CN113260507A - 包含tpe的发泡片材和由其得到的产品以及制造其的方法 - Google Patents

包含tpe的发泡片材和由其得到的产品以及制造其的方法 Download PDF

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Publication number
CN113260507A
CN113260507A CN201980087170.9A CN201980087170A CN113260507A CN 113260507 A CN113260507 A CN 113260507A CN 201980087170 A CN201980087170 A CN 201980087170A CN 113260507 A CN113260507 A CN 113260507A
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China
Prior art keywords
sheet
less
layer
foam
styrene
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CN201980087170.9A
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Inventor
迈赫迪·萨涅伊
马克·E·林登费尔泽
詹姆斯·K·萨科拉福斯
尼古拉斯·R·托拉科
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MuCell Extrusion LLC
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MuCell Extrusion LLC
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Publication of CN113260507A publication Critical patent/CN113260507A/zh
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Abstract

本公开涉及具有至少一个实心层和在实心层的相反侧或一侧上的至少一个发泡层的包含TPE(例如，TPO)的多层片材。幅宽可以高至3.2米宽且具有小于1％的测量值变化，并且片材在整个幅宽上的每单位面积的重量(克/m2)的平均变化小于2％。本发明的泡沫片材可以具有小于50密耳的总厚度和根据TAPPI/ANSI T 489om‑15在泰伯挺度单位配置中小于5的抗弯挺度值。

Description

包含TPE的发泡片材和由其得到的产品以及制造其的方法
技术领域
本发明涉及可以用于屋顶和地板应用的多层热塑性弹性体泡沫片材。
背景技术
本发明涉及包含热塑性弹性体(TPE)(例如，热塑性烯烃(TPO))泡沫的非交联泡沫片材。片材在整个幅宽(web)上的物理机械特性和厚度均匀性与等效实心对应物的那些相当，或者对于几个特性甚至超过等效实心对应物的那些。本发明中产品的优点在于用于广泛的应用，例如但不限于休闲车(recreational vehicle，RV)车顶和地板、商业屋顶、室内外地板、室内外镶板、土工膜、水保护和保存、浮动挡板、软油箱、诸如遮蓬和横幅的广告应用。
与交联橡胶例如SBR、NBR、EPDM等相比，PET产品由于容易处理和后处理、回收能力、无毒和为环境友好的而得到更多的关注。多层TPE和橡胶片材常规上通过使用粘合材料、粘合剂或/和中间织物层、以及交联剂来粘合几个单层片材而生产。因此，可以在堆叠在一起的几个发泡片材和实心片材之间使用中间粘合层来制造多层发泡片材。然而，所得产品既没有令人满意的层间粘合性，也没有窄的厚度变化，这影响了片材的抗弯挺度。此外，在制造过程中的困难和后处理步骤的数量导致产品昂贵。
专利申请US 2009/0286893公开了生产多层交联TPE泡沫片材的方法，所述多层交联TPE泡沫片材包括至少两个泡沫片材和/或网层、以及用于熔融粘合的TPE膜，其中所有层都应经历热压缩步骤以粘合在一起。
专利申请US 2016/0288455公开了交联的多层TPE泡沫，其中将包含至少交联剂和化学起泡剂的TPE原材料混合并通过捏合机加热直至混合物熔融并均匀地混合，然后将其轧制成片材。然后将粗片材堆叠在一起并经历热压缩过程，在该过程期间粘合和发泡一起发生。
Welsh等在其专利US 6544450 B2中公开了通过牵拉并压缩挤出物来制造具有均匀厚度的热塑性泡沫片材的方法。然而，所得泡沫片材可能不一定具有均匀的每单位面积的重量(g/m2)，因此不一定具有均匀的在整个幅宽上的密度。
本发明的目的是制造共挤出宽多层TPE(例如，TPO)泡沫片材，主要集中在但不限于RV车顶和地板行业，其具有与实心对应物相当的物理机械特性，具有非常稳定的几何形状，例如，在整个幅宽上的测量值变化小于4％)，具有在整个幅宽上的变化小于4％的非常一致的基重，以及与现有商购实心产品的抗弯挺度的数量级相同的抗弯挺度。本发明公开了解决上述加工中的困难(例如，厚度变化)以及现有技术说明的相似方法(例如，用于粘合以及交联的热压缩过程)中的缺点的解决方案，在本发明中我们的方法之一是生产在芯中具有泡沫层的共挤出多层TPE泡沫片材。虽然片材的特性对于市场而言是令人满意的，但是高至10％的测量值变化(其仍然小于商购实心产品的测量值变化)不满足我们的预期。鉴于上述困难和复杂性，需要开发更可行的制造方法来生产多层TPE泡沫片材。因此，本发明公开了多层TPE(例如，TPO)泡沫片材，其包括在实心层的相反侧或一侧上的至少一个发泡层。
发明内容
本发明涉及具有至少一个实心层和在实心层的相反侧或一侧上的至少一个发泡层的包含TPE(例如，TPO)的多层片材。
在一个方面中，提供了共挤出非交联多层热塑性弹性体泡沫片材。所述片材包括至少一个实心层和在实心层的相反侧或一侧上的至少一个热塑性弹性体发泡层。所述片材的整个幅宽上的平均测量值变化(average gauge variation)小于5％和/或所述片材的整个幅宽上的每单位面积的重量(克/m2)的平均变化小于5％。
在一个方面中，提供了共挤出非交联多层热塑性弹性体泡沫片材。所述片材包括至少一个实心层和与实心层相邻的至少一个热塑性弹性体发泡层。所述片材的整个幅宽上的平均测量值变化小于5％和/或所述片材的整个幅宽上的每单位面积的重量(克/m2)的平均变化小于5％。
在一些情况下，非常少量的物理起泡剂(例如，少于1重量％)，优选惰性气体例如氮，可以以超临界状态在非常高的注射压力下引入熔融树脂中以形成单相聚合物/起泡剂混合物。
在一些实施方案中，所得多层片材可以具有在整个幅宽上小于1％的平均测量值变化、在整个幅宽上平均变化小于2％的一致的基重、根据TAPPI/ANSI T 489 om-15小于5的泰伯抗弯挺度、以及根据ASTM D412大于900％的断裂伸长率。
在一些实施方案中，表层的泡沫结构可以包括具有10μm至100μm的平均泡孔尺寸和102个泡孔/cm3至109个泡孔/cm3的泡孔密度的泡孔。由于在本发明的方法中可以不需要后处理步骤，例如，在上述常规方法中说明的将单独的层粘合，因此不存在可导致层间剥离的层间不连续性。
具体实施方式
除非上下文中另外明确指出，否则单数形式包括复数对象。
如在说明书中和权利要求中所使用的，术语“包含/包括”可以包括“由……组成”和“基本上由……组成”的实施方案。
本文所公开的所有范围均包括所列举的端点并且可独立地组合(例如，2g至10g的范围”包括端点2g和10g，以及所有中间值)。
如本文所使用的，近似语言可以应用于修饰可变化而不引起与其相关的基本功能改变的任何定量表术。因此，由一个或多个术语例如“约”和“基本上”修饰的值可以不限于所指定的精确值。修饰语“约”还应被视为公开了由两个端点的绝对值限定的范围。例如，表述“约2至约4”也公开了范围“2至4”。
术语“泡沫”是指当将气体吹入熔融聚合物中时形成的多孔结构，当气体扩散出聚合物时，即在应用热力学不稳定性之后，随着聚合物固化，气泡成核。
术语“幅宽”是指沿横向测量的共挤出片材的宽度，或者在使用环形模具时的平铺宽度。
本公开涉及多层TPE(例如，TPO)泡沫片材，其可以用于广泛应用，例如但不限于休闲车车顶，商业屋顶，室内外地板，室内外镶板，土工膜，水保护，水保存，用于储罐和池塘的覆盖物/底板，浮动挡板，用于地下储库的挡板帘，二次安全壳，软油箱，诸如遮蓬、横幅的广告应用。
常规上，厚多层TPE和橡胶片材包括薄中间层(例如，织物或粘结剂层)以用于粘合或增强的目的。然而，所得产品既没有令人满意的层间粘合性，也没有窄的厚度变化，这可以影响片材的抗弯挺度。此外，在制造过程中的困难和后处理步骤的数量导致产品昂贵。本文所述的多层片材是使用共挤出生产线生产的，其中不同的层在熔融时可以在模具(例如平片模具)内部粘合在一起。因此，不需要在芯层和其他层之间使用中间粘结剂层或粘合层。然后使平坦的挤出物通过冷轧辊以固化，这还可以有助于保持在整个幅宽上的均匀厚度。此外，在通过冷轧辊时，片材的一侧或两侧可以被纹理化、压花或雕刻。
在使用平模生产共挤出多层片材时，通常除了避免褶皱和起皱(其在发生发泡时甚至变得更加显著和严重，从而导致较高的体积输出)之外，最具挑战性的问题是在整个幅宽上具有均匀的厚度以及一致的片材密度分布。将熔体均匀地铺展通过内层例如，芯层是非常困难的，特别是当使用非常宽的片材模具(例如，3米宽)时。无论利用多歧管片材模具的可能性如何，与使用可以改善各层厚度均匀性的组合模块或共挤出模块相比，至关重要的是控制和匹配各层中熔体的粘度。
本公开涉及可以用物理起泡剂生产的共挤出非交联多层TPE(例如，TPO)泡沫片材，其包括至少一个实心层和在一个或更多个实心层的相反侧或一侧上的至少一个发泡层。在另一个实施方案中，共挤出非交联多层热塑性弹性体泡沫片材包括至少一个实心层和至少一个热塑性弹性体发泡层，其中至少一个发泡层与实心层相邻。可能不需要包括用于粘合相邻层的中间层(例如，中间粘结剂层)。
在一个实施方案中，本文所述的产品包括在表层之间的至少一个泡沫层。在另一个实施方案中，任一个表层的发泡倍率(expansion ratio)为约1至1.2。
用于制造一个或更多个泡沫层的起泡剂可以为氮、二氧化碳、或氮和二氧化碳的混合物。在一些情况下，任何种类的化学起泡剂可以为用作发泡剂的一种选择。非常少且精确量的作为加工助剂和起泡剂的上述超临界气体(例如，小于1重量％)可以在作为挤出机筒的延伸部的高效且有效的混合器(例如，腔传递式混合器)的内部，在高压(例如，大于34巴，在一些情况下大于73.8巴，在一些情况下大于240巴，以及在一些情况下大于380巴)下注入到熔融聚合物中。混合器的温度可以精确地控制在±1℃内。包含非常少量的气体，会改变聚合物的粘度，以及精确地控制混合区域的温度可以提供匹配不同层中熔体粘度的可能性。这可以使我们能够在芯和表层的整个幅宽上均匀地铺展熔体，从而可以得到一致的层厚度。本文所述的产品的多层泡沫片材可以生产为至少0.5米宽，在一些情况下至少1.5米宽，在一些情况下至少2米宽，以及在一些情况下至少2.5米宽。
本文所述的多层共挤出泡沫片材的至少一个层可以包含TPE家族中的任何树脂，例如但不限于丙烯-乙烯共聚物、苯乙烯-乙烯-丁二烯-苯乙烯(SEBS)、苯乙烯-丁二烯-苯乙烯(SBS)、苯乙烯-[乙烯-(乙烯-丙烯)]-苯乙烯嵌段共聚物(SEEPS)、苯乙烯-异戊二烯嵌段共聚物(SIS)、热塑性烯烃(TPO)、热塑性聚氨酯(TPU)、可熔融加工橡胶(MeltProcessible Rubbers，MPR)、共聚酯-醚(COPE)、聚醚嵌段酰胺(PEBA)。
本文所述的多层共挤出泡沫片材的至少一个层可以包含任何热塑性树脂，例如但不限于聚乙烯(PE)、聚丙烯(PP)、聚苯乙烯(PS)、乙烯乙酸乙烯酯(EVA)、乙烯乙烯醇(EVOH)、聚氯乙烯(PVC)、聚偏二氯乙烯(PVDC)、聚酰胺(PA)、聚氨酯(PU)、或马来酸酐、或离聚物。
在一些实施方案中，本文所述的多层泡沫片材产品的至少一个层包含小于50重量％的聚丙烯，在一些情况下小于30重量％的PP，在一些情况下小于20重量％的PP，以及在一些情况下小于10重量％的PP。
在一些另外的实施方案中，本文所述的产品可以在表层中的一者或两者中具有适量的着色颜料。
据申请人所知，与已有技术中的制品相比，本文所述的所有多层泡沫片材(其厚度可以为10密耳至400密耳，在一些实施方案中大于400密耳)具有多组改善的物理机械特性和几何特性，如在整个幅宽上的平均测量值变化可以小于1％，以及在整个幅宽上的每单位面积的重量(克/cm3)的平均变化可以小于2％。在一个实施方案中，可以制造厚度小于10密耳的本文所述的产品。
在一些实施方案中，所述的多层泡沫片材在整个幅宽上的平均测量值变化可以小于5％，在一些情况下小于3％，以及在一些情况下小于1％。此外，在一些实施方案中，所述片材在整个幅宽上的每单位面积的重量(克/cm3)的平均变化可以小于5％，在一些实施方案中小于3％，以及在一些另外的实施方案中小于1％。
在一些实施方案中，根据TAPPI/ANSI T 489om-15，本文所述的产品的泰伯抗弯挺度可以小于100，在一些情况下小于50，在一些情况下小于20，以及在一些另外的情况下小于10；其中厚度小于100密耳的片材的泰伯抗弯挺度可以小于10，在一些实施方案中小于5，在一些实施方案中小于2，以及在一些另外实施方案中小于1。
本发明中的多层泡沫片材可以具有与实心非发泡对应物的机械特性相当的机械特性，或者甚至在一些情况下超过实心非发泡对应物的机械特性。在一些情况下，本文所述产品的断裂伸长率可以大于100％。在一些实施方案中，泡沫片材的断裂伸长率可以大于900％。
发泡层的多孔形态可以通过添加0.05重量％至15重量％的成核剂来控制，所述成核剂可以是可以使我们能够在溶解的物理起泡剂的存在下具有异质泡孔成核的任何有机添加剂或无机添加剂。在一个实施方案中，本文所述的多层片材的至少一个层包含含量小于1重量％的成核剂/澄清剂。发泡表层的结构可以包括具有10μm至1000μm的平均泡孔尺寸、102个泡孔/cm3至109个泡孔/cm3的平均泡孔密度、以及1至9的发泡倍率的均匀分散的泡孔。例如，与实心对应物相比，泡沫产品可以具有5％至45％的密度减小。在另一个实施方案中，与非发泡片材相比，泡沫片材可以具有大于45％的密度减小。本发明中使用的所有设备均为常规的聚合物加工设备，为本领域技术人员所熟知并且在文献中被很好地标记和广泛地描述。
在一些情况下，本发明中的多层共挤出产品可以在吹膜工艺或本领域已知的任何其他方法中使用环形模具来生产。
在另一个实施方案中，在芯中包括多孔结构并且在芯层的相反侧上具有实心层和/或发泡层的共挤出多层片材可以属于本发明的产品。
以下实施例示出了本公开的方法。实施例仅为说明性的，并且不旨在对关于本文所阐述的材料、条件、应用、尺寸或加工参数的公开内容进行限制。
实施例
该实施例中的片材包括在共挤出生产线上生产的三个层，该共挤出生产线包括一个6.5英寸主挤出机和一个4.5英寸共挤出机(二者均来自Davis-Standard)，配备有能够注入N2和/或CO2的超临界气体注入单元以及MuCell传递式混合器(MuCell Transfer Mixer，MTM)(二者均来自MuCell Extrusion LLC)，以及120英寸宽的平片模具。
该实施例中的所有样品均用乙烯-丙烯共聚物(对于芯层，其还与20重量％的抗冲改性剂共混)生产。所有层还包含有5.6重量％的抗UV添加剂。将超临界氮用作物理起泡剂并以0.020％至0.06％的浓度非常精确地注入到MuCell传递式混合器(MTM)中。提供实心样品以及芯层被发泡的样品#13用于比较。
为了表征片材的拉伸强度、伸长率(根据ASTM D412)、穿刺强度(根据ASTM F1306)和撕裂强度(根据ASTM D624)，使用来自Tenious Olsen的配备有适合的气动夹具和两个在1000(N)和10(KN)范围内的负荷单元的万能试验机。为了表征片材的抗弯挺度，使用来自Taber Industries的泰伯挺度测试仪150-E型。根据TAPPI/ANSI T 489 om-15在泰伯挺度单位配置中测量样品的抗弯挺度。
下表中列出的所有示出的样品均包括三个层。样品#SOLID为样品#10、#12和#13的实心对应物。与样品#10相比，样品#13在芯中具有泡沫层，#12包括实心芯和在实心芯层的相反侧上的两个泡沫层。与在芯中具有泡沫层的样品#13相比，对于样品#12，在整个幅宽上的测量值变化已改善至小于平均0.7％。
相似地，在样品#12中，平均比重变化(克/cm3)已减小至小于2％。更重要地，与实心样品以及样品#13相比，样品#12中的泰伯抗弯挺度降低至小于1％。
在泰伯单位配置中，样品#12的抗弯挺度急剧下降至小于1，这可能是由于在实心芯层的相反侧上包括发泡表层。样品#12的断裂伸长率得到改善并且超过实心对应物的断裂伸长率。
Figure BDA0003138103150000081

Claims (35)

1.一种共挤出非交联多层热塑性弹性体泡沫片材，包括至少一个实心层和在所述实心层的相反侧或一侧上的至少一个热塑性弹性体发泡层，其中所述片材的整个幅宽上的平均测量值变化小于5％和/或所述片材的整个幅宽上的每单位面积的重量(克/m2)的平均变化小于5％。
2.一种共挤出非交联多层热塑性弹性体泡沫片材，包括至少一个实心层和至少一个热塑性弹性体发泡层，其中至少一个发泡层与所述实心层相邻，以及所述片材的整个幅宽上的平均测量值变化小于5％和/或所述片材的整个幅宽上的每单位面积的重量(克/m2)的平均变化小于5％。
3.根据任一前述权利要求所述的片材，其中所述片材的幅宽为约0.5米至3.2米宽。
4.根据任一前述权利要求所述的膜，其中在相邻层之间不使用粘结剂层。
5.根据任一前述权利要求所述的片材，其中所述片材的整个幅宽上的平均测量值变化小于3％。
6.根据任一前述权利要求所述的片材，其中所述片材的整个幅宽上的每单位面积的重量(克/m2)的平均变化小于3％。
7.根据任一前述权利要求所述的片材，其中所述片材的厚度小于100密耳。
8.根据任一前述权利要求所述的片材，其中根据TAPPI/ANSI T 489om-15在泰伯挺度单位配置中，所述片材的抗弯挺度值小于20。
9.根据任一前述权利要求所述的片材，其中所述片材的厚度小于50密耳。
10.根据任一前述权利要求所述的片材，其中根据TAPPI/ANSI T 489om-15在泰伯挺度单位配置中，所述片材的抗弯挺度值小于5。
11.根据任一前述权利要求所述的片材，其中根据ASTM D624，所述片材的撕裂强度大于38kN/m。
12.根据任一前述权利要求所述的片材，其中根据ASTM F1306，所述片材的最大穿刺力大于30(N)。
13.根据任一前述权利要求所述的片材，其中断裂伸长率大于100％。
14.根据任一前述权利要求所述的片材，其中断裂伸长率大于500％。
15.根据任一前述权利要求所述的片材，其中所述片材的厚度大于50密耳。
16.根据任一前述权利要求所述的片材，其中根据TAPPI/ANSI T 489om-15在泰伯挺度单位配置中，所述片材的抗弯挺度值小于100。
17.根据任一前述权利要求所述的片材，其中至少一个层包含本领域已知为TPE家族的任何树脂，例如但不限于丙烯-乙烯共聚物、苯乙烯-乙烯-丁二烯-苯乙烯(SEBS)、苯乙烯-丁二烯-苯乙烯(SBS)、苯乙烯-[乙烯-(乙烯-丙烯)]-苯乙烯嵌段共聚物(SEEPS)、苯乙烯-异戊二烯嵌段共聚物(SIS)、热塑性烯烃(TPO)、热塑性聚氨酯(TPU)、可熔融加工橡胶(MPR)、共聚酯-醚(COPE)、聚醚嵌段酰胺(PEBA)。
18.根据任一前述权利要求所述的片材，其中至少一个层包含本领域已知为热塑性塑料的任何树脂，例如但不限于聚乙烯(PE)、聚丙烯(PP)、聚苯乙烯(PS)、乙烯-乙酸乙烯酯(EVA)、乙烯乙烯醇(EVOH)、聚氯乙烯(PVC)、聚偏二氯乙烯(PVDC)、聚酰胺(PA)、聚氨酯(PU)、或马来酸酐、或离聚物。
19.根据任一前述权利要求所述的片材，通过平片挤出、吹膜工艺、或本领域已知的任何方法生产。
20.根据任一前述权利要求所述的片材，其通过平片模具或环形挤出模具生产。
21.根据任一前述权利要求所述的片材，其中泡沫层包含泡孔成核剂以及具有10μm至1000μm的平均尺寸和在102个泡孔/cm3至109个泡孔/cm3的范围内的泡孔密度的泡孔，以及所述泡沫层的密度在0.1克/cm3至0.9克/cm3的范围内。
22.根据任一前述权利要求所述的片材，其中在所述发泡层中仅包含0.5重量％至15重量％的无机添加剂和/或有机添加剂作为气泡成核剂。
23.根据任一前述权利要求所述的片材，其中至少一个层包含含量小于1重量％的成核剂/澄清剂。
24.根据任一前述权利要求所述的片材，其中至少一个层包含一些适量的其他添加剂以包括颜料、增滑剂、抗静电剂、UV稳定剂和抗氧化剂。
25.根据任一前述权利要求所述的片材，其中所述片材包括在表层之间的至少一个泡沫层。
26.根据任一前述权利要求所述的片材，其中所述表层的发泡倍率为约1至1.2。
27.根据任一前述权利要求所述的片材，其在一侧的表面上具有纹理，包括任意的压花纹理或雕刻纹理。
28.一种包括根据任一前述权利要求所述的片材的制品。
29.根据任一前述权利要求所述的片材或制品，其中所述片材或所述制品用于休闲车车顶/底板，商业屋顶，室内外地板，室内外镶板，土工膜，水保护，水保存，用于储罐和池塘的覆盖物/底板，浮动挡板，用于地下储库的挡板帘，二次安全壳，软油箱，诸如遮蓬、横幅的广告应用。
30.一种制造根据任一前述权利要求所述的片材的方法，包括在熔融聚合物中引入物理起泡剂以在共挤出生产线中形成单相聚合物/气体混合物，将所述混合物通过模具挤出以形成具有多孔结构的片材，以及使挤出物在冷轧辊之间后成形和固化以形成在整个幅宽上具有均匀厚度、和/或均匀基重(克/cm2)、和/或均匀密度的泡沫片材。
31.根据权利要求30所述的方法，其中所使用的超临界起泡剂为氮、二氧化碳、或氮和二氧化碳的混合物。
32.根据权利要求30所述的方法，其中在大于240巴的注射压力下，将超临界起泡剂引入混合段的内部。
33.根据权利要求30所述的方法，其中将化学起泡剂用作发泡剂。
34.根据权利要求30所述的方法，其中产品通过平片挤出、吹膜工艺或本领域已知的任何方法生产。
35.根据权利要求30所述的方法，其中产品通过平片模具或环形挤出模具生产。
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