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CN106536659B - 用于织物-弹性体粘合的方法 - Google Patents

用于织物-弹性体粘合的方法 Download PDF

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CN106536659B
CN106536659B CN201480080517.4A CN201480080517A CN106536659B CN 106536659 B CN106536659 B CN 106536659B CN 201480080517 A CN201480080517 A CN 201480080517A CN 106536659 B CN106536659 B CN 106536659B
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fabric
rosin
olefin
copolymer
resin
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CN106536659A (zh
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陈勇
陈永春
W·顾
Y·梁
X·庞
H·余
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Dow Global Technologies LLC
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Abstract

本发明涉及用于使织物粘合到聚烯烃弹性体的方法。所述方法包含对织物施用：(a)10到90重量％热塑性聚合物的水性分散液；和(b)90到10重量％松香的水性分散液，其中百分比是基于热塑性聚合物和松香的总干重。

Description

用于织物-弹性体粘合的方法
本发明涉及使用水性粘合剂使织物与聚烯烃弹性体粘合的方法。
已描述使用聚烯烃树脂分散液粘合聚烯烃弹性体与织物。举例来说，JP2002-012812披露用于在织物上施用皮肤涂层的水性聚烯烃分散液。然而，现有技术并未披露在本申请案中所披露的单组分粘合剂配制物。
本发明解决的问题是提供织物与弹性材料的良好粘合。
发明内容
本发明提供用于使织物与聚烯烃弹性体粘合的方法；所述方法包含对织物施用：(a)10到90重量％热塑性聚合物的水性分散液；和(b)10到90重量％松香的水性分散液，其中百分比是基于热塑性聚合物和松香的总干重。
具体实施方式
除非另外规定，否则百分比是重量百分比(wt％)并且温度以℃为单位。对室温(RT)或环境温度的参考表示20-25℃的温度；除非另外说明，否则制备和测试是在环境温度下进行。单体残基的重量百分比是以聚合物中单体残基的总重量计。聚合物和松香的重量百分比是以干重计。
织品优选是合成织物，即包含至少40重量％，优选至少50重量％，优选至少60重量％，优选至少70重量％，优选至少80重量％，优选至少90重量％合成聚合物的织物。优选合成织物包括包含聚酰胺纤维(例如NYLON)或聚酯纤维(优选聚对苯二甲酸乙二醇酯(PET))的织物。织物优选具有100到500，优选150到400，优选200到350克/平方米(g/m2)的重量。
聚烯烃弹性体是一种聚合物或共聚物，其包含至少一种非极性(即，仅含有碳和氢)的基于烯烃的聚合物。每种至少一种非极性的基于烯烃的聚合物包含至少50重量％烯烃单体的聚合单元和非极性组分(即，含有除碳和氢以外的元素的单体单元)。优选的是，非极性的基于烯烃的聚合物包含丙烯/α-烯烃共聚物，优选丙烯/乙烯共聚物，和以下各者中的至少一个：(i)苯乙烯嵌段共聚物，(ii)均质分支链乙烯/α-烯烃共聚物，(iii)烯烃嵌段共聚物和(iv)无规聚丙烯共聚物。中间泡沫层优选包含丙烯/α-烯烃共聚物和组分(i)-(iv)中的至少两种、三种或全部四种。至少一种非极性的基于烯烃的聚合物可包含单丙烯/α-烯烃共聚物或两种或更多种丙烯/α-烯烃共聚物的掺合物。类似地，(i)苯乙烯类嵌段共聚物，(ii)均质分支链乙烯/α-烯烃共聚物，(iii)烯烃嵌段共聚物和(iv)无规聚丙烯共聚物中的每一种可以纯净形式存在或以两种或更多种共聚物的掺合物形式存在。至少一种非极性的基于烯烃的聚合物还可以包含一或多种任选的添加剂，如加工助剂、延长剂、封闭剂、颜料和/或染料、抗氧化剂、UV稳定剂和/或吸收剂、阻燃剂、填充剂(如滑石、碳酸钙)等。
优选的是，所述至少一种非极性的基于烯烃的聚合物包含至少30，优选至少40，优选至少50重量百分比(wt％)丙烯/α-烯烃共聚物。所述至少一种极性的基于烯烃的聚合物中的丙烯/α-烯烃共聚物的最大量优选不超过90，优选不超过80，优选不超过70重量％。除可归因于起泡过程的气体和副产物以外，中间泡沫层可在成分上与顶部皮肤层相同。
所述至少一种极性的基于烯烃的聚合物中(i)苯乙烯类嵌段共聚物，(ii)均质分支链、直链乙烯/α-烯烃共聚物，(iii)烯烃嵌段共聚物和(iv)无规聚丙烯共聚物的总量优选是至少10，优选至少20，优选至少30重量％。中间泡沫层中(i)苯乙烯类嵌段共聚物，(ii)均质分支链乙烯/α-烯烃共聚物，(iii)烯烃嵌段共聚物和(iv)无规聚丙烯共聚物的最大总量优选不超过70，优选不超过60，优选不超过50重量％。
丙烯/α-烯烃共聚物优选表征为具有实质上等规丙烯序列。“实质上等规丙烯序列”意指通过13C NMR测量，序列具有大于0.85；优选大于0.90；优选大于0.92；优选大于0.93的等规三单元组(mm)。等规三单元组在所属领域中是众所周知的并且在例如美国专利案5,504，172和国际公开案第WO 00/01745号中描述，其是指通过13C NMR光谱测定，就共聚物分子链中的三单元组单元来说的等规序列。
丙烯/α-烯烃共聚物优选具有在0.1到25g/10min范围内的熔体流动速率(MFR)，根据ASTM D-1238(在230℃/2.16Kg下)测量。这一范围包括和披露从0.1到25g/10min的所有个别值和子范围；举例来说，MFR可以从下限0.1g/10min、0.2g/10min或0.5g/10min到上限25g/10min、15g/10min、10g/10min、8g/10min或5g/10min。举例来说，丙烯/α-烯烃共聚物可具有0.1到10g/10min范围内的MFR；或丙烯/α-烯烃共聚物可具有0.2到10g/10min范围内的MFR。在一个优选实施例中，丙烯/α-烯烃是丙烯/乙烯共聚物。
优选的是，丙烯/α-烯烃共聚物具有0.85到0.89g/cc的密度。本文中包括和披露从0.85到0.89g/cc的所有个别值和子范围；举例来说，密度可以从下限0.85、0.86、0.87或0.88g/cc到上限0.855、0.865、0.875、0.885或0.89g/cc。举例来说，密度可以是0.85到0.89g/cc，或在替代方案中，0.85到0.87g/cc，或在替代方案中，0.87到0.89g/cc，或在替代方案中，0.86到0.888g/cc。丙烯/α-烯烃优选是丙烯/乙烯共聚物。
丙烯/α-烯烃共聚物包含来源于丙烯和一或多种α-烯烃共聚单体的单元。用于制造丙烯/α-烯烃共聚物的例示性共聚单体是C2到C10α-烯烃；例如C2、C4、C6和C8α-烯烃。丙烯/α-烯烃共聚物包含1到30重量％一或多种来源于一或多种α-烯烃共聚单体的单元。
丙烯/α-烯烃共聚物具有3.5或更低；或3.0或更低；或1.8到3.0的分子量分布(MWD)，定义为重量平均分子量除以数目平均分子量(Mw/Mn)。在另一实施例中，丙烯/α-烯烃是丙烯/乙烯共聚物。这类丙烯/α-烯烃共聚物进一步描述于美国专利案6,960,635和6,525，157中。这类丙烯/α-烯烃共聚物可以商标名VERSIFYTM从The Dow Chemical Company购得，或以商标名VISTAMAXXTM从ExxonMobil Chemical Company 购得。
优选的是，以上组分(a)中的热塑性聚合物是C2-C8(优选C2-C4)脂肪族α-烯烃的均聚物或共聚物，如乙烯、丙烯、1-丁烯等，或其组合；α-烯烃的官能化(顺丁烯二酸酐和/或羧酸)均聚物或共聚物；C2-C8(优选C2-C4)脂肪族α-烯烃与苯乙烯的共聚物；聚氨基甲酸酯；环氧化物，或其组合。如本文中所使用，术语用酸酐和/或羧酸官能化的基于烯烃的聚合物是指内部或上面接枝有顺丁烯二酸酐和/或羧酸官能团的基于烯烃的聚合物。接枝反应描述于例如美国专利案8,450,430和7,763,692中。或者，官能团可存在于共聚物中(即，羧酸官能团)，其与烯烃单体共聚合以形成基于烯烃的聚合物。尤其优选的热塑性聚合物包括例如苯乙烯-乙烯-丁烯-苯乙烯(SEBS)嵌段共聚物(优选具有不超过35重量％的苯乙烯含量)和经顺丁烯二酸酐改性的乙烯-乙酸乙烯酯(EVA)共聚物。优选的是，热塑性聚合物的Mw是20,000到100,000；优选是至少25,000，优选是至少30,000；优选不超过85,000，优选不超过70,000。
优选的是，热塑性聚合物是苯乙烯乙烯丁烯苯乙烯(SEBS)嵌段共聚物，其具有等于或小于35重量％的苯乙烯含量，并且优选杨氏模数(Young′s modulus)等于或小于10MPa。本文中包括和披露等于或小于10MPa的所有个别值和子范围；举例来说，热塑性弹性体的杨氏模数可以等于或小于10MPa，或在替代方案中，等于或小于9MPa，或在替代方案中，等于或小于8MPa，或在替代方案中，等于或小于6MPa，或在替代方案中，等于或小于4MPa。在一个优选实施例中，热塑性聚合物的杨氏模数不小于0.5MPa。本文中包括和披露等于或小于35重量％的苯乙烯含量的所有个别值和子范围。举例来说，苯乙烯含量可以从上限35重量％，或在替代方案中，30重量％，或在替代方案中，25重量％开始。优选的是，聚苯乙烯饱和聚丁二烯-聚苯乙烯和聚苯乙烯饱和聚异戊二烯-聚苯乙烯嵌段共聚物包含具有5,000到35,000的数目平均分子量的聚苯乙烯末端嵌段和具有20，000到170，000的数目平均分子量的饱和聚丁二烯或饱和聚异戊二烯中间嵌段。饱和聚丁二烯嵌段优选具有35-55％1，2-构形并且饱和聚异戊二烯嵌段优选具有大于85％1，4-构形。如果共聚物具有直链结构，那么苯乙烯类嵌段共聚物的总数目平均分子量优选是30,000到250,000。这类嵌段共聚物优选具有10重量％到30％，优选10重量％到20重量％的平均聚苯乙烯含量。
优选热塑性聚合物的水性分散液含有分散剂。在一个优选实施例中，分散剂是C18-C32脂肪族羧酸，优选是C18-C28脂肪族羧酸，优选是C20-C26脂肪族羧酸。在本发明的一个优选实施例中，分散剂是烯烃-丙烯酸共聚物，优选是具有10重量％到30重量％、优选15重量％到25重量％丙烯酸的烯烃-丙烯酸共聚物。在本发明的优选实施例中，也可以使用其它材料作为分散剂，如部分水解的聚乙烯醇、苯乙烯顺丁烯二酸酐共聚物、顺丁烯二酸酐改性的聚乙烯、聚丙烯，或聚烯烃共聚物、顺丁烯二酸酐改性的苯乙烯-二烯嵌段共聚物，或其混合物。任选地，常规阳离子性、离子性或非离子性表面活性剂可与上述聚合分散剂组合使用。优选的是，热塑性聚合物的水性分散液包含30到70重量％热塑性聚合物(以水性分散液的总重量计)，优选40到60重量％，优选45到55重量％。当分散剂是C18-C32脂肪族羧酸时，以热塑性聚合物的重量计，其优选以2到10重量％，优选2到8重量％，优选3到7重量％的量存在。当分散剂是烯烃-丙烯酸共聚物时，以热塑性聚合物的重量计，其优选以15到35重量％，优选20到30重量％，优选22到28重量％的量存在。优选的是，水性分散液实质上不含有机溶剂，即以总分散液重量计，其含有小于3重量％，优选小于2重量％，优选小于1重量％，优选小于0.5重量％，优选小于0.2重量％，优选小于0.1重量％有机溶剂。优选的是，可以所述界限存在于水性分散液(由热塑性聚合物的制备)或组合物中的溶剂是烃基溶剂，优选是芳香族溶剂，优选是甲苯。
优选的是，热塑性共聚物和松香的组合水性分散液包含至少20重量％，优选至少30重量％，优选至少35重量％，优选至少40重量％；优选不超过80重量％，优选不超过70重量％，优选不超过65重量％，优选不超过60重量％热塑性聚合物，百分比是以干燥热塑性聚合物和松香的总重量计。优选的是，热塑性共聚物和松香的水性分散液包含至少20重量％，优选至少30重量％，优选至少35重量％，优选至少40重量％；优选不超过80重量％，优选不超过70重量％，优选不超过65重量％，优选不超过60重量％松香，百分比是以干燥热塑性聚合物和松香的总重量计。
优选的是，水性松香分散液包含松香酯树脂、非氢化脂肪族C5树脂、氢化脂肪族C5树脂、芳香族改性的C5树脂、萜类树脂、氢化C9树脂或其组合，其中“C5”和“C9”是指所用起始物质中碳原子的数量。优选的是，松香具有25到180℃，优选65到160℃，优选90到140℃的软化点。优选的是，松香的密度是0.92g/cc到1.06g/cc且熔融粘度在175℃下小于1000帕斯卡秒(Pa·s)。优选的是，松香重均分子量(Mw)是300到2，000。优选的是，松香实质上不含有机溶剂，如上文关于热塑性聚合物所定义。
优选的是，热塑性共聚物和松香的水性分散液(统称为“粘合剂”)在室温下混合在一起，优选使用常规混合设备。在室温下在织物衬底上涂布粘合剂。织物上粘合剂的涂层厚度优选是2到30微米，优选是4到15微米，优选是5到10微米。优选的是，干燥经涂布的织物以移除水，优选在烘箱中在低于150℃，优选低于140℃，优选低于130℃，优选低于120℃；优选至少100℃，优选至少110℃的温度下。经涂布的干燥织物与聚烯烃弹性体层合，优选在80到180℃，优选100到160℃，优选115到155℃的温度下。优选的是，在层合期间的压缩力是2到50kN，优选4到25kN，优选8到20kN。
实例
·涂布程序
1)在印刷纸上通过胶带固定织物(尺寸是约20×19cm)。
2)将来自步骤1的样品固定到涂布机上。选择线杆。固定杆并且留下胶布的空间以固定胶。
3)在具有覆盖胶带的区域上添加足够的粘合剂。
4)启动发动机并且快速施用胶粘剂。
5)释放线杆并且将其快速清洁。取出样品并且将其放入罩盖中约5分钟并且接着移至热烘箱中在80-120℃下保持2分钟。
6)取出样品并且放入罩盖中并且使其冷却到室温。
7)测试涂层重量(15-20gsm)并且收集样品。
·层合程序
1)应在层合之前制备POE薄片。
2)将热压机设定在所需温度(例如120℃)、压力(例如500kg)下。将PET衬垫放在压机的底部平台上。在设定温度下关闭平台。
3)将POE薄片(15x15cm)放在织物的经底涂的侧面的顶部上。在层合物的一个开始部分中，在薄片与织物之间插入纸条以便在层合之后易于释放。
4)打开压机并且将POE//织物放到板上。用铝箔覆盖POE薄片以防止POE粘住平台。快速关闭压机。
5)开始计时并且在设定时间(30-60s)打开压机。
6)取出样品并且使其在室温下冷却，同时使箔侧面向下对着实验台表面。
7)移除箔并且收集样品。
A)原料
·织物：在本研究中使用的织物是典型市售黑色PET织物。
·POE薄片：POE薄片由Dow产品XUS57551(0.87g/cc，3.35MFR)制成，其是INFUSETM与VERSIFYTM的掺合物。
·水性分散液1-1：分散液的基底树脂是FUSABOND C250，一种经顺丁烯二酸酐(MAH)改性的乙烯-乙酸乙烯酯(EVA)共聚物，并且分散液的表面活性剂封装是DMEA中和的乙烯-丙烯酸(EAA)共聚物。分散液1-1的平均粒度是约550nm，固体含量是50.0重量％并且粘度是约380cp。
·水性分散液1-2：分散液的基底树脂是KRATON G1643，一种苯乙烯乙烯丁烯苯乙烯(SEBS)嵌段共聚物，其苯乙烯含量是16.6-20.6％，并且分散液的表面活性剂封装是DMEA中和的乙烯-丙烯酸(EAA)共聚物。分散液1-2的平均粒度是约960nm，固体含量是50.0重量％并且粘度是约295cp。
·水性分散液2：使用水性松香分散液作为增粘剂分散液，并且分散液的表面活性剂封装是DMEA中和的乙烯-丙烯酸(EAA)共聚物。分散液2的平均粒度是约550nm，固体含量是50.0重量％并且粘度是约580cp。
注意：所有上文提及的水性分散液是使用Dow的机械分散液技术生产。
B)粘合剂制备和应用
1)粘合剂配制
上述FUSABOND C250分散液(水性分散液1-1)或SEBS(水性分散液1-2)和松香分散液(水性分散液2)在搅拌下，在设计的质量比下冷掺合。在涂布和层合试验之前，关于平均粒度测试掺合物的稳定性，并且测试目的是确保不存在相分离问题。
2)涂层和层合
根据上述过程，用所制备的粘合剂涂布织物，接着将经涂布的织物置放于烘箱中在120℃下保持3分钟，以用于水分蒸发和薄膜形成目的。接着使用压缩模制器在115℃下将经涂布的织物与POE薄片层合在一起，其中压力是4kN。
3)剥离强度测试(ASTM D751-06，ASTM D2724-03)
将层合的POE到PET织物样品切割成3cm×15cm矩形样品并且使用Instron通过180度剥离测试来测量剥离强度，其中十字头速度是300mm/min。记录平均负载(kgf)并且计算平均剥离强度(Kgf/3cm)。
C)实例说明
松香分散液是以商标名ROSIN GLYCEROL ESTER 202出售的水性松香酯胶。
实例1
水性FUSABOND C250/松香分散液(固体质量比，50/50)掺合物；其中固体含量是45.0重量％。
实例2
水性KRATON G1643/松香分散液(固体质量比，50/50)掺合物；其中固体含量是45.0重量％。
比较实例1
水性FUSABOND C250分散液，其中固体含量是45.0重量％。
比较实例2
水性KRATON G1643分散液，其中固体含量是45.0重量％。
比较实例3
水性松香分散液，其中固体含量是45.0重量％。
D)结果和论述
表1展示通过使用不同粘合剂制备的层合样品的粘合强度。也呈现空白样品(POE薄片与织物直接层合，两者之间无任何粘合剂)。
表1
样品 平均剥离强度(Kgf/3cm)
实例1 2.49
实例2 2.71
比较实例1 0.84
比较实例2 0.82
比较实例3 0.12
空白 0.48
观察结果：
·从表1观察到，实例展示超过2.0Kgf/3cm的剥离强度，其可符合剥离强度要求，但比较实例不符合效能要求。
·相信SEBS或EVA-g-MAH分散液和松香分散液的掺合物在涂布过程期间对织物结构具有良好渗透，并且在干燥过程之后充当热熔融粘合剂。松香可以是基底树脂的有效增粘剂，并且出人意料的协同作用增强粘附作用。
结论：
本发明的实例(SEBS或EVA-g-MAH分散液和松香分散液的掺合物)提供效能与成本(包括环境效益)的良好平衡。

Claims (3)

1.一种用于使织物粘合到聚烯烃弹性体的方法；所述方法包含对织物施用：(a)40到80重量％热塑性聚合物的水性分散液；和(b)60到20重量％松香的水性分散液，其中百分比是以热塑性聚合物和松香的总干重计,其中所述热塑性聚合物是经顺丁烯二酸酐改性的乙烯-乙酸乙烯酯共聚物,其中所述织物包含至少50重量％聚酰胺或聚酯纤维。
2.根据权利要求1所述的方法，其中所述松香是松香酯树脂、非氢化脂肪族C5树脂、氢化脂肪族C5树脂、芳香族改性的C5树脂、萜类树脂、氢化C9树脂或其组合。
3.根据权利要求2所述的方法，其中所述聚烯烃弹性体包含至少50重量％烯烃单体的聚合单元。
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