CN110229477A - 一种石墨烯原位接枝聚酯薄膜及其制备方法 - Google Patents
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Abstract
本发明公开一种石墨烯原位接枝聚酯薄膜及其制备方法:以羟基化石墨烯、氨基化石墨烯为改性剂,与对苯二甲酸、乙二醇缩合共聚得到改性PET原料,并按100:(0.5‑2.5):(1‑3):(0.5‑1.5)的质量比与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,熔融挤出、流延铸片、拉伸成型;缩合反应体系包括以下质量百分比原料:羟基化石墨烯6‑10%、氨基化石墨烯4‑6%、对苯二甲酸42‑52%、乙二醇36‑38%、硅烷偶联剂0.5‑1%、稳定剂0.5‑1.5%、复合催化剂1‑1.5%。本发明利用具有特殊官能团结构的石墨烯与对苯二甲酸单体、乙二醇单体发生化学交联共聚反应,将石墨烯引入聚酯分子链中,进而使石墨烯在聚酯体系中长期保持稳定相容状态,使聚酯薄膜具有永久性抗静电能力。
Description
技术领域
本发明属于聚酯薄膜加工技术领域,具体涉及一种石墨烯原位接枝聚酯薄膜及其制备方法。
背景技术
聚酯薄膜简称PET薄膜,是以聚对苯二甲酸乙二醇酯为原料,采用挤出法制成厚片,再经双向拉伸制成的薄膜材料。聚酯薄膜一般为无色透明、有光泽的薄膜,机械性能优良,刚性、硬度及韧性高,耐穿刺,耐摩擦,耐高温和低温,耐化学药品性、耐油性、气密性和保香性良好,是常用的阻透性复合薄膜基材之一。
聚酯薄膜因其分子特性决定了其电绝缘性,表面电阻达到1014-1016Ω,因此,聚酯薄膜在加工、生产过程中易造成静电荷积累的问题,不仅影响正常使用,还因静电作用吸附环境中粉尘、灰粒或油脂,影响其表面光洁度。现有技术,主要通过采用物理掺杂的方式将以炭黑、碳纤维、碳纳米管、石墨、金属微粒等为主要成分的无机抗静电剂填充在聚酯树脂中制造抗静电PET薄膜,无机填料和有机高分子材料之间相容性较差,易出现界面分层现象或无机粒子沉积析出现象,影响聚酯薄膜抗静电性,随着时间的增长,复合体系的稳定性越差,抗静电性不断衰减。如申请号为CN201210185667.4的专利,公开一种抗静电母粒及其制备方法,通过直接将纳米石墨、碳纳米纤维按1:1质量比或纳米石墨、纳米ATO粉、碳纳米管按1:1:1质量比组成抗静电剂物理添加到聚酯树脂中的方式改善抗静电性能;如申请号为CN201711042210.7的专利,公开一种抗静电母粒及使用该抗静电母粒的聚酯薄膜,通过物理添加氧化石墨烯增强聚酯薄膜导电性。
基于以上所述,本发明利用具有特殊官能团结构的石墨烯与对苯二甲酸单体、乙二醇单体发生化学交联共聚反应,将石墨烯引入聚酯分子链中,形成稳定性高的石墨烯原位接枝聚酯的共聚物,进而使石墨烯在聚酯体系中长期稳定相容,与具有π-共轭结构的聚苯撑乙烯协同提高薄膜导电性,使聚酯薄膜具有永久性抗静电能力;进一步,本发明还利用荷叶疏水剂、全氟辛基三乙氧基硅烷协同提高复合薄膜的疏水疏油及耐污性能。
发明内容
针对现有技术的不足之处,本发明的目的在于提供一种石墨烯原位接枝聚酯薄膜及其制备方法。
本发明的技术方案概述如下:
一种石墨烯原位接枝聚酯薄膜:以羟基化石墨烯、氨基化石墨烯为改性剂,与对苯二甲酸、乙二醇缩合共聚得到改性PET原料,并按100:(0.5-2.5):(1-3):(0.5-1.5)的质量比与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,熔融挤出、流延铸片、拉伸成型;
缩合反应体系包括以下质量百分比原料:羟基化石墨烯6-10%、氨基化石墨烯4-6%、对苯二甲酸42-52%、乙二醇36-38%、硅烷偶联剂0.5-1%、稳定剂0.5-1.5%、复合催化剂1-1.5%。
优选的是,所述稳定剂为亚磷酸三苯酯。
优选的是,所述复合催化剂由甲醇锑、氯化亚砜按1:(0.2-0.8)的质量比组成。
一种石墨烯原位接枝聚酯薄膜的制备方法,包括以下步骤:
S1:合成改性PET原料:将羟基化石墨烯、氨基化石墨烯分散于乙二醇中,滴加硅烷偶联剂,搅拌30min,再加入对苯二甲酸、稳定剂、复合催化剂,在温度为260-280℃,真空度为100-300Pa的反应条件下,缩合共聚6-12h;
S2:120-150℃将S1制出的改性PET原料干燥3h,与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,在270-285℃熔融挤出后,15-25℃流延在冷鼓上铸片,再于110-120℃进行双向拉伸,控制纵向拉伸比为4-5倍,横向拉伸比为2-3倍。
本发明的有益效果:
本发明利用具有羟基和氨基官能团结构的石墨烯与对苯二甲酸单体、乙二醇单体发生化学交联共聚反应,将石墨烯引入聚酯分子链中,形成稳定性高的石墨烯原位接枝聚酯的共聚物,进而使石墨烯在聚酯体系中长期保持稳定相容状态,与具有π-共轭结构的聚苯撑乙烯协同提高薄膜导电性,使聚酯薄膜具有永久性抗静电能力;进一步地,本发明还利用荷叶疏水剂、全氟辛基三乙氧基硅烷协同提高复合薄膜的疏水疏油及耐污性能。
附图说明
图1为石墨烯原位接枝聚酯薄膜制备方法工艺流程图。
具体实施方式
下面结合实施例对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。
实施例1制备石墨烯原位接枝聚酯薄膜
S1:合成改性PET原料:按质量百分比将6%羟基化石墨烯、4%氨基化石墨烯分散于36%乙二醇中,滴加0.5%硅烷偶联剂,搅拌30min,再加入52%对苯二甲酸、0.5%亚磷酸三苯酯、1%复合催化剂,复合催化剂由甲醇锑、氯化亚砜按1:0.5的质量比组成,在温度为260℃,真空度为150Pa的反应条件下,缩合共聚6h;
S2:120℃将S1制出的改性PET原料干燥3h,按100:1:1:1的质量比与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,在270℃熔融挤出后,15℃流延在冷鼓上铸片,再于110℃进行双向拉伸,控制纵向拉伸比为4倍,横向拉伸比为2倍。
实施例2制备石墨烯原位接枝聚酯薄膜
S1:合成改性PET原料:按质量百分比将8%羟基化石墨烯、5%氨基化石墨烯分散于37%乙二醇中,滴加0.8%硅烷偶联剂,搅拌30min,再加入47%对苯二甲酸、1%亚磷酸三苯酯、1.2%复合催化剂,复合催化剂由甲醇锑、氯化亚砜按1:0.6的质量比组成,在温度为270℃,真空度为200Pa的反应条件下,缩合共聚8h;
S2:130℃将S1制出的改性PET原料干燥3h,按100:2:2:1的质量比与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,在280℃熔融挤出后,20℃流延在冷鼓上铸片,再于110℃进行双向拉伸,控制纵向拉伸比为4倍,横向拉伸比为2倍。
实施例3制备石墨烯原位接枝聚酯薄膜
S1:合成改性PET原料:按质量百分比将10%羟基化石墨烯、6%氨基化石墨烯分散于38%乙二醇中,滴加1%硅烷偶联剂,搅拌30min,再加入42%对苯二甲酸、1.5%亚磷酸三苯酯、1.5%复合催化剂,复合催化剂由甲醇锑、氯化亚砜按1:0.8的质量比组成,在温度为280℃,真空度为200Pa的反应条件下,缩合共聚12h;
S2:140℃将S1制出的改性PET原料干燥3h,按100:2.5:3:1.5的质量比与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,在285℃熔融挤出后,25℃流延在冷鼓上铸片,再于120℃进行双向拉伸,控制纵向拉伸比为5倍,横向拉伸比为3倍。
对实施例1-3制出的改性聚酯薄膜进行性能检测,试验结构如下表所示:
由上表数据可知,本发明显著降低了聚酯薄膜表面电阻,进而大幅度改善其抗静电性能,且其膜表面与水的接触角≥131°,水滴在膜表面的滚动角≤7°,具有荷叶疏水效应,提高聚酯薄膜疏水疏油性能,进而改善其光洁度与自洁性能。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。
Claims (4)
1.一种石墨烯原位接枝聚酯薄膜,其特征在于:以羟基化石墨烯、氨基化石墨烯为改性剂,与对苯二甲酸、乙二醇缩合共聚得到改性PET原料,并按100:(0.5-2.5):(1-3):(0.5-1.5)的质量比与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,熔融挤出、流延铸片、拉伸成型;
缩合反应体系包括以下质量百分比原料:羟基化石墨烯6-10%、氨基化石墨烯4-6%、对苯二甲酸42-52%、乙二醇36-38%、硅烷偶联剂0.5-1%、稳定剂0.5-1.5%、复合催化剂1-1.5%。
2.根据权利要求1所述一种石墨烯原位接枝聚酯薄膜,其特征在于,所述稳定剂为亚磷酸三苯酯。
3.根据权利要求1所述一种石墨烯原位接枝聚酯薄膜,其特征在于,所述复合催化剂由甲醇锑、氯化亚砜按1:(0.2-0.8)的质量比组成。
4.一种石墨烯原位接枝聚酯薄膜的制备方法,其特征在于,包括以下步骤:
S1:合成改性PET原料:将羟基化石墨烯、氨基化石墨烯分散于乙二醇中,滴加硅烷偶联剂,搅拌30min,再加入对苯二甲酸、稳定剂、复合催化剂,在温度为260-280℃,真空度为100-300Pa的反应条件下,缩合共聚6-12h;
S2:120-150℃将S1制出的改性PET原料干燥3h,与聚苯撑乙烯、荷叶疏水剂、全氟辛基三乙氧基硅烷共混后,在270-285℃熔融挤出后,15-25℃流延在冷鼓上铸片,再于110-120℃进行双向拉伸,控制纵向拉伸比为4-5倍,横向拉伸比为2-3倍。
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CN115322347A (zh) * | 2022-07-07 | 2022-11-11 | 广东轻工职业技术学院 | 一种pet聚酯中石墨烯的分散方法 |
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