CN106170507A - 抗静电涂覆的聚酯膜 - Google Patents

抗静电涂覆的聚酯膜 Download PDF

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Publication number
CN106170507A
CN106170507A CN201580007630.4A CN201580007630A CN106170507A CN 106170507 A CN106170507 A CN 106170507A CN 201580007630 A CN201580007630 A CN 201580007630A CN 106170507 A CN106170507 A CN 106170507A
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China
Prior art keywords
film
antistatic
ion
polymer
coating
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CN201580007630.4A
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English (en)
Inventor
D·S·斯特里克兰
J·N·鲁滨逊
J·H·西蒙兹
C·小查普尔
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DuPont Teijin Films US LP
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DuPont Teijin Films US LP
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Publication of CN106170507A publication Critical patent/CN106170507A/zh
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    • C09D7/63—Additives non-macromolecular organic
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Abstract

一种抗静电聚酯膜包含自支撑聚酯基材膜，在其至少一个表面上带有一抗静电层，其包括a)一种或多种包含根据式(I)的重复单元的抗静电聚合物，其中R1和R2各自独立地为H或CH3，R3为具有2‑10范围碳数的烯基，R4和R5各自独立地为具有1‑5范围碳数的饱和烃基，R6为具有2‑5范围碳数的烯基，n为0‑40范围的整数，m为1‑40范围的整数，和Y‑为卤离子、硝酸根离子、硫酸根离子、烷基硫酸根离子、磺酸根离子、烷基磺酸根离子或磷酸二氢根离子；b)一种或多种非聚合阳离子抗静电剂；和c)一种或多种交联剂。

Description

抗静电涂覆的聚酯膜
相关申请的交叉引用
本申请主张2014年2月7日提交的美国临时申请No.61/937,154的权益，其内容通过引用以其整体并入本文用于所有目的。
发明背景
当在辊和片材中处理时，聚酯膜产生静电荷。对于可以更有效地驱散电荷并且相对于抗静电涂层的性能更加稳定的水性在线涂层存在需求，即当膜被卷起和/或处理时显示出抗静电组分向该膜的表面更小的发展和/或抗静电组分向其它表面的传输显示较低趋势的涂层。
发明概述
本发明提供一种抗静电聚酯膜，其包括自支撑聚酯基材膜，在其至少一个表面上带有一抗静电层，其包括：
a)一种或多种包含根据式(I)的重复单元的抗静电聚合物
其中R1和R2各自独立地为H或CH3，R3为具有2-10范围碳数的烯基，R4和R5各自独立地为具有1-5范围碳数的饱和烃基，R6为具有2-5范围碳数的烯基，n为0-40范围的整数，m为1-40范围的整数，以及Y-为卤离子、硝酸根离子、硫酸根离子、烷基硫酸根离子、磺酸根离子、烷基磺酸根离子或磷酸二氢根离子；
b)一种或多种非聚合阳离子抗静电剂；和
c)一种或多种交联剂。
具体实施方式
本发明提供抗静电聚酯膜，其是如下形成的：使用包含聚季铵丙烯酰胺抗静电聚合物、交联剂和非聚合抗静电剂的水性涂层组合物涂覆聚酯基材，接着将所述涂层干燥以在基材上形成抗静电层。根据本发明的膜提供与普通可商购的膜相比在许多方面优异的抗静电性能，且所述抗静电性能显著地耐受归因于处理的降解，显示出优异的抗静电性能并且耐擦掉。以下详细描述包括使用抗静电组合物涂覆的自支撑聚酯膜基材的膜。
聚季铵丙烯酰胺抗静电聚合物
所述涂层组合物包括一种或多种包含根据式(I)的重复单元的聚季铵丙烯酰胺抗静电聚合物
其中R1和R2各自独立地为H或CH3，R3为具有2-10范围碳数的烯基，R4和R5各自独立地为具有1-5范围碳数的饱和烃基，R6为具有2-5范围碳数的烯基，n为0-40范围的整数，m为1-40范围的整数，以及Y-为卤离子、硝酸根离子、硫酸根离子、烷基硫酸根离子、磺酸根离子、烷基磺酸根离子或磷酸二氢根离子。在一些实施方案中，R1和R2各自为H，R3为(CH2)3，n为零，R4和R5各自为CH3，以及m为1。在一些实施方案中，Y-为CH3SO3 -。
根据式(I)的重复单元占聚合物中的重复单元的至少50mol％，或至少75mol％，或至少90mol％，或至少95mol％，或至少98mol％或100mol％。在聚合物中其它重复单元可以包括-CHR1-CR2(COOCH3)-、-CHR1-CR2(COOC2H5)-和/或-CHR1-CR2(CONH2)-，其中R1和R2如上所定义，和/或乙烯单元。
并入根据式(I)单元的聚合物可以如在美国专利No.6,103,368中所描述地获得，其通过引用并入本文。任选使用乙烯作为共聚单体、通过乳液聚合来聚合丙烯酸酯以获得具有2,000至100,000重均分子量的聚丙烯酸酯。在一个实施例中，通过与N，N-二烷基氨基烷基胺(例如N，N-二甲基氨基丙基胺或N，N-二乙基氨基丙基胺)反应酰胺化所述聚合物，并且酰胺化聚合物上的N，N-二烷基氨基基团经历季铵羟烷基化。聚合物的数均分子量通常为至少3,000，或至少5,000，和通常最多300,000或最多100,000。
基于干燥固体(不包括表面活性剂或任何滑动颗粒)，一种或多种具有根据式(I)的重复单元的聚合物总共占所述涂层组合物的至少5wt％，或至少10wt％，或至少20wt％。它们占所述涂层组合物最多40wt％，或最多50wt％，或最多60wt％。
交联剂
所述涂层组合物包括一种或多种交联剂。这些可以是有机聚合交联剂，例如带有多个碳二亚胺、异氰酸酯、氮杂环丙烷或噁唑啉基的聚合物。实例包括噁唑啉官能化的丙烯酸聚合物，例如包含根据式(II)重复单元的交联剂，
其中R7和R8各自独立地为H或CH3。在一些实施方案中，R7和R8各自为H。其它合适的交联剂包括蜜胺-甲醛、苯并胍胺-甲醛、甘脲-甲醛、脲-甲醛和环氧树脂、以及硅烷和钛酸酯。通常合适的交联剂在水中是可溶的。
基于干燥固体(不包括表面活性剂或任何滑动颗粒)，一种或多种交联剂总共占所述涂层组合物的至少0.5wt％，或至少1.5wt％，或至少3wt％。它们占所述涂层组合物最多10wt％，或最多25wt％，或最多40wt％。
非聚合抗静电剂
所述涂层组合物包括一种或多种非聚合阳离子抗静电剂，通常为季铵盐，最通常每个分子仅具有单一的季铵部分，或仅具有两个季铵部分。合适的实例包括硬脂酰胺丙基二甲基-2-羟乙基铵盐，例如硝酸盐或磷酸二氢盐。
基于干燥固体(不包括表面活性剂或任何滑动颗粒)，一种或多种非聚合阳离子抗静电剂总共占所述涂层组合物的至少30wt％，或至少45wt％，或至少60wt％。它们占所述涂层组合物最多75wt％，或最多80wt％，或最多85wt％。
表面活性剂
一种或多种表面活性剂通常以足够提供基材润湿的量包括。如果存在，基于干燥固体，表面活性剂总共将通常占涂层组合物的至少0.1wt％，或至少1wt％，或至少2wt％。它们将通常占涂层组合物最多10wt％，或最多20wt％或最多60wt％。在一些实施方案中，仅使用非离子表面活性剂，或仅使用阳离子表面活性剂，或使用其组合。示例性非离子表面活性剂包括A60聚氧乙烯二苯乙烯化的苯基醚，获自Kao SpecialtiesAmericas，LLC，High Point，NC的非离子表面活性剂。其它合适的表面活性剂包括DowChemical的Tergitol NP-10，Univar Ltd.的NP10异壬基苯乙氧基化物和AirProducts的104表面活性剂。
所述涂层组合物是水性组合物，并且通常不含有机溶剂。在本发明的一些实施方案中，希望某些其它成分排除出涂层组合物。例如，可能有必要排除有机硅烷，或排除存在含有缩水甘油基团的单体和/或聚合物。有时所有颗粒材料可以被排除，虽然在某些情况下二氧化硅颗粒、交联的聚(甲基丙烯酸甲酯)颗粒，和/或带正电荷的颗粒可以例外。有时可以排除阴离子抗静电剂。
在本发明的一些实施方案中，所述涂层组合物可以包括由一种或多种水性溶液或乳液聚合物，例如丙烯酸聚合物组成的粘合剂。取决于应用需要，加入粘合剂树脂可以赋予某些所需的性能。例如包括丙烯酸类可以使得抗静电层可印刷。然而，在本发明的一些实施方案中，某些聚合物最好排除出所使用的涂层组合物以制备抗静电层。这些可以包括以下的任意或全部：聚酯、聚氨酯、环氧树脂、乙烯基树脂、聚醚树脂，和中性(即，非阴离子，非阳离子和非两性)聚合物，其包含取代的或未取代的丙烯酸酯单体和/或取代的或未取代的丙烯酰胺单体的单元。在一些实施方案中，在涂层组合物中不存在任何不同于阳离子抗静电聚合物和交联剂的类型的聚合物。在一些实施方案中，不同于并入根据式(I)重复单元的那些的阳离子抗静电聚合物也可被排除。在一些实施方案中，不同于交联剂的非抗静电聚合物可以排除，乳液聚合物或其它非水溶性聚合物也可以被排除。通常，阴离子聚合物和/或阴离子表面活性剂被排除出所述涂层组合物。
聚酯基材
所述聚酯基材包括由一种或多种甘醇或二醇(例如乙二醇或丙二醇或丁二醇)与一种或多种二酸或其酯(通常为甲基酯)的缩聚制备的结晶聚酯。合适的二酸包括对苯二甲酸、萘二甲酸、间苯二甲酸、联苯甲酸和癸二酸。可用于本发明的示例性聚酯膜包括聚对苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚对苯二甲酸丙二酯和聚对苯二甲酸丁二酯，或这些的混合物，或其中存在以上提及的聚酯的任一项的共聚酯膜。例如，根据本发明可以使用聚对苯二甲酸乙二酯/间苯二甲酸乙二酯(PETIP)共聚酯膜。另一个合适的实例是PET和PEN的共聚酯制成的膜。通常将使用PET。
在典型的聚酯膜制造中，将聚酯树脂熔融并且作为无定型片挤出至抛光的旋转流延鼓上以形成聚合物的流延片材。此后，将聚合物的流延片材加热至刚好高于其玻璃化转变温度，对于聚对苯二甲酸乙二酯为80℃至100℃，并且通常在一个或多个方向进行拉伸或牵拉。通常，在两个方向拉伸：挤出方向(纵向方向)，和垂直于挤出方向(横向方向)以制备双轴取向膜。第一拉伸(其赋予膜强度和韧性)，通常以约2.0至约4.5的因数增加膜的原始长度。随后的拉伸步骤各自还增加约2.0至约4.5倍的膜尺寸。一般地，优选首先在纵向方向拉伸并且随后在横向方向拉伸。所述膜随后加热定型，对于聚对苯二甲酸乙二酯通常在约190℃至240℃范围的温度，以锁定强度、韧性和其它物理性能，并且随后在缠绕在辊上之前冷却。
涂覆聚酯基材
根据本发明使用的涂层组合物为挥发性稀释剂的溶液形式，其可以包括溶剂。在一些实施方案中，所述组合物的所有组分溶解在挥发性稀释剂中，并且因此所述组合物是溶液。然而，在一些实施方案中，所述组合物可以含有一些分散的物质，例如丙烯酸乳液。在大多数情况下，稀释剂将是水性的，如在本文中所使用的其是指稀释剂为至少50wt％的水。在大多数实施方案中，水性稀释剂为至少90wt％的水，以及在许多情况下，其将是100wt％的水。这种溶液将通常具有约0.5wt％至15wt％的范围和更通常约2至5wt％的干燥固体用于单向拉伸之后的在线凹版辊应用，但对于其它应用方法其可以更高。如本文所使用的，“干燥固体”是指涂层组合物中存在的非挥发物质的量，即在干燥之后涂层中保留的物质，即使一些非挥发物质在室温下可能是液体。所有的抗静电化合物和表面活性剂对于计算干燥固体的目的被视为是非挥发的。
对于凹版式涂覆法，涂层组合物的粘度将通常在1-100mPas的范围，但对于其它涂覆方法可以大得多。
可以使用任何常规涂覆方法，例如喷涂、辊涂、缝涂、弯液面涂、浸渍涂布、绕线棒涂、气刀涂、幕涂、刮刀涂、直接和反向凹版涂法等以施加涂层组合物。所述涂层通常作为具有约0.5至30微米范围厚度的连续湿涂层施加，更通常约1.5-6微米的范围，如通过湿式红外线计测量。在干燥之后，所述涂层通常具有约100至范围的厚度，通常约和更通常为约的范围。
在本发明其它的实施方案中，使用本领域已知的各种类的涂覆方法，可以使用常规离线涂覆工艺。然而，相对于离线工艺(其中涂覆步骤在聚酯基材的制造已经完成之后进行)，能够使用在线涂覆给予经济性和效率性的优点，因为离线工艺可能涉及有机溶剂和/或要求用户采用不方便并且高成本的干燥步骤。相反地，制造商的在线涂覆为消费者提供了现成的膜，从而为消费者节省了展开未涂覆的膜、涂覆并且随后再次卷起所必须提供的时间和设备。
如果使用在线工艺，通常在最终牵拉膜之前施加涂层组合物。对于单轴拉伸膜，涂层组合物优选在牵拉之后施加。对于双轴或单轴取向膜，涂层组合物通常在中间牵拉阶段期间施加，即在膜已经被拉伸之后但在第二次拉伸之前。
在一些实施方案中，与抗静电层相反的聚酯基材的表面可以使用包含颗粒材料的“滑动涂料”涂覆以帮助处理膜，例如以改善可缠绕性和最小化或阻止“阻塞”。这种涂料例如可以在膜取向之前或之后和在最终缠绕之前在线施加。合适的滑动涂料可以包含硅酸钾，例如美国专利Nos.5,925,428和5,882,798所公开的，其公开内容通过引用并入本文。或者，滑动涂料可以包含丙烯酸和/或甲基丙烯酸聚合物树脂的不连续层，任选进一步包含交联剂，如例如EP-A-0408197所公开的。在一些实施方案中，颗粒可以加入到抗静电涂层以提供滑动。示例性滑动颗粒包括二氧化硅和交联聚(甲基丙烯酸甲酯)珠。提供滑动的填料颗粒也可以分散在聚酯基材膜中或包括在共挤出于其上的层中。
实施例
术语表
A60-聚氧乙烯二苯乙烯化的苯基醚，获自Kao SpecialtiesAmericas，LLC，High Point，NC的非离子表面活性剂，本文作为20％的水溶液使用。
477E-牛脂基二胺五甲基二氯(“季铵化合物，N，N，N，N′，N′-五甲基-N′-牛脂基烷基三亚甲基二-，氯化物”)，乙醇中56wt％(如测量的)，可获自EvonikGoldschmidt Corporation，Hopewell，VA。
SN-硬脂酰胺丙基二甲基-2-羟乙基硝酸铵，50∶50异丙醇-水混合物中50％的溶液，可获自Cytec Industries Inc.，West Paterson，NJ。以下显示结构。
SP-硬脂酰胺丙基二甲基-2-羟乙基磷酸二氢铵，50∶50异丙醇-水混合物中35％的溶液，可获自Cytec Industries Inc。
EPOCROSTM WS-300-噁唑啉官能化水溶性丙烯酸共聚物的10wt％水溶液，可获自Nippon Shokubai Co.，LTD，大阪，日本。
聚合物A-具有以下所示结构的阳离子均聚物的35wt％水溶液。
丙烯酸类粘合剂-组成为甲基丙烯酸甲酯/丙烯酸乙酯/丙烯腈/N-羟甲基丙烯酰胺的丙烯酸类共聚物的45％固体乳液。
测试步骤
静电衰减测试
设备：Monroe静电分析仪，型号276A
步骤：完全电压设置在2000V。所选择的测试顺序为10秒充电，60秒暗衰减。记录峰值电压，静电荷衰减至峰值电压二分之一的时间，静电荷衰减至峰值电压十分之一的时间和静电荷衰减至＜5V(完全衰减)的时间。
表面电阻率测试
设备：电子静电计(Keithley型号617)，电阻率适配器/环状电极(Keithley型号6105)和Blue M型号WP-4800潮湿箱(具有手套口以进入)。
步骤：
电压源设置为100.0V和在2mAMAX下操作。
将尺寸大约为31/2″x31/2″的膜样品在潮湿箱中调整(conditioned)至少20分钟。在电阻率适配器关闭和闭锁之后30秒读数。
计算：
表面电阻率(log ohms/sq)＝log(5340/微安[由电子显示])+安培指数(指数为：毫安＝3，微安＝6，纳安＝9，微微安＝12)
实施例1
涂层组合物1和2如在表1中所示制备，并且通过拉伸期间凹版涂覆(即在双轴取向的两个阶段之间涂覆)而涂覆在具有AB共挤出结构的聚酯膜的“A”层上。“A”层为二氧化硅填充(粗糙表面)的PET层，和“B”层为纯净的未填充的PET。各个涂层随后被稀释，保持在总溶液中表面活性剂水平相同，以制备具有较小干燥厚度的涂层。由未稀释和稀释的组合物制成的涂层(分别指定为A和B)的性能，以及两个其它抗静电涂层(3和4，在以下实施例2中制备)和五个可商购抗静电涂覆的PET膜的结果示于表3。
表1
实施例2
涂层组合物3和4如在表2中所示制备并且类似地拉伸期间涂覆到含有玻璃珠碾碎的13X沸石颗粒的单一层PET膜上。再次，各个涂层被稀释，保持在总溶液中表面活性剂水平相同，以制备具有较小干燥厚度的涂层。涂层的性能示于表3。
表2
表3
认为商业膜包括以下抗静电剂：
膜1 聚(3，4-乙撑二氧噻吩)
膜2 硬脂酰胺丙基二甲基2-硝酸羟乙基铵
膜3 磷酸钾
膜4 未知
膜5 三氟甲烷磺酸锂
由于抗静电涂层通常具有湿润的性能，通常存在抗静电剂容易由表面移除的趋势。因此，表面电阻率(SR)和静电放电(SD)测试在不同的相对湿度(RH)条件在用棉布擦拭膜10次之前和之后获得，以模拟消费者处理膜。结果示于表3，其中较低的数字表示更好的性能。
可以看出，本发明的抗静电涂层在50％RH(8.9-10.0log ohm/sq)和在35％RH(9.7-10.9log ohm/sq)均提供了优异的表面电阻率。35％RH的数字是更重要的，因为静电在较干燥的条件下更是一个问题。商购膜展示了一定范围的表面电阻率，变化超过一个数量级，并且在50％和35％RH下仅膜#4表现得与本发明涂层相当。
然而，商购膜#4在静电荷衰减速度方面比本发明的膜显著更差，所述静电荷衰减相比表面电阻率测量是更加指示性的使用性能。在22-24％RH下静电放电测量对于本发明的涂层显示了优异的性能，膜充电至仅140-530V并且随后快速衰减。电荷衰减至原始值的10％经过的运行时间为大约2秒或对于最好的涂层更少。
在电荷衰减方面，商购膜的性能显著地变化。最佳充电至240-440V，但只有一个例外，衰减时间相比本发明的膜显著更长。仅商购膜#5提供了良好的电荷衰减：2.4秒衰减至原始值的10％，但其表面电阻率高于本发明的膜。
在擦拭之后，本发明的表面电阻率增加小于1个数量级。静电荷衰减至10％的时间增加很少，由无增加至大约3X。例外，涂层3B具有小于最佳范围的涂层厚度。虽然一些商购膜(#1和#4)在擦拭之后对于静电放电性能损失具有抗性，但它们相比使用本发明涂层的最佳膜显示了较差的绝对性能。
本发明膜1A具有最佳的整体性能，其具有低表面电阻率、接受电荷的低倾向，2秒衰减至原始值10％的时间，和在擦拭之后性能的略微降低。其它本发明的膜也整体表现近似，并且相比商购膜显著整体更好。
实施例3
表面活性剂的水平不显著影响涂层的静电耗散性能。表4显示了涂层，样品5，相比先前的实施例具有较低的表面活性剂水平。其涂覆在实施例2所描述的膜上。在50％RH下SR值为9.6和在35％RH下SR值为10.4。电荷衰减测试中最大电压为408V和衰减时间为1/2衰减1.79秒，1/10衰减2.78秒和完全衰减4.90秒。
表4
实施例4
随着干燥涂层厚度的增加，可以将丙烯类和其它乳液并入到涂层中以维持抗静电性能。表5显示了两个涂层配方，其拉伸期间使用Meyer棒施加在未填充的PET上以致计算的干燥涂层厚度为如在表6中所见，抗静电性能非常好。
表5
表6
使用样品6和7实现了良好的抗静电性能，其二者均含有添加的丙烯酸类乳液。
虽然本发明通过参考具体的实施方案在此阐明和描述，但本发明不旨在限制为所示的细节。相反，在权利要求的等同物的范围内不脱离本发明的情况下可以在细节上做出多种改变。

Claims (13)

1.一种抗静电聚酯膜，其包含自支撑聚酯基材膜，在其至少一个表面上带有一抗静电层，该抗静电层包括
a)一种或多种包含根据式(I)的重复单元的抗静电聚合物
其中R1和R2各自独立地为H或CH3，R3为具有2-10范围碳数的烯基，R4和R5各自独立地为具有1-5范围碳数的饱和烃基，R6为具有2-5范围碳数的烯基，n为0-40范围的整数，m为1-40范围的整数，以及Y-为卤离子、硝酸根离子、硫酸根离子、烷基硫酸根离子、磺酸根离子、烷基磺酸根离子或磷酸二氢根离子；
b)一种或多种非聚合阳离子抗静电剂；和
c)一种或多种交联剂。
2.如权利要求1的所述膜，其中所述抗静电层进一步包含一种或多种非离子和/或阳离子表面活性剂。
3.如权利要求1或2所述的膜，其中所述一种或多种交联剂包括带有多个噁唑啉基团的聚合物。
4.如任何前述权利要求所述的膜，其中所述一种或多种交联剂包括包含根据式(II)重复单元的聚合物
其中R7和R8各自独立地为H或CH3。
5.如任何前述权利要求所述的膜，其中所述抗静电层不包含乳液聚合物。
6.如任何前述权利要求所述的膜，其中所述抗静电层不包含不同于聚合交联剂的非抗静电聚合物。
7.如权利要求1-6任一项所述的膜，其中所述一种或多种非聚合阳离子抗静电剂包含硬脂酰胺丙基二甲基-2-羟乙基磷酸二氢铵。
8.如权利要求1-6任一项所述的膜，其中所述一种或多种非聚合阳离子抗静电剂包含硬脂酰胺丙基二甲基-2-羟乙基硝酸铵。
9.如权利要求1-6任一项所述的膜，其中所述一种或多种非聚合阳离子抗静电剂包含牛脂基二胺五甲基二氯。
10.如任何前述权利要求所述的膜，其中R1和R2各自为H，R3为(CH2)3，n为零，R4和R5各自为CH3，以及m为1。
11.如任何前述权利要求的膜，其中Y-为CH3SO3 -。
12.如权利要求4-11的任一项所述的膜，其中R7和R8各自为H。
13.如任何前述权利要求所述的膜，其中所述抗静电层进一步包含滑动颗粒。
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