CN113478936B - 一种抗静电双向拉伸聚酯薄膜及其制备方法 - Google Patents

一种抗静电双向拉伸聚酯薄膜及其制备方法 Download PDF

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CN113478936B
CN113478936B CN202110790248.2A CN202110790248A CN113478936B CN 113478936 B CN113478936 B CN 113478936B CN 202110790248 A CN202110790248 A CN 202110790248A CN 113478936 B CN113478936 B CN 113478936B
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黄剑
王红兵
陈铸红
张涛
张少伟
年陈瑞
丁道俊
王恒煜
张鸿翔
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Anhui Guofeng New Material Co ltd
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Abstract

本发明公开了一种抗静电双向拉伸聚酯薄膜，由上表层、芯层和下表层构成，所述上表层、下表层由下述质量百分比的原料制成：抗静电PET切片20‑30％、抗粘母料70‑80％，所述芯层由下述质量百分比的原料制成：PET切片94‑98％、乙烯基离聚物成核剂2‑6％；所述抗静电PET切片是以PET树脂和聚甲基丙烯酸为原料，经过混合、熔融挤出制得。本发明还公开了抗静电双向拉伸聚酯薄膜的制备方法。本发明制备的抗静电聚酯薄膜不仅具有优良的抗静电性，而且具有较高的力学性能、光学性能和热稳定性。

Description

一种抗静电双向拉伸聚酯薄膜及其制备方法
技术领域
本发明涉及高分子材料技术领域，尤其涉及一种抗静电双向拉伸聚酯薄膜及其制备方法。
背景技术
热转印打印是用热和压力将油墨从碳带介质转印到纸或薄膜的过程，当标签通过打印机的打印头和压轴时，将油墨转印到标签上。静电的产生和释放一直是热转印中的一个重要问题，首先，在热转印碳带制备中，静电量大会引起油墨涂布不均匀等不良现象；其次，在热转印打印中，静电会影响到打印质量，静电吸附的微小颗粒会对打印质量产生负面的影响，造成转印字符不清晰，白点等现象。
一些已应用的技术可以很有效地减少静电，如背涂、共聚、共混等方式。背涂法是在双向拉伸聚酯(BOPET)薄膜表面通过涂覆抗静电背涂层来达到抗静电效果，这种方式可以做到106Ω·m，但是在运输和使用过程中常常会因为薄膜磨损或者形变而丢失抗静电性。
共聚法通常是在共聚过程中加入聚乙二醇(PEG)，形成PET-PEG共聚物，这种方式要求PEG的分子量要超过2000以上，添加比例也要达到20％以上才会有较为明显的抗静电效果，而且，由于聚醚链段的引入，共聚酯分子会变得非常柔顺且不易结晶，所以这种方法目前也只是处于研究阶段，很难进行中试放大。
共混是目前使用最多的一种方式。共混通常是在聚酯中混入金属粉末或聚醚及其衍生物类的高分子抗静电剂等，这种方式能得到不错的抗静电效果，但由于两者相容性差，抗静电的效果尤其是耐久性不甚理想，且由于聚醚的热稳定性差，共混改性过程中的降解问题较为突出，因而应用受到很大限制。同时，随着共混含量的增加，BOPET薄膜的透明性度和力学性能下降严重，对薄膜的印刷效果和耐用性产生明显的不良影响。因此，如何在不降低物理和光学性能的情况下提升BOPET薄膜的抗静电性能，仍是目前亟待解决的问题难点。
发明内容
基于背景技术存在的技术问题，本发明提出了一种抗静电双向拉伸聚酯薄膜及其制备方法。
本发明提出的一种抗静电双向拉伸聚酯薄膜，由上表层、芯层和下表层构成，所述上表层、下表层由下述质量百分比的原料制成：抗静电PET切片20-30％、抗粘母料70-80％，所述芯层由下述质量百分比的原料制成：PET切片94-98％、乙烯基离聚物成核剂2-6％；
所述抗静电PET切片是以PET树脂和聚甲基丙烯酸为原料，经过混合、熔融挤出制得。由于聚甲基丙烯酸中含有大量的羧基基团，与PET进行高温共混时能发生一定程度的交联反应，形成支化的PET。由于交联反应的发生和高吸水性聚甲基丙烯酸的引入，使得PET在保证强度的条件下，抗静电性也得到极大提升，可以达到108Ω·m-1010Ω·m；而且，由于聚甲基丙烯酸分子链上甲基的位阻作用，使支化的PET分子链之间难以靠拢，改变PET本身规整性，无法规整化排列形成晶体，降低PET分子结晶度，提高透明性。
优选地，所述抗静电PET切片是以96.5-98.5质量份PET树脂和1-3质量份聚甲基丙烯酸为原料，经过混合、熔融挤出制得。
优选地，所述抗静电PET切片是以96.5-98.5质量份PET树脂、1-3质量份聚甲基丙烯酸和0.3-1质量份抗氧剂为原料，经过混合、熔融挤出制得；优选地，所述抗氧剂为β-(3，5-二叔丁基-4-羟基苯基)丙酸十八碳醇酯，N，N’-二-β-萘基-对苯二胺，或N，N’-双-(3-(3，5-二叔丁基-4-羟基苯基)丙酰基)己二胺。其中，加入抗氧剂是为了防止PET在熔融挤出时，在高温条件下发生降解。
优选地，所述抗静电PET切片的制备过程中，熔融挤出的温度为270-285℃。
优选地，所述抗静电PET切片的制备过程中，PET树脂和聚甲基丙烯酸在混合前，在140-160℃下干燥4-6h。
优选地，所述抗粘母料中含有3000-3500ppm的爽滑粒子，余量为PET树脂；优选地，所述爽滑粒子的粒径为0.6-1.4μm；优选地，所述爽滑粒子为二氧化硅。
优选地，所述乙烯基离聚物成核剂为乙烯/甲基丙烯酸锂盐共聚物、乙烯/甲基丙烯酸钠盐共聚物、乙烯/甲基丙烯酸锌盐共聚物中的至少一种。乙烯基离聚物成核剂在熔融共混中可与PET分子链反应而形成带离子端基的产物PET-COO-M+，在结晶过程中起到异相成核的作用。
优选地，所述芯层的厚度为3.0-4.0μm，所述上表层的厚度为0.5-0.6μm，所述下表层的厚度为0.5-0.6μm。
一种所述的抗静电双向拉伸聚酯薄膜的制备方法，包括下述步骤：
S1、将芯层的原料混合后，加热熔融挤出，过滤得到芯层熔体；分别将上表层、下表层的原料混合后，加热熔融，抽真空，挤出过滤得到上表层熔体和下表层熔体；
S2、将芯层熔体、上表层熔体和下表层熔体通过模头共挤出制成厚片，将得到的厚片依次经过纵向拉伸、横向拉伸、热定型，得到抗静电双向拉伸聚酯薄膜。
优选地，S1中，芯层的原料的加热熔融温度为275-285℃，上表层、下表层的原料的加热熔融温度为270-280℃。
优选地，S1中，芯层的原料中，PET切片在混合前，在140-160℃下干燥4-6h。
优选地，S2中，纵向拉伸的预热温度为50-100℃，拉伸温度为103-106℃，拉伸倍数为4.1-4.3倍；横向拉伸的预热温度为99-102℃，拉伸温度为103-110℃，拉伸倍数为3.8-4.1倍；热定型温度为235-240℃。
本发明的有益效果如下：
与现有技术相比，本发明在BOPET薄膜的上表层、下表层以抗静电PET切片为主要原料，该抗静电PET切片是通过在PET中引入吸水性的聚甲基丙烯酸制成，可以提升薄膜抗静电性，达到108Ω·m，同时亲水性基团的引入也大幅提高抗静电稳定性，耐久性优异，并且，本发明通过交联反应形成的支化PET，由于聚甲基丙烯酸分子链上甲基的位阻作用，使支化的PET分子链之间难以靠拢，改变PET本身规整性，无法规整化排列形成晶体，降低PET分子结晶度，有利于提高薄膜的透明性；本发明还在芯层中添加了乙烯/甲基丙烯酸金属盐离聚物，可以进一步改善结晶性能，提高薄膜的光学性能，同时由于离聚物与支化PET中都存在聚甲基丙烯酸链段，可以提升薄膜层间界面体系的稳定性和结合力，从而改善薄膜的力学性能，使得制备的抗静电聚酯薄膜不仅具有优良的抗静电性，还具有较高的力学性能、光学性能和热稳定性。
具体实施方式
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种抗静电双向拉伸聚酯薄膜，由上表层、芯层和下表层构成，上表层、下表层由下述质量百分比的原料制成：抗静电PET切片30％、抗粘母料70％，芯层由下述质量百分比的原料制成：膜级PET切片98％、乙烯/甲基丙烯酸钠共聚物2％；
其中，抗静电PET切片是将98.5质量份PET树脂和1质量份聚甲基丙烯酸分别在140-160℃下干燥4-6h后，与0.5质量份抗氧剂混合均匀，用双螺杆挤出机熔融挤出制得，熔融挤出的温度为270-285℃；
抗粘母料中含有3300ppm的粒径为1.2μm的二氧化硅，余量为PET树脂；
乙烯/甲基丙烯酸钠共聚物为杜邦公司的Surlyn 8920，其中乙烯-甲基丙烯酸重量比为90/10，金属盐中和度为45％。
其中，芯层的厚度为3.5μm，所述上表层的厚度为0.55μm，所述下表层的厚度为0.55μm。
制备抗静电双向拉伸聚酯薄膜：
S1、称取芯层的原料，将膜级PET切片在140-160℃下干燥4-6h，然后与乙烯/甲基丙烯酸钠共聚物混合，在275-285℃下加热熔融挤出，过滤得到芯层熔体；分别将上表层、下表层的原料混合后，在270-280℃下加热熔融，抽真空，挤出过滤得到上表层熔体和下表层熔体；
S2、将芯层熔体、上表层熔体和下表层熔体通过模头共挤出制成厚片，将得到的厚片依次经过纵向拉伸、横向拉伸、热定型，得到抗静电双向拉伸聚酯薄膜，其中纵向拉伸的预热温度为50-100℃，拉伸温度为103-106℃，拉伸倍数为4.1-4.3倍；横向拉伸的预热温度为99-102℃，拉伸温度为103-110℃，拉伸倍数为3.8-4.1倍；热定型温度为235-240℃。
实施例2
一种抗静电双向拉伸聚酯薄膜，由上表层、芯层和下表层构成，上表层、下表层由下述质量百分比的原料制成：抗静电PET切片25％、抗粘母料75％，芯层由下述质量百分比的原料制成：膜级PET切片96％、乙烯/甲基丙烯酸钠共聚物4％；
其中，抗静电PET切片是将98质量份PET树脂和3质量份聚甲基丙烯酸分别在140-160℃下干燥4-6h后，与1质量份抗氧剂混合均匀，用双螺杆挤出机熔融挤出制得，熔融挤出的温度为270-285℃；
抗粘母料中含有3000ppm的粒径为1.4μm的二氧化硅，余量为PET树脂；
乙烯/甲基丙烯酸钠共聚物中，乙烯-甲基丙烯酸重量比为90/10，金属盐中和度为45％。
其中，芯层的厚度为3.0μm，所述上表层的厚度为0.5μm，所述下表层的厚度为0.5μm。
薄膜的制备方法同实施例1。
实施例3
一种抗静电双向拉伸聚酯薄膜，由上表层、芯层和下表层构成，上表层、下表层由下述质量百分比的原料制成：抗静电PET切片20％、抗粘母料80％，芯层由下述质量百分比的原料制成：膜级PET切片94％、乙烯基离聚物成核剂6％；
其中，抗静电PET切片是将96.5质量份PET树脂和1质量份聚甲基丙烯酸分别在140-160℃下干燥4-6h后，与0.3质量份抗氧剂混合均匀，用双螺杆挤出机熔融挤出制得，熔融挤出的温度为270-285℃；
抗粘母料中含有3000ppm的粒径为0.6μm的二氧化硅，余量为PET树脂；
乙烯/甲基丙烯酸钠共聚物中，乙烯-甲基丙烯酸重量比为90/10，金属盐中和度为45％。
其中，芯层的厚度为4.0μm，所述上表层的厚度为0.6μm，所述下表层的厚度为0.6μm。
薄膜的制备方法同实施例1。
对比例1
对比例1与实施例1的区别仅为：抗静电PET切片的制备方法不同，具体如下：将98.5质量份PET树脂和1质量份聚丙烯酸分别在140-160℃下干燥4-6h后，与0.5质量份抗氧剂混合均匀，用双螺杆挤出机熔融挤出制得，熔融挤出的温度为270-285℃。
对比例2
对比例2与实施例1的区别仅为：芯层的原料不同，具体如下：芯层由下述质量百分比的原料制成：膜级PET切片100％。
对比例3
对比例3与实施例1的区别仅为：芯层的原料不同，具体如下：芯层由下述质量百分比的原料制成：膜级PET切片98％、聚四氟乙烯粉末成核剂2％；
其中，聚四氟乙烯粉末成核剂为杜邦公司MP1000。
试验例
对实施例1-3和对比例1-3制得的双向拉伸聚酯薄膜进行性能测试，测试结果如表1所示：
表1双向拉伸聚酯薄膜性能测试结果
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (10)

1.一种抗静电双向拉伸聚酯薄膜，其特征在于，由上表层、芯层和下表层构成，所述上表层、下表层由下述质量百分比的原料制成：抗静电PET切片20-30%、抗粘母料70-80%，所述芯层由下述质量百分比的原料制成：PET切片94-98%、乙烯基离聚物成核剂2-6%；
所述抗静电PET切片是以96.5-98.5质量份PET树脂、1-3质量份聚甲基丙烯酸和0.3-1质量份抗氧剂为原料，经过混合、熔融挤出制得；
所述乙烯基离聚物成核剂为乙烯/甲基丙烯酸锂盐共聚物、乙烯/甲基丙烯酸钠盐共聚物、乙烯/甲基丙烯酸锌盐共聚物中的至少一种。
2.根据权利要求1所述的抗静电双向拉伸聚酯薄膜，其特征在于，所述抗氧剂为β-(3，5-二叔丁基-4-羟基苯基)丙酸十八碳醇酯，N，N’-二-β-萘基-对苯二胺，或N，N’-双-(3-(3，5-二叔丁基-4-羟基苯基)丙酰基)己二胺。
3.根据权利要求1所述的抗静电双向拉伸聚酯薄膜，其特征在于，所述抗静电PET切片的制备过程中，熔融挤出的温度为270-285℃。
4.根据权利要求1所述的抗静电双向拉伸聚酯薄膜，其特征在于，所述抗粘母料中含有3000-3500ppm的爽滑粒子，余量为PET树脂。
5.根据权利要求4所述的抗静电双向拉伸聚酯薄膜，其特征在于，所述爽滑粒子的粒径为0.6-1.4μm。
6.根据权利要求4所述的抗静电双向拉伸聚酯薄膜，其特征在于，所述爽滑粒子为二氧化硅。
7.根据权利要求1所述的抗静电双向拉伸聚酯薄膜，其特征在于，所述芯层的厚度为3.0-4.0μm，所述上表层的厚度为0.5-0.6μm，所述下表层的厚度为0.5-0.6μm。
8.一种如权利要求1所述的抗静电双向拉伸聚酯薄膜的制备方法，其特征在于，包括下述步骤：
S1、将芯层的原料混合后加热熔融挤出，过滤得到芯层熔体；分别将上表层、下表层的原料混合后，加热熔融，抽真空，挤出过滤得到上表层熔体和下表层熔体；
S2、将芯层熔体、上表层熔体和下表层熔体通过模头共挤出制成厚片，将得到的厚片依次经过纵向拉伸、横向拉伸、热定型，得到抗静电双向拉伸聚酯薄膜。
9.根据权利要求8所述的抗静电双向拉伸聚酯薄膜的制备方法，其特征在于，S1中，芯层的原料的加热熔融温度为275-285℃，上表层、下表层的原料的加热熔融温度为270-280℃。
10.根据权利要求8或9所述的抗静电双向拉伸聚酯薄膜的制备方法，其特征在于，S2中，纵向拉伸的预热温度为50-100℃，拉伸温度为103-106℃，拉伸倍数为4.1-4.3倍；横向拉伸的预热温度为99-102℃，拉伸温度为103-110℃，拉伸倍数为3.8-4.1倍；热定型温度为235-240℃。
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