基硅烷;3-氨丙基甲基二乙氧基硅烷;4-氨基丁基三乙氧基硅烷;3-氨基丙基二异丙基乙氧基硅烷;1-氨基-2-(二甲基乙氧基甲硅烷基)丙烷;(氨基乙基氨基)-3-异丁基二甲基甲氧基硅烷;N-(2-氨基乙基)-3-氨基异丁基甲基二甲氧基硅烷;(氨基乙基氨基甲基)苯乙基三甲氧基硅烷;N-(2-氨基乙基)-3-氨基丙基甲基二甲氧基硅烷;N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷;N-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷;N-(6-氨基己基)氨基甲基三甲氧基硅烷;N-(6-氨基己基)氨基甲基三甲氧基硅烷;N-(6-氨基己基)氨基丙基三甲氧基硅烷;N-(2-氨基乙基)-1,1-氨基十一烷基三甲氧基硅烷;1,1-氨基十一烷基三乙氧基硅烷;3-(间氨基苯氧基)丙基三甲氧基硅烷;间氨基苯基三甲氧基硅烷;对氨基苯基三甲氧基硅烷;(3-三甲氧基甲硅烷基丙基)二亚乙基三胺;N-甲基氨基丙基甲基二甲氧基硅烷;N-甲基氨基丙基三甲氧基硅烷;二甲基氨基甲基乙氧基硅烷;(N,N-二甲基氨基丙基)三甲氧基硅烷;(N-乙酰基甘氨酰)-3-氨基丙基三甲氧基硅烷,N-苯基-3-氨基丙基三甲氧基硅烷,N-苯基-3-氨基丙基三乙氧基硅烷,苯基氨基丙基三甲氧基硅烷,氨基乙基氨基丙基三甲氧基硅烷和氨基乙基氨基丙基甲基二甲氧基硅烷。基于脲的硅烷可以是3-脲基丙基三乙氧基硅烷。基于巯基的硅烷可以选自包含以下物质的组:3-巯基丙基甲基二甲氧基硅烷,3-巯基丙基三甲氧基硅烷和3-巯基丙基三乙氧基硅烷。具有羟基的烷氧基硅烷可以选自包含以下物质的组:羟甲基三乙氧基硅烷;N-(羟乙基)-N-甲基氨基丙基三甲氧基硅烷;双(2-羟乙基)-3-氨基丙基三乙氧基硅烷;N-(3-三乙氧基甲硅烷基丙基)-4-羟基丁酰胺;1,1-(三乙氧基甲硅烷基)十一烷醇;三乙氧基甲硅烷基十一烷醇;乙醛缩乙二醇;和N-(3-乙氧基甲硅烷基丙基)葡糖酰胺。
在一些方面,所述烷基硅烷可以用以下通式表示:RnSi(OR')4-n,其中n是1、2或3;R是C1-20烷基或C2-20链烯基;和R'是C1-20烷基。术语“烷基”本身或作为另一取代基的一部分,是指具有1至20个碳原子,例如1至10个碳原子,例如1至8个碳原子,优选1至6个碳原子的、通过单碳-碳键连接的直链、支链或环状饱和烃基。当在本文中在碳原子之后使用下标时,所述下标是指所述基团可包含的碳原子的数目。因此,例如,C1-6烷基是指1-6个碳原子的烷基。烷基的实例是甲基,乙基,丙基,异丙基,丁基,异丁基,仲丁基,叔丁基,2-甲基丁基,戊基,异戊基及其异构体,己基及其异构体,庚基及其异构体,辛基及其异构体,癸基及其异构体,十二烷基及其异构体。术语“C2-20链烯基”本身或作为另一取代基的一部分,是指不饱和烃基,其可以是直链或支链的,包含一个或多个碳-碳双键,具有2至20个碳原子。C2-6链烯基的实例是乙烯基,2-丙烯基,2-丁烯基,3-丁烯基,2-戊烯基及其异构体,2-己烯基及其异构体,2,4-戊二烯基等。
在一些方面,所述烷基硅烷可以选自包含以下物质的组:甲基三甲氧基硅烷;甲基三乙氧基硅烷;乙基三甲氧基硅烷;乙基三乙氧基硅烷;丙基三甲氧基硅烷;丙基三乙氧基硅烷;己基三甲氧基硅烷;己基三乙氧基硅烷;辛基三甲氧基硅烷;辛基三乙氧基硅烷;癸基三甲氧基硅烷;癸基三乙氧基硅烷;十二烷基三甲氧基硅烷;十二烷基三乙氧基硅烷;十三烷基三甲氧基硅烷;十二烷基三乙氧基硅烷;十六烷基三甲氧基硅烷;十六烷基三乙氧基硅烷;十八烷基三甲氧基硅烷;十八烷基三乙氧基硅烷,三甲基甲氧基硅烷,甲基氢二甲氧基硅烷,二甲基二甲氧基硅烷,二异丙基二甲氧基硅烷,二异丁基二甲氧基硅烷,异丁基三甲氧基硅烷,正丁基三甲氧基硅烷,正丁基甲基二甲氧基硅烷,苯基三甲氧基硅烷,苯基三甲氧基硅烷,苯基甲基二甲氧基硅烷,三苯基甲硅烷醇,正己基三甲氧基硅烷,正辛基三甲氧基硅烷,异辛基三甲氧基硅烷,癸基三甲氧基硅烷,十六烷基三甲氧基硅烷,环己基甲基二甲氧基硅烷,环己基乙基二甲氧基硅烷,二环戊基二甲氧基硅烷,叔丁基乙基二甲氧基硅烷,叔丁基丙基二甲氧基硅烷,二环己基二甲氧基硅烷及它们的组合。
在一些方面,所述烷基硅烷化合物可以选自三乙氧基辛基硅烷,三甲氧基辛基硅烷及其组合。
可以被用作硅烷交联剂的硅烷的其它实例包括但不限于通式CH2=CR-(COO)x(CnH2n)ySiR′3的那些,其中R是氢原子或甲基;x是0或1;y是0或1;n是1至12的整数;每个R′可以是有机基团并且可以独立地选自具有1至12个碳原子的烷氧基(例如甲氧基,乙氧基,丁氧基),芳氧基(例如苯氧基),芳基烷氧基(例如苄氧基),具有1至12个碳原子的脂肪族酰氧基(例如甲酰氧基,乙酰氧基,丙酰氧基),氨基或取代的氨基(例如烷基氨基,芳基氨基),或具有1至6个碳原子的低级烷基。x和y可以都等于1。在一些方面,三个R'基团中不多于一个是烷基。在其它方面,三个R'基团中不超过两个是烷基。
可有效地接枝到和交联烯烃聚合物的、本领域已知的任何硅烷或硅烷混合物可以被用于本发明的实践中。在一些方面,硅烷交联剂可以包括但不限于包括烯键式不饱和烃基(例如乙烯基,烯丙基,异丙烯基,丁烯基,环己烯基或γ-(甲基)丙烯酰氧基烯丙基)和可水解基团(例如烃氧基,酰氧基或烃基氨基)的不饱和硅烷。可水解基团的非限制性实例包括但不限于甲氧基,乙氧基,甲酰氧基,乙酰氧基,丙酰氧基,和烷基或芳基氨基。在其它方面,硅烷交联剂是不饱和的烷氧基硅烷,其可以被接枝到聚合物上。在其它方面,另外的示例性硅烷交联剂包括乙烯基三甲氧基硅烷,乙烯基三乙氧基硅烷,甲基丙烯酸3-(三甲氧基甲硅烷基)丙基酯、γ-(甲基)丙烯酰氧基丙基三甲氧基硅烷和它们的混合物。
硅烷交联剂可以以从大于0重量%至大约10重量%(包括从大约0.5重量%至大约5重量%)范围内的量存在于所述硅烷接枝的聚烯烃弹性体中。硅烷交联剂的量可以根据烯烃聚合物的性质、硅烷本身、加工条件、接枝效率、应用和其它因素而变化。硅烷交联剂的量可以为至少2重量%,包括至少4重量%或至少5重量%,基于反应性组合物的重量计。在其它方面,硅烷交联剂的量可以为至少10重量%,基于反应性组合物的重量计。在其它方面,硅烷交联剂的含量为至少1%,基于反应性组合物的重量计。在一些实施方案中,进料至挤出机的硅烷交联剂可以包括约0.5重量%至约10重量%的硅烷单体,约1重量%至约5重量%的硅烷单体,或约2重量%至约4重量%的硅烷单体。
缩合催化剂
缩合催化剂能够促进在硅烷接枝的聚烯烃弹性体上的硅烷接枝物的水解和随后的缩合,以形成交联。在一些方面,可以通过使用电子束辐射来辅助交联。在一些方面,缩合催化剂可以包括例如有机碱、羧酸和有机金属化合物(例如有机钛酸盐和铅、钴、铁、镍、锌和锡的络合物或羧酸盐)。在其它方面,缩合催化剂可以包括脂肪酸和金属络合物化合物,例如金属羧酸盐;三乙酰丙酮铝,三乙酰丙酮铁,四乙酰丙酮锰,四乙酰丙酮镍,六乙酰丙酮铬,四乙酰丙酮钛和四乙酰丙酮钴;金属醇盐,例如乙醇铝,丙醇铝,丁醇铝,乙醇钛,丙醇钛和丁醇钛;金属盐化合物,例如乙酸钠,辛酸锡,辛酸铅,辛酸钴,辛酸锌,辛酸钙,环烷酸铅,环烷酸钴,二辛酸二丁基锡,二月桂酸二丁基锡,马来酸二丁基锡和二(2-乙基己酸)二丁基锡;酸性化合物,例如甲酸,乙酸,丙酸,对甲苯磺酸,三氯乙酸,磷酸,单烷基磷酸,二烷基磷酸,(甲基)丙烯酸对羟基乙基酯的磷酸酯,单烷基亚磷酸和二烷基亚磷酸;酸,例如对甲苯磺酸,邻苯二甲酸酐,苯甲酸,苯磺酸,十二烷基苯磺酸,甲酸,乙酸,衣康酸,草酸和马来酸,这些酸的铵盐、低级胺盐或多价金属盐;氢氧化钠;氯化锂;有机金属化合物,例如二乙基锌和四(正丁氧基)钛;和胺,例如二环己胺,三乙胺,N,N-二甲基苄胺,N,N,N',N'-四甲基-1,3-丁二胺,二乙醇胺,三乙醇胺和环己基乙胺。在其它方面,缩合催化剂可以包括二月桂酸二丁基锡,马来酸二辛基锡,二乙酸二丁基锡,二辛酸二丁基锡,乙酸亚锡,辛酸亚锡,环烷酸铅,辛酸锌和环烷酸钴。取决于所述发泡的硅烷交联的聚烯烃弹性体或共混物的所需的最终材料性质,可以使用单一缩合催化剂或缩合催化剂的混合物。缩合催化剂可以以约0.01重量%至约1.0重量%(包括约0.25重量%至约8重量%)范围内的量存在,基于所述硅烷接枝的聚烯烃弹性体/共混物组合物的总重量计。
在一些方面,交联体系可以包括和使用辐射、热、水分和额外的缩合催化剂的组合中的一种或全部。在一些方面,缩合催化剂可以以0.25重量%至8重量%的量存在。在其它方面,可以以约1重量%至约10重量%或约2重量%至约5重量%的量包括缩合催化剂。
发泡剂
发泡剂可以是化学发泡剂(例如有机或无机发泡剂)和/或物理发泡(例如气体和挥发性低重量分子),其被在挤出和/或模塑过程中添加到硅烷接枝的聚烯烃弹性体和缩合催化剂共混物中以制备发泡的硅烷交联的聚烯烃弹性体。
在一些方面,发泡剂可以是物理发泡剂,包括微胶囊化的发泡剂,其在本领域中也被称为微胶囊化的起泡剂(MEBA)。MEBA包括一族物理发泡剂,其被定义为可热膨胀的微球,其通过将挥发性烃包封到丙烯酸系共聚物壳中而形成。当所述丙烯酸系共聚物壳膨胀时,所述挥发性烃(例如丁烷)在所述可硅烷交联的聚烯烃弹性体中产生泡沫并减轻其重量。在一些方面,所述MEBA具有约20μm至约30μm的平均粒度。示例性的MEBA包括以商品名MATSUMOTO F-AC170D销售的那些。在一些方面,MEBA可以与包括有机和无机发泡剂在内的其它发泡剂组合使用。
在一些方面,发泡剂可以是吸热和/或放热发泡化合物的组合,其在温度高于150℃的模具中能够使用水释放剂产生泡结构以加速硫化时间,例如40秒至100秒。
可以使用的有机发泡剂可以包括例如偶氮化合物,例如偶氮二酰胺(ADCA),偶氮二羧酸钡,偶氮二异丁腈(AIBN),偶氮环己腈和偶氮二氨基苯;N-亚硝基化合物,例如N,N'-二亚硝基五亚甲基四胺(DPT),N,N'-二甲基-N,N'-二亚硝基对苯二甲酰胺和三亚硝基三甲基三胺;酰肼化合物,例如4,4'-氧双(苯磺酰肼)(OBSH),对甲苯磺酰肼,二苯砜-3,3'-二磺酰肼,2,4-甲苯二磺酰肼,对,对-双(苯磺酰肼)醚,苯-1,3-二磺酰肼,和烯丙基双(磺酰肼);氨基脲化合物,例如对甲苯磺酰基氨基脲和4,4'-氧双(苯磺酰基氨基脲);氟代烷,例如三氯一氟甲烷和二氯一氟甲烷;和三唑化合物,例如5-吗啉基-1,2,3,4-噻三唑,和其它已知的有机发泡剂。在一些方面,使用偶氮化合物和N-亚硝基化合物。在其它方面,使用偶氮二酰胺(ADCA)和N,N'-二亚硝基五亚甲基四胺(DPT)。上面列出的有机发泡剂可以单独使用或以两种或更多种的任何组合使用。
所使用的有机发泡剂的分解温度和量能够对发泡的硅烷交联聚烯烃弹性体的密度和材料性质产生重要影响。在一些方面,有机发泡剂的分解温度为约150℃至约210℃。有机发泡剂的用量可以为约0.1重量%至约40重量%,约5重量%至约30重量%,约5重量%至约20重量%,约10重量%至约30重量%,或约1重量%至约10重量%,基于聚合物共混物的总重量计。如果有机发泡剂的分解温度低于150℃,则在配混过程中可能发生早期发泡。同时,如果有机发泡剂的分解温度高于210℃,则可能需要较长时间(例如大于15分钟)来模塑泡沫体,导致低的生产率。另外的发泡剂可以包括其分解温度在上述范围内的任何化合物。
可以使用的无机发泡剂包括例如碳酸氢盐,如碳酸氢钠和碳酸氢铵;碳酸盐,如碳酸钠和碳酸铵;亚硝酸盐,如亚硝酸钠和亚硝酸铵;硼氢化物,如硼氢化钠;以及其它已知的无机发泡剂如叠氮化物。在一些方面,可以使用碳酸氢盐。在其它方面,可以使用碳酸氢钠。上面列出的无机发泡剂可以单独使用或以两种或更多种的任何组合使用。无机发泡剂的用量可以为约0.1重量%至约40重量%,约5重量%至约30重量%,约5重量%至约20重量%,约10重量%至约30重量%,或约1重量%至约10重量%,基于聚合物共混物的总重量计。
可以使用的物理发泡剂包括例如超临界二氧化碳,超临界氮,丁烷,戊烷,异戊烷,环戊烷。在一些方面,各种矿物或无机化合物(例如滑石和碳酸盐)可以被用作超临界流体的成核剂。物理发泡剂的用量可以为约0.1重量%至约40重量%,约5重量%至约30重量%,约5重量%至约20重量%,约10重量%至约30重量%,或约1重量%至约10重量%,基于聚合物共混物的总重量计。
任选的另外的组分
所述发泡的硅烷交联的聚烯烃弹性体可以任选地包括一种或多种填料。填料可以与硅烷接枝的聚烯烃一起挤出。在一些方面,填料可以包括金属氧化物,金属氢氧化物,金属碳酸盐,金属硫酸盐,金属硅酸盐,粘土,滑石,炭黑和二氧化硅。取决于应用和/或所需的性质,这些材料可以是火成的或煅烧的。
进一步关于所述任选的填料,所述金属氧化物、金属氢氧化物、金属碳酸盐、金属硫酸盐或金属硅酸盐的金属可以选自碱金属(例如锂,钠,钾,铷,铯和钫);碱土金属(例如铍,镁,钙,锶,钡和镭);过渡金属(例如锌,钼,镉,钪,钛,钒,铬,锰,铁,钴,镍,铜,钇,锆,铌,锝,钌,铑,钯,银,铪,钽,钨,铼,锇,铱,铂,金,汞,Rf,钅杜,钅喜,钅波,钅黑和鎶);后过渡金属(例如铝,镓,铟,锡,铊,铅,铋和钋);镧系元素(例如镧,铈,镨,钕,钷,钐,铕,钆,铽,镝,钬,铒,铥,镱和镥);锕系元素(例如,锕,钍,镤,铀,镎,钚,镅,锔,锫,锎,锿,镄,钔,锘和铹);锗;砷;锑;和砹。
所述发泡的硅烷交联的聚烯烃弹性体或共混物的填料可以以在从大于0重量%至约50重量%(包括约1重量%至约20重量%和约3重量%至约10重量%)范围内的量存在。
所述发泡的硅烷交联的聚烯烃弹性体和/或所形成的相应制品(例如中底18)还可以包括蜡(例如石蜡,微晶蜡,HDPE蜡,LDPE蜡,热降解的蜡,副产物聚乙烯蜡,任选氧化的费托蜡和官能化的蜡)。在一些实施方案中,所述蜡以约0重量%至约10重量%的量存在。
增粘树脂(例如脂肪族烃,芳族烃,改性烃,萜烯,改性萜烯,氢化萜烯,松香,松香衍生物,氢化松香及它们的混合物)也可以被包括在所述硅烷交联的聚烯烃弹性体/共混物中。增粘树脂可以具有在70℃至约150℃的范围内的环球软化点和在177℃下小于约3,000cP的粘度。在一些方面,增粘树脂以约0重量%至约10重量%的量存在。
在一些方面,所述发泡的硅烷交联的聚烯烃弹性体可以包括一种或多种油。非限制性的油的类型包括石蜡油和环烷油。在一些实施方案中,油以约0重量%至约10重量%的量存在。
制备发泡的硅烷交联的聚烯烃弹性体的方法
所述发泡的硅烷交联的聚烯烃弹性体的合成/生产可以通过使用单步Monosil工艺在一个挤出机中或使用两步Sioplas工艺在两个挤出机中组合各个组分来进行,这消除了对在挤出之前混合和运输橡胶配混物的额外步骤的需要。
现在参考图3,提供了在用于合成所述发泡的硅烷交联的聚烯烃弹性体的单步Monosil工艺和两步Sioplas工艺过程中使用的通用化学过程。该过程从接枝步骤开始,该接枝步骤包括由接枝引发剂引发,然后与第一和第二聚烯烃增长和链转移。所述接枝引发剂(在一些方面,过氧化物或偶氮化合物)均裂解以形成两个自由基引发剂片段,其通过增长步骤转移到第一和第二聚烯烃链之一上。现在位于第一或第二聚烯烃链上的自由基然后可以转移到硅烷分子和/或另一个聚烯烃链上。一旦引发剂和自由基被消耗,第一和第二聚烯烃的硅烷接枝反应就完成了。
仍参考图3,一旦硅烷接枝反应完成,就产生了稳定的第一和第二硅烷接枝聚烯烃的混合物。然后可以将交联催化剂加入到所述第一和第二硅烷接枝聚烯烃中以形成硅烷接枝的聚烯烃弹性体。交联催化剂可首先促进接枝到聚烯烃主链上的甲硅烷基的水解,以形成反应性硅烷醇基团。然后,所述硅烷醇基团可以与在其它聚烯烃分子上的其它硅烷醇基团反应以形成通过硅氧烷键连接在一起的弹性体聚烯烃聚合物链的交联网络。整个硅烷接枝的聚烯烃弹性体中硅烷交联键的密度能够影响弹性体所表现出的材料性能。
现在参考图4和5A,显示了使用两步Sioplas工艺制备中底18的方法200。方法200可以从步骤204开始,该步骤204包括一起挤出(例如用双螺杆挤出机252)密度小于0.86g/cm3的第一聚烯烃240、第二聚烯烃244和包括硅烷交联剂(例如乙烯基三甲氧基硅烷(VTMO))和接枝引发剂(例如过氧化二枯基)的硅烷混合物248,以形成硅烷接枝的聚烯烃共混物。可以使用添加料斗256将第一聚烯烃240和第二聚烯烃244添加到反应性双螺杆挤出机252中。所述硅烷混合物248可以被在挤出生产线更下游加入到双螺杆260中,以帮助促进与第一和第二聚烯烃240,244共混物的更好混合。强制的挥发性有机化合物(VOC)真空264可以被用在所述反应性双螺杆挤出机252上,以帮助维持所需的反应压力。双螺杆挤出机252被认为是反应性的,因为自由基引发剂和硅烷交联剂与所述第一和第二聚烯烃240,244反应并与所述第一和第二聚烯烃240,244形成新的共价键。熔融的硅烷接枝聚烯烃共混物可以使用齿轮泵268离开所述反应性双螺杆挤出机252,该齿轮泵268将所述熔融的硅烷接枝聚烯烃共混物注入水造粒机272中,该水造粒机272能够形成粒化的硅烷接枝聚烯烃共混物276。在一些方面,所述熔融的硅烷接枝聚烯烃共混物可以被挤出成粒料、枕型物或任何其它构型,然后引入缩合催化剂280(参见图5B)和形成最终的制品。
所述反应性双螺杆挤出机252可以被构造成具有多个不同的温度区(例如图5A中所示的Z0-Z12),它们在双螺杆挤出机252的不同长度处延伸。在一些方面,各个温度区的温度可以为约室温至约180℃,约120℃至约170℃,约120℃至约160℃,约120℃至约150℃,约120℃至约140℃,约120℃至约130℃,约130℃至约170℃,约130℃至约160℃,约130℃至约150℃,约130℃至约140℃,约140℃至约170℃,约140℃至约160℃,约140℃至约150℃,约150℃至约170℃,和约150℃至约160℃。在一些方面,Z0可具有约60℃至约110℃的温度或不冷却;Z1可具有约120℃至约130℃的温度;Z2可具有约140℃至约150℃的温度;Z3可具有约150℃至约160℃的温度;Z4可具有约150℃至约160℃的温度;Z5可具有约150℃至约160℃的温度;Z6可具有约150℃至约160℃的温度;Z7可具有约150℃至约160℃的温度;Z8-Z12可具有约150℃至约160℃的温度。
在一些方面,硅烷接枝的聚烯烃弹性体的数均分子量可以在约4,000g/mol至约30,000g/mol的范围内,包括约5,000g/mol至约25,000g/mol和约6,000g/mol至约14,000g/mol。所述接枝聚合物的重均分子量可以为约8,000g/mol至约60,000g/mol,包括约10,000g/mol至约30,000g/mol。
现在参考图4和5B,方法200接下来包括将所述硅烷接枝的聚烯烃共混物276和缩合催化剂280一起挤出以形成可硅烷交联的聚烯烃共混物298的步骤208。在一些方面,可以将一种或多种任选的添加剂284与所述硅烷接枝的聚烯烃共混物276和缩合催化剂280一起加入,以调节所述可硅烷交联的聚烯烃共混物的最终材料性能。在步骤208中,将所述硅烷接枝的聚烯烃共混物276与硅烷醇形成缩合催化剂280混合,以在硅烷接枝上形成反应性硅烷醇基团,其随后在暴露于湿气和/或热时能够交联。在一些方面,所述缩合催化剂是280可以包括磺酸、抗氧化剂、加工助剂和用于着色的炭黑的混合物,其中对于此缩合催化剂280来说环境水分足以在较长时间段内(例如约48小时)交联所述可硅烷交联的聚烯烃共混物298。可以使用添加料斗(类似于图5A中的描绘的添加料斗256)和加料齿轮泵296将硅烷接枝的聚烯烃共混物276和缩合催化剂280加入到反应性单螺杆挤出机288中。硅烷接枝的聚烯烃共混物276和缩合催化剂280以及在一些方面一种或多种任选的添加剂284的组合,可以被加入到反应性单螺杆挤出机288的单螺杆292中。单螺杆挤出机288被认为是反应性的,因为所述硅烷接枝的聚烯烃共混物276和缩合催化剂280被熔化并合并在一起以将缩合催化剂280彻底且均匀地混合在整个熔融的硅烷接枝聚烯烃共混物276中。熔融的可硅烷交联的聚烯烃共混物298可通过模头300离开所述反应性单螺杆挤出机288,该模头300能够将所述熔融的可硅烷交联的聚烯烃共混物298注射到鞋底模具302中。
在步骤208过程中,随着所述硅烷接枝的聚烯烃共混物276被与所述缩合催化剂280一起挤出以形成可硅烷交联的聚烯烃共混物298,可发生一定量的交联。在一些方面,所述可硅烷交联的聚烯烃共混物298可以是约25%硫化的,约30%硫化的,约35%硫化的,约40%硫化的,约45%硫化的,约50%硫化的,约55%硫化的,约60%硫化的,约65%硫化的,或约70%硫化的,其中凝胶试验(ASTM D2765)可以被用于测定最终的发泡的硅烷交联聚烯烃弹性体中的交联量。
参考图4和5B,方法200还包括将所述可硅烷交联的聚烯烃共混物298在鞋底模具302中模压成型以形成鞋底部件314的步骤212。特别地,单螺杆挤出机288熔融并通过模头300挤出所述可硅烷交联的聚烯烃298,所述模头300能够将熔融的可硅烷交联的聚烯烃共混物298注射入鞋底模具302的半部306,310中以形成鞋底部件314。如将在图8-11中进一步描述的,所述可硅烷交联的聚烯烃共混物298和部件314也可以使用几种不同的模塑方法之一模塑和硫化,所述模塑方法包括:模压成型(图8),注射成型(图9),注射模压成型(图10)和超临界注射成型(图11)。
再次参考图4,方法200可以还包括使所述可硅烷交联的聚烯烃共混物298和鞋底部件314在150℃和400℃之间,150℃和300℃之间,150℃和200℃之间,大于150℃,大于175℃,大于200℃,约150℃,约180℃或约200℃的温度交联以形成中底18(参见图1)的步骤216。另外,所述使可硅烷交联的聚烯烃共混物298和鞋底部件314交联的步骤216可以在环境湿度或在加压蒸汽下进行,以形成具有约0.15g/cm3至约0.40g/cm3的密度的中底18。更具体地,在该交联过程中,水使所述可硅烷交联的聚烯烃弹性体的硅烷水解以产生硅烷醇。在各硅烷接枝上的硅烷醇基团然后能够被缩合以形成分子间的、不可逆的Si-O-Si交联位点。通过控制生产过程,包括所使用的催化剂的量,能够调节交联的硅烷基团的量和因此最终的聚合物性能。
方法200的步骤216的交联/硫化可以在从大于0至约20小时的时间段内发生。在一些方面,在约60秒至400秒,1小时至约20小时,10小时至约20小时,约15小时至约20小时,约5小时至约15小时,约1小时至约8小时,或约3小时至约6小时的时间段内发生硫化。硫化过程中湿度可以为约30%至约100%、约40%至约100%或约50%至约100%。
在一些方面,使用能够在接近TPV加工条件的注射成型热设置下注射成型热塑性塑料的注射成型设置,其中挤出物在环境条件下交联从而变成热固性的。在其它方面,可以通过蒸汽暴露来加速该过程。在刚刚成型之后,凝胶含量(也称为交联密度)可以为约60%,但在环境条件下96小时后,凝胶含量可以达到大于约95%。
应当理解,前面概述和教导中底18及它们各自的组分/组成的描述可以被以任何组合形式使用且同样适用于图4中显示的使用两步Sioplas工艺制备中底18的方法200。
现在参考图6和7,显示了使用一步Monosil工艺制备中底18的方法400。方法400可以从步骤404开始,该步骤404包括一起挤出(例如用单螺杆挤出机444)密度小于0.86g/cm3的第一聚烯烃240、第二聚烯烃244、包括硅烷交联剂(例如乙烯基三甲氧基硅烷(VTMO))和接枝引发剂(例如过氧化二枯基)的硅烷混合物248和缩合催化剂280,以形成可交联的硅烷接枝的聚烯烃共混物298。可以使用添加料斗440将第一聚烯烃240、第二聚烯烃244和硅烷混合物248添加到反应性单螺杆挤出机444中。在一些方面,所述硅烷混合物248可以被在挤出生产线更下游加入到单螺杆448中,以帮助促进与第一和第二聚烯烃240,244共混物的更好混合。在一些方面,一种或多种任选的添加剂284可以被与第一聚烯烃240、第二聚烯烃244和硅烷混合物248一起添加,以改变可硅烷交联的聚烯烃共混物298的最终材料性能。单螺杆挤出机444被认为是反应性的,因为硅烷混合物248的自由基引发剂和硅烷交联剂与所述第一和第二聚烯烃240,244反应并与所述第一和第二聚烯烃240,244形成新的共价键。另外,所述反应性单螺杆挤出机444将缩合催化剂280与熔融的硅烷接枝的聚烯烃共混物276一起混合。熔融的可硅烷交联的聚烯烃共混物298可以使用齿轮泵(未示出)和/或模头300离开反应性单螺杆挤出机444,所述齿轮泵和/或模头300能够将所述熔融的可硅烷交联的聚烯烃共混物298喷射到鞋底模具302中。
在步骤404期间,随着第一聚烯烃240、第二聚烯烃244、硅烷混合物248和缩合催化剂280被一起挤出时,在反应性单螺杆挤出机444中可以发生一定量的交联。在一些方面,当离开反应性单螺杆挤出机444时,所述可硅烷交联的聚烯烃共混物298可以是约25%硫化的,约30%硫化的,约35%硫化的,约40%硫化的,约45%硫化的,约50%硫化的,约55%硫化的,约60%硫化的,约65%硫化的,或约70%硫化的。凝胶试验(ASTM D2765)可以被用于测定最终的发泡的硅烷交联聚烯烃弹性体中的交联量。
所述反应性单螺杆挤出机444可以被构造成具有多个沿挤出机的不同长度延伸的不同温度区(例如图7中所示的Z0-Z7)。在一些方面,各个温度区的温度可以在以下范围内:约室温至约180℃,约120℃至约170℃,约120℃至约160℃,约120℃至约150℃,约120℃至约140℃,约120℃至约130℃,约130℃至约170℃,约130℃至约160℃,约130℃至约150℃,约130℃至约140℃,约140℃至约170℃,约140℃至约160℃,约140℃至约150℃,约150℃至约170℃,和约150℃至约160℃。在一些方面,Z0可具有约60℃至约110℃的温度或不冷却;Z1可具有约120℃至约130℃的温度;Z2可具有约140℃至约150℃的温度;Z3可具有约150℃至约160℃的温度;Z4可具有约150℃至约160℃的温度;Z5可具有约150℃至约160℃的温度;Z6可具有约150℃至约160℃的温度;和Z7可具有约150℃至约160℃的温度。
在一些方面,所述硅烷接枝的聚烯烃弹性体的数均分子量可以在约4,000g/mol至约30,000g/mol的范围内,包括约5,000g/mol至约25,000g/mol和约6,000g/mol至约14,000g/mol。所述接枝聚合物的重均分子量可以为约8,000g/mol至约60,000g/mol,包括约10,000g/mol至约30,000g/mol。
参考图6和7,方法400还包括将所述可硅烷交联的聚烯烃共混物298在鞋底模具302中模塑成鞋底部件314的步骤412。单螺杆挤出机444熔融并通过模头300挤出所述可硅烷交联的聚烯烃298,所述模头300能够将熔融的可硅烷交联的聚烯烃共混物298注射入鞋底模具302的半部306,310中。如将在图8-11中进一步描述的,所述可硅烷交联的聚烯烃共混物298和部件314也可以使用几种不同的模塑方法之一模塑和硫化,所述模塑方法包括:模压成型(图8),注射成型(图9),注射模压成型(图10)和超临界注射成型(图11)。
仍参考图6,方法400可以还包括使所述可硅烷交联的聚烯烃共混物298和鞋底部件314在150℃和400℃之间,150℃和300℃之间,150℃和200℃之间,大于150℃,大于175℃,大于200℃,约150℃,约180℃或约200℃的模塑温度下交联以形成中底18(参见图1)的步骤412。另外,所述使可硅烷交联的聚烯烃共混物298和鞋底部件314交联的步骤412可以在环境湿度或在加压蒸汽下进行,以形成具有约0.15g/cm3至约0.40g/cm3的密度的中底18。通过控制生产过程,包括所使用的催化剂的量,能够调节交联的硅烷基团的量和因此最终的聚合物性能。
交联所述可硅烷交联的聚烯烃共混物298的步骤412可以在从大于0至约20小时的时间段内发生,或者可以是在大于150℃或约180℃的温度下40秒至400秒。在一些方面,硫化在约1小时至约20小时,10小时至约20小时,约15小时至约20小时,约5小时至约15小时,约1小时至约8小时,或约3小时至约6小时的时间段内发生。交联和硫化期间的温度(模具温度)可以是约室温,约150℃,约180℃,约20℃至约225℃,约20℃至约200℃,约25℃至约100℃,约20℃至约75℃。硫化期间的湿度可以为约30%至约100%、约40%至约100%或约50%至约100%。
在一些方面,使用能够在接近TPV加工条件的注射成型热设置下注射成型热塑性塑料的注射成型设置,其中挤出物在环境条件下或在升高的温度下交联从而变成热固性的。在其它方面,可以通过蒸汽暴露来加速该过程。在刚刚成型之后,凝胶含量(也称为交联密度)可以为约60%,但在环境条件下96小时后,凝胶含量可以达到大于约95%。
应当理解,可以被以任何组合形式使用的、概述和教导前面讨论的各种中底18及它们各自的组分/组成的描述同样适用于使用一步Monosil工艺制备中底18的方法400。
模塑技术
将可硅烷交联的聚烯烃弹性体共混物298注射或添加到鞋底模具302中以形成鞋底部件314(参见图4-7)可以使用几种不同方法中的一种进行。取决于所选择的模塑方法,可以获得中底18的不同材料性能。可以通过使用以下四种方法之一来进行模塑:模压成型(图8),注射成型(图9),注射模压成型(图10)和超临界注射成型(图11)。
参考图8,提供了压缩模具458的示意性剖视图。按照模压成型方法,可硅烷交联的聚烯烃弹性体298(或鞋底部件314,未显示)被在压缩模具458中加压或在预定的温度、压力和时间条件下压制,以获得呈板状海绵形式的发泡的硅烷交联的聚烯烃弹性体(未显示)。所述压缩模具458包括上模具460和下模具464。随着所述可硅烷交联的聚烯烃弹性体298被在压缩模具458中加热和压制,化学和/或物理发泡剂被活化以形成所述发泡的硅烷交联的聚烯烃弹性体。然后可以将板状海绵的一些部分和/或边缘切削、切割和/或研磨成具有所希望的厚度和形状的中底18(参见图1-2)。随后,所述中底18被再次在最终模具中在热和压力下与大底14和其它各组件模制,并且然后在冷却期间在模具的闭合状态下对组件加压(该过程在鞋工业中被称为phylon模制),以生产最终的鞋底(例如鞋底10)。
现在参考图9,提供了一种注射模具的示意性剖视图。按照注射成型方法,在Sioplas或Monosil工艺中使用的反应性单螺杆挤出机288,444制备可硅烷交联的聚烯烃弹性体298并将其注射入具有上模306和下模310的模具302中。在将可硅烷交联的聚烯烃弹性体298初始注射入模具302中后,形成未硫化的中底18a,如图9的步骤1中所提供的。随着未硫化的中底18a被加热和硫化,化学和/或物理发泡剂被活化以形成发泡的硅烷交联的聚烯烃弹性体。在这些方面中使用的模具302被设计成具有比最终的硫化的中底18(发泡的硅烷交联聚烯烃弹性体)的尺寸小的尺寸。在可硅烷交联的聚烯烃弹性体发泡和膨胀之后,所述未硫化的中底18a膨胀至所需的中底18尺寸并且所述模具302释放最终制品,如图9的步骤2中所提供的。
参考图10,提供了一种注射压缩模具的示意性剖视图。注射压缩模具通过利用图8中描述的模压成型和图9中描述注射成型两者的特征提供了用于形成中底18的混合方法。按照注射压缩方法,在Sioplas或Monosil工艺中使用的反应性单螺杆挤出机288,444制备可硅烷交联的聚烯烃弹性体298并将其注射入具有上模306和下模310的模具302中,如图10的步骤1中所提供的。然后所述可硅烷交联的聚烯烃弹性体298被在模具302中加热和压制以形成未硫化的中底18a,同时化学和/或物理发泡剂被活化以形成发泡的硅烷交联的聚烯烃弹性体,构成最终的硫化的中底18,如图10的步骤2中所提供的。在这些注射压缩方法中使用的模具302被设计成具有比最终的硫化的中底18(发泡的硅烷交联聚烯烃弹性体)的尺寸小的尺寸。在硅烷交联的聚烯烃弹性体发泡和膨胀之后,释放模具以取出最终的硫化的中底18,如图10的步骤3中所提供的。
现在参考图11,提供了一种配有超临界流体注射器484的反应性单螺杆挤出机480的示意性剖视图。该方法由一起挤出(例如用所述反应性单螺杆挤出机480)密度小于0.86g/cm3的第一聚烯烃240、第二聚烯烃244、包括硅烷交联剂(例如乙烯基三甲氧基硅烷VTMO)和接枝引发剂(例如过氧化二枯基)的硅烷混合物248以及缩合催化剂280以形成可交联的硅烷接枝的聚烯烃共混物298开始。可以使用添加料斗440和齿轮泵268将第一聚烯烃240、第二聚烯烃244和硅烷混合物248添加到反应性单螺杆挤出机480中。在一些方面,硅烷混合物248可以被在挤出生产线更下游添加到单螺杆448中,以帮助促进与第一和第二聚烯烃240,244共混物的更好混合。在一些方面,可以将一种或多种任选的添加剂284与第一聚烯烃240、第二聚烯烃244和硅烷混合物248一起添加,以调整可硅烷交联的聚烯烃共混物298的最终材料性能。
仍参考图11,所述超临界流体注射器484可以被用于在将可硅烷交联的聚烯烃共混物298通过模头300注射入模具302之前将超临界流体如二氧化碳或氮气加入到所述可硅烷交联的聚烯烃共混物298中。然后,所述反应性单螺杆挤出机480将所述可硅烷交联的聚烯烃弹性体298注射入具有上模306和下模310的模具302中。在将可硅烷交联的聚烯烃弹性体298初始注射入模具302中后,形成未硫化的中底18a,如图11的步骤1中所提供的。随着所述未硫化的中底18a被加热和硫化,所述超临界流体发泡剂膨胀以形成发泡的硅烷交联的聚烯烃弹性体。在这些方面中使用的模具302被设计成具有比最终的硫化的中底18(发泡的硅烷交联的聚烯烃弹性体)的尺寸小的尺寸。在发泡之后,使用芯拉回使所述发泡的硅烷交联的聚烯烃弹性体膨胀至所需的中底18尺寸以适应膨胀,并且模具释放,如图11的步骤2中所提供的。
发泡的硅烷交联的聚烯烃弹性体的物理性能
本文中使用的“热塑性塑料”被定义为是指当暴露于热时软化并在冷却至室温时恢复其初始状态的聚合物。本文中使用的“热固性塑料”被定义为是指当被硫化时固化并且不可逆地“固定”或“交联”的聚合物。在上述的Monosil工艺或Sioplas工艺中,重要的是理解用于生产最终的热固性发泡硅烷交联聚烯烃弹性体或中底18的各种不同材料的热塑性和热固性性能的仔细平衡。使用反应性双螺杆挤出机、非反应性单螺杆挤出机和反应性单螺杆挤出机混合和反应的中间体聚合物材料中的每一种是热固性塑料。因此,所述硅烷接枝的聚烯烃共混物和所述可硅烷交联的聚烯烃共混物是热塑性的并且能够通过加热被软化,因此各种材料可以流动。一旦所述可硅烷交联的聚烯烃共混物被挤出、模塑、压制和/或成形入鞋底模具302或其它各自制品,所述可硅烷交联的聚烯烃共混物能够在大于150℃的温度和环境湿度下开始交联或硫化,以形成中底18和发泡的硅烷交联的聚烯烃共混物。在高于150℃的温度下,所述可硅烷交联的聚烯烃共混物能够在40秒至400秒,40秒至200秒,40秒至100秒或约60秒的模塑时间内发泡和交联。
所述可硅烷交联的聚烯烃共混物和相应的发泡的硅烷交联聚烯烃共混物的热塑性/热固性行为对于本文中公开的各种组合物和制品(例如图1中显示的中底18)来说是重要的,原因在于使用这些材料所提供的潜在的能量节约。例如,因为能够在高于150℃的温度和环境湿度下硫化所述可硅烷交联的聚烯烃共混物,制造商能够节省大量的能量。该硫化过程在工业中通常通过施加大量能量来加热或蒸汽处理可交联的聚烯烃来进行。采用相对低的温度和/或环境湿度或者通过在升高的温度下缩短的硫化时间硫化本发明的可硅烷交联的聚烯烃共混物的能力不是可交联聚烯烃必然具有的性能。相反,这种温度/湿度硫化能力是依赖于所述可硅烷交联的聚烯烃共混物的相当低的密度的性能。在一些方面,除了挤出机中所提供的以外,不使用额外的硫化炉、加热炉、蒸汽炉或其它形式的生热机器来形成所述发泡的硅烷交联的聚烯烃弹性体。
本公开的发泡的硅烷交联聚烯烃弹性体的比重可以低于本领域中使用的现有TPV和EPDM复配物的比重。这些材料的降低的比重可以导致低重量的鞋子,由此帮助鞋制造商满足日益增长的对更轻量鞋的要求。例如,本公开的发泡的硅烷交联聚烯烃弹性体的比重可以为约0.10g/cm3至约0.50g/cm3,约0.15g/cm3至约0.50g/cm3,约0.15g/cm3至约0.40g/cm3,约0.15g/cm3至约0.35g/cm3,约0.20g/cm3至约0.40g/cm3,约0.20g/cm3至约0.45g/cm3,约0.25g/cm3至约0.35g/cm3,约0.30g/cm3至约0.50g/cm3,约0.30g/cm3至约0.40g/cm3,约0.35g/cm3至约0.40g/cm3,约0.50g/cm3,约0.45g/cm3,约0.40g/cm3,约0.35g/cm3,约0.30g/cm3,约0.25g/cm3,约0.20g/cm3,或者约0.15g/cm3,而现有的TPO材料可以具有大于0.35g/cm3或大于0.40g/cm3的比重。
所述发泡的硅烷交联的聚烯烃弹性体可以被作为闭孔泡沫生产。所述发泡的硅烷交联的聚烯烃弹性体的孔大小可以为约0.10mm至约0.50mm,约0.10mm至约0.40mm,约0.10mm至约0.30mm,约0.10mm至约0.25mm,约0.10mm至约0.50mm,或约0.10mm,约0.12mm,约0.14mm,约0.16mm,约0.18mm,约0.20mm,约0.22mm,约0.24mm,约0.26mm,约0.28mm,或约0.30mm。
已经观察了本公开的示例性的发泡硅烷交联聚烯烃弹性体(即图例中的“发泡的硅烷交联的聚烯烃弹性体”)的应力/应变行为,与两种常规的EPDM材料相比。本公开的发泡的硅烷交联聚烯烃的应力/应变曲线之间存在较小的面积,与所述两种EPDM化合物的应力/应变曲线之间的面积相比。发泡硅烷交联聚烯烃弹性体的应力/应变曲线之间的这种较小面积对于中底应用来说可能是理想的。弹性体材料通常具有非线性应力-应变曲线,当反复承受应力时具有显著的能量损失。本公开的发泡的硅烷交联的聚烯烃弹性体可以表现出更大的弹性和更小的粘弹性(例如它们具有更线性的曲线并且显示非常低的能量损失)。本文中描述的发泡硅烷交联聚烯烃弹性体的实施方案不具有掺入这些材料中的任何填料或增塑剂,因此它们的相应的应力/应变曲线不具有或显示任何Mullins效应和/或Payne效应。这些发泡的硅烷交联的聚烯烃弹性体不具有Mullins效应是由于在所述发泡的硅烷交联的聚烯烃共混物中没有添加任何填料或增塑剂,因此应力/应变曲线不依赖于最大加载量,以前在没有瞬间和不可逆软化的情况下将遇到该问题。这些硅烷交联的聚烯烃弹性体不具有Payne效应是由于所述硅烷交联的聚烯烃共混物中没有添加任何填料或增塑剂,因此应力-应变曲线不依赖于小应变振幅,以前在没有基于应变幅度的粘弹性储能模量改变的情况下将遇到该问题。
所述发泡的硅烷交联的聚烯烃弹性体或中底18可以显示出约5.0%至约30.0%,约5.0%至约25.0%,约5.0%至约20.0%,约5.0%至约15.0%,约5.0%至约10.0%,约10.0%至约25.0%,约10.0%至约20.0%,约10.0%至约15.0%,约15.0%至约30.0%,约15.0%至约25.0%,约15.0%至约20.0%,约20.0%至约30.0%,约20.0%至约25.0%,或约1.0%至约40.0%的压缩变定,按照ASTM D 395测量(在23℃、50℃、70℃、80℃、90℃、125℃和/或175℃,48小时)。
在其它实施方案中,所述发泡的硅烷交联的聚烯烃弹性体或中底18可以显示出约5.0%至约20.0%,约5.0%至约15.0%,约5.0%至约10.0%,约7.0%至约20.0%,约7.0%至约15.0%,约7.0%至约10.0%,约9.0%至约20.0%,约9.0%至约15.0%,约9.0%至约10.0%,约10.0%至约20.0%,约10.0%至约15.0%,约12.0%至约20.0%,约12.0%至约15.0%,或约1.0%至约50.0%的压缩变定,按照ASTM D 395(在23℃、50℃、70℃、80℃、90℃、125℃和/或175℃,48小时)测量。
所述发泡的硅烷交联的聚烯烃弹性体或中底18可以具有约5%至约40%,约5%至约25%,约5%至约15%,约10%至约20%,约10%至约15%,或约11%至约14%的结晶度,使用密度测量、差示扫描量热法(DSC)、X射线衍射、红外光谱和/或固态核磁谱测定。
所述发泡的硅烷交联的聚烯烃弹性体或中底18可以显示约-75℃至约-25℃,约-65℃至约-40℃,约-60℃至约-50℃,约-50℃至约-25℃,约-50℃至约-30℃,或约-45℃至约-25℃的玻璃化转变温度,按照差示扫描量热法(DSC)测量,使用以5℃/min或10℃/min的速率进行的第二次加热运行。
实施例
以下实施例代表了根据本公开的鞋底、组合物和制备它们的方法的某些非限制性实例。
材料
所有化学品、前体和其它成分均从商业供应商获得并且以供应商所提供的形式使用,无需进一步纯化。
实施例1
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出48.7重量%ENGAGETMXLT8677或XUS 38677.15和48.7重量%ENGAGETM8842以及2.6重量%SILAN RHS14/032或SILFIN 29,以形成ED108-2A硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.17kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.3重量%的气体加载量,注射速度为75mm/s。所用ED108-2A材料的重量为153.9克。使用上述方法制备两个不同的中底样品,其中第一个样品具有更少和更大的泡孔,而第二个样品具有更小的泡孔。使用密度标尺测量,第一个样品的密度为0.609g/cm3,第二个样品的密度为0.477g/cm3。没有添加缩合催化剂。实施例1的材料性能被列于下表1中,其中压缩变定值按照ASTM D 395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。下面提供的每个实施例的压缩变定数据通过如下方法获得:在50℃下将各个样品以25%和50%的幅度压缩6小时,然后在从试验台上取下样品后30分钟、24小时和48小时时进行压缩变定测量。
表1
实施例2
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出48.7重量%ENGAGETMXLT8677或XUS 38677.15和48.7重量%ENGAGETM8842以及2.6重量%SILAN RHS14/032或SILFIN 29,以形成ED108-2A硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.29kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.5重量%的气体加载量,注射速度为75mm/s。所用ED108-2A材料的重量为153.7克。使用密度标尺测量,所得样品的密度为0.392g/cm3。没有添加缩合催化剂,精密开口为0.7mm。实施例2的材料性能被列于下表2中,其中压缩变定值按照ASTM D 395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。
表2
实施例3
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出48.7重量%ENGAGETMXLT8677或XUS 38677.15和48.7重量%ENGAGETM8842以及2.6重量%SILAN RHS14/032或SILFIN 29,以形成ED108-2A硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.29kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.5重量%的气体加载量,注射速度为75mm/s。所用ED108-2A材料的重量为153.4克。使用密度标尺测量,所得样品的密度为0.382g/cm3。没有添加缩合催化剂,精密开口为1.5mm。实施例3的材料性能被列于下表3中,其中压缩变定值按照ASTM D 395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。
表3
实施例4
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出48.7重量%ENGAGETMXLT8677或XUS 38677.15和48.7重量%ENGAGETM8842以及2.6重量%SILAN RHS14/032或SILFIN 29,以形成ED108-2A硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.29kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.5重量%的气体加载量,注射速度为75mm/s。所用ED108-2A材料的重量为153.6克。使用密度标尺测量,所得样品的密度为0.373g/cm3。没有添加缩合催化剂。精密开口为2mm。在图12中提供了在此实施例中阐述的、使用超临界流体方法形成的中底的横截面的显微照片。实施例4的材料性能被列于下表4中,其中压缩变定值按照ASTM D 395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。
表4
实施例5
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出48.7重量%ENGAGETMXLT8677或XUS 38677.15和48.7重量%ENGAGETM8842以及2.6重量%SILAN RHS14/032或SILFIN 29,以形成ED108-2A硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.29kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.5重量%的气体加载量,注射速度为75mm/s。所用ED108-2A材料的重量为153.7克。使用密度标尺测量,所得样品的密度为0.543g/cm3。没有添加缩合催化剂,精密开口为3.5mm。实施例5的材料性能被列于下表5中,其中压缩变定值按照ASTM D 395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。
表5
实施例6
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出82.55重量%ENGAGETM8842和14.45重量%MOSTENTMTB 003以及3.0重量%SILAN RHS 14/032或SILFIN29,以形成ED76-4A硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.29kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.5重量%的气体加载量,注射速度为75mm/s。所用ED76-4A材料的重量为154.3克。使用密度标尺测量,所得样品的密度为0.420g/cm3。添加RHS 16/001N作为缩合催化剂,精密开口为2mm。实施例6的材料性能被列于下表6中,其中压缩变定值按照ASTM D 395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。
表6
实施例7
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出60重量%INFUSE 9530,30重量%INFUSE 9817和8重量%PP Ml 25(熔体指数为25的聚丙烯)以及2.0重量%SILAN RHS 14/032或SILFIN 29,以形成RH 17/021硅烷接枝的聚烯烃弹性体。接下来,使用配备有超临界流体注射器484的反应性单螺杆挤出机480(参见图11)来进一步处理该共混物,其中超临界流体介质是氮气(N2),气体流量为0.29kg/h。注射器打开时间为10秒,压力保持在140巴。使用0.5重量%的气体加载量,注射速度为75mm/s。所用RHS 17/021材料的重量为146克。使用密度标尺测量,所得样品的密度为0.449g/cm3。没有添加缩合催化剂,精密开口为2mm。实施例7的材料性能被列于下表7中,其中压缩变定值按照ASTM D395测量,密度值通过测量样品的重量、长度、宽度和厚度(大约9cm×10cm,并且厚度为0.2-0.5cm)来测量。
表7
实施例8
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出82.55重量%ENGAGETM8842和14.45重量%MOSTENTMTB 003以及3.0重量%SILAN RHS 14/032或SILFIN29,以形成ED76-4A硅烷接枝的聚烯烃弹性体。接下来,使用反应性单螺杆挤出机288来加载和挤出硅烷接枝的聚烯烃弹性体以及1.0重量%二月桂酸二辛基锡(DOTL)缩合催化剂和10重量%MEBA化学发泡剂。相应的发泡的硅烷交联聚烯烃弹性体中底18的密度为0.304g/cm3,使用密度标尺测量。实施例8的压缩变定数据被列于下表8中。图13提供了根据此实施例的、使用MEBA化学发泡剂形成的中底的横截面的三个不同显微照片。
表8
实施例9
发泡的中底如下制备:使用反应性双螺杆挤出机252(参见图5A)挤出82.55重量%ENGAGETM8842和14.45重量%MOSTENTMTB 003以及3.0重量%SILAN RHS 14/032或SILFIN29,以形成ED76-4A硅烷接枝的聚烯烃弹性体。然后使用反应性单螺杆挤出机288来加载和挤出硅烷接枝的聚烯烃弹性体以及1.0重量%二月桂酸二辛基锡(DOTL)缩合催化剂和10重量%MEBA化学发泡剂。相应的发泡的硅烷交联聚烯烃弹性体中底18的密度为0.25g/mL3,使用密度标尺测量。实施例9的压缩变定数据被列于下表9中。而且,图14是根据此实施例的、使用化学发泡剂形成的中底的横截面的显微照片。
表9
本领域普通技术人员将理解,所描述的装置和其它部件的构造可以不限于任何特定材料。除非本文另有说明,否则本文中公开的装置的其它示例性实施方案可以由各种各样的材料形成。
就本公开而言,术语“偶联的”(以其所有形式,偶联、连接、偶联的等)通常是指两个部件(电子或机械的)直接或间接地彼此连接。这种连接性质上可以是固定的或者性质上是可移动的。这种连接可以通过彼此完整地形成为一个整体的所述两个部件(电子或机械的)和任何另外的中间构件实现,或者可以由上述两个部件(电子或机械的)实现。这种连接性质上可以是永久性的,或者性质上可以是可移除的或可释放的,除非另有说明。
同样重要的是要注意,示例性实施方案中所显示的装置的构造和元件布置仅是说明性的。尽管在本公开中仅详细描述了本发明的一些实施方案,但是阅读了本公开的本领域技术人员将容易理解,许多修改(例如各种元件的大小、尺寸、结构、形状和比例,参数的值,安装布置,材料的使用,颜色,取向等的变化)是可能的,而不实质性地偏离所述主题的新颖教导和优点。例如,被显示为整体形成的元件可以由多个部件构成,或者被显示为多个部件的元件可以被整体形成,界面的操作可以颠倒或以其它方式变化,系统的结构和/或构件或连接器或其它元件的长度或宽度可以改变,元件之间所提供的调节位置的性质或数量可以改变。应该注意的是,系统的元件和/或组件可以由各种各样材料中的任何一种构成,所述材料以各种各样的颜色、纹理和组合提供足够的强度或耐久性。因此,所有这样的修改应被包括在本发明的范围内。在不脱离本发明的精神的情况下,可以在所述理想的和其它示例性的实施方案的设计、操作条件和安排方面进行其它替换、修改、改变和省略。
应该理解,任何所描述的方法或所描述的方法中的步骤可以与其它所公开的方法或步骤组合以形成在本装置范围内的结构。本文中公开的示例性结构和方法用于举例说明的目的,而不应被解释为限制。
还应该理解,在不脱离本发明的概念的情况下,可以对前述结构进行变化和修改,并且还应理解,这些概念意图由所附权利要求覆盖,除非这些权利要求的语言明确另有说明。
以上描述被认为仅是举例说明的实施方案的描述。本领域技术人员以及制造或使用所述装置的人员将能够想到该装置的修改。因此,应该理解,附图中显示和上文所描述的实施方案仅用于说明的目的,并非意图限制由所附权利要求书定义的装置的范围,所述权利要求书应按照专利法的原则解释,包括等同原则。
非限制性实施方案列表
实施方案A是鞋底,其包含一种组合物,该组合物包含密度小于0.50g/cm3的发泡的硅烷交联聚烯烃弹性体,其中所述鞋底具有约1.0%至约50.0%的压缩变定,根据ASTM D395测量(48小时,50℃)。
实施方案A的鞋底,其中所述密度小于约0.30g/cm3。
实施方案A或具有任何介入特征的实施方案A的鞋底,其中所述鞋底具有约50至约52的Asker C硬度。
实施方案A或具有任何介入特征的实施方案A的鞋底,其中所述压缩变定为约15.0%至约20.0%。
实施方案A或具有任何介入特征的实施方案A的鞋底,其还包含着色剂。
实施方案A或具有任何介入特征的实施方案A的鞋底,其中所述硅烷接枝的聚烯烃弹性体包含密度小于0.86g/cm3的第一聚烯烃、结晶度小于40%的第二聚烯烃、硅烷交联剂、接枝引发剂、缩合催化剂和发泡剂。
实施方案A或具有任何介入特征的实施方案A的鞋底,其中所述鞋底具有至少60%的回弹性。
实施方案B是制造鞋底的方法,该方法包括:将密度小于0.86g/cm3的第一聚烯烃、第二聚烯烃、硅烷交联剂和自由基引发剂一起挤出,以形成硅烷接枝的聚烯烃共混物;将所述硅烷接枝的聚烯烃共混物、发泡剂和缩合催化剂一起挤出,以形成可交联的聚烯烃共混物;将所述可交联的聚烯烃共混物注射成型成鞋底部件;和在大于150℃的温度和环境湿度下交联所述可交联的聚烯烃共混物,以形成密度小于0.50g/cm3的鞋底。
实施方案B的方法,其中所述鞋底具有小于0.35g/cm3的密度。
实施方案B或具有任何介入特征的实施方案B的方法,其中所述发泡剂包含超临界流体。
实施方案B或具有任何介入特征的实施方案B的方法,其中所述鞋底具有约1.0%至约50.0%的压缩变定,根据ASTM D 395测量(48小时,50℃)。
实施方案B或具有任何介入特征的实施方案B的方法,其中所述鞋底具有至少60%的回弹性。
实施方案B或具有任何介入特征的实施方案B的方法,其中所述硅烷接枝的聚烯烃弹性体包含约60重量%至约85重量%的第一聚烯烃和约10重量%至约35重量%的第二聚烯烃。
实施方案B或具有任何介入特征的实施方案B的方法,其中所述鞋底具有约50至约52的Asker C硬度。
实施方案C是制造鞋底的方法,该方法包括:将密度小于0.86g/cm3的第一聚烯烃、第二聚烯烃、硅烷交联剂和自由基引发剂一起挤出,以形成硅烷接枝的聚烯烃共混物;将所述硅烷接枝的聚烯烃共混物、发泡剂和缩合催化剂一起挤出,以形成可交联的聚烯烃共混物;将所述可交联的聚烯烃共混物模压成型成鞋底部件;和在大于150℃的温度和环境湿度下交联所述可交联的聚烯烃共混物,以形成密度小于0.50g/cm3的鞋底。
实施方案C的方法,其中所述发泡剂包含超临界流体。
实施方案C或具有任何介入特征的实施方案C的方法,其中所述鞋底具有约1.0%至约50.0%的压缩变定,根据ASTM D 395测量(6小时,50℃)。
实施方案C或具有任何介入特征的实施方案C的方法,其中所述鞋底具有至少60%的回弹性。
实施方案C或具有任何介入特征的实施方案C的方法,其中所述硅烷接枝的聚烯烃弹性体包含约60重量%至约85重量%的第一聚烯烃和约10重量%至约35重量%的第二聚烯烃。
实施方案C或具有任何介入特征的实施方案C的方法,其中所述交联步骤的温度为约180℃,并且所述交联进行40秒至100秒的时间。
Claims (20)
1.鞋底,其包含一种组合物,该组合物包含密度小于0.50g/cm3的发泡的硅烷交联聚烯烃弹性体,其中所述鞋底具有约1.0%至约50.0%的压缩变定,根据ASTM D 395测量(48小时,50℃)。
2.权利要求1所述的鞋底,其中所述密度小于约0.30g/cm3。
3.权利要求1或权利要求2所述的鞋底,其中所述鞋底具有约50至约52的Asker C硬度。
4.权利要求1-3中任一项所述的鞋底,其中所述压缩变定为约15.0%至约20.0%。
5.权利要求1-4中任一项所述的鞋底,其还包含着色剂。
6.权利要求1-5中任一项所述的鞋底,其中所述硅烷接枝的聚烯烃弹性体包含密度小于0.86g/cm3的第一聚烯烃、结晶度小于40%的第二聚烯烃、硅烷交联剂、接枝引发剂、缩合催化剂和发泡剂。
7.权利要求1-6中任一项所述的鞋底,其中所述鞋底具有至少60%的回弹性。
8.制造鞋底的方法,该方法包括:
将密度小于0.86g/cm3的第一聚烯烃、第二聚烯烃、硅烷交联剂和自由基引发剂一起挤出,以形成硅烷接枝的聚烯烃共混物;
将所述硅烷接枝的聚烯烃共混物、发泡剂和缩合催化剂一起挤出,以形成可交联的聚烯烃共混物;
将所述可交联的聚烯烃共混物注射成型成鞋底部件;和
在大于150℃的温度和环境湿度下交联所述可交联的聚烯烃共混物,以形成密度小于0.50g/cm3的鞋底。
9.权利要求8所述的方法,其中所述鞋底具有小于0.35g/cm3的密度。
10.权利要求8或权利要求9所述的方法,其中所述发泡剂包含超临界流体。
11.权利要求8-10中任一项所述的方法,其中所述鞋底具有约1.0%至约50.0%的压缩变定,根据ASTM D 395测量(48小时,50℃)。
12.权利要求8-11中任一项所述的方法,其中所述鞋底具有至少60%的回弹性。
13.权利要求8-12中任一项所述的方法,其中所述硅烷接枝的聚烯烃弹性体包含约60重量%至约85重量%的第一聚烯烃和约10重量%至约35重量%的第二聚烯烃。
14.权利要求8-13中任一项所述的方法,其中所述鞋底具有约50至约52的Asker C硬度。
15.制造鞋底的方法,该方法包括:
将密度小于0.86g/cm3的第一聚烯烃、第二聚烯烃、硅烷交联剂和自由基引发剂一起挤出,以形成硅烷接枝的聚烯烃共混物;
将所述硅烷接枝的聚烯烃共混物、发泡剂和缩合催化剂一起挤出,以形成可交联的聚烯烃共混物;
将所述可交联的聚烯烃共混物模压成型成鞋底部件;和
在大于150℃的温度和环境湿度下交联所述可交联的聚烯烃共混物,以形成密度小于0.50g/cm3的鞋底。
16.权利要求15所述的方法,其中所述发泡剂包含超临界流体。
17.权利要求15或权利要求16所述的方法,其中所述鞋底具有约1.0%至约50.0%的压缩变定,根据ASTM D 395测量(6小时,50℃)。
18.权利要求15-17中任一项所述的方法,其中所述鞋底具有至少60%的回弹性。
19.权利要求15-18中任一项所述的方法,其中所述硅烷接枝的聚烯烃弹性体包含约60重量%至约85重量%的第一聚烯烃和约10重量%至约35重量%的第二聚烯烃。
20.权利要求15-19中任一项所述的方法,其中所述交联步骤的温度为约180℃,并且所述交联进行40秒至100秒的时间。
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