CN113773618A - 一种改性聚酯母料及疏水隔热双向拉伸聚酯薄膜 - Google Patents
一种改性聚酯母料及疏水隔热双向拉伸聚酯薄膜 Download PDFInfo
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Abstract
本发明公开了一种改性聚酯母料及疏水隔热双向拉伸聚酯薄膜，涉及聚酯薄膜技术领域，所述改性聚酯母料是将聚羟基氟硅油、对苯二甲酸、乙二醇、催化剂、气凝胶混合，进行酯化反应和缩聚反应后得到的；所述疏水隔热双向拉伸聚酯薄膜包括上表层、芯层和下表层；所述上表层和下表层的原料包括：聚酯切片20～40％、上述改性聚酯母料60～80％；所述芯层原料为膜级聚酯切片。本发明在聚酯母料生产过程中加入聚羟基氟硅油进行共聚改性，从而在聚酯链段上引入氟硅原子，降低了聚酯的表面能，提高了聚酯的疏水性。制备的聚酯薄膜具有优异的超疏水性能，添加的疏水二氧化硅气凝胶作为抗粘粒子，在聚酯薄膜表面构筑了微纳米双尺寸的结构，保温隔热。
Description
技术领域
本发明涉及聚酯薄膜技术领域，尤其涉及一种改性聚酯母料及疏水隔热双向拉伸聚酯薄膜。
背景技术
由于未作相应处理的汽车玻璃，其自身热绝缘性较差，在夏天车辆冷却系统能源消耗大大增加，而在冬季保温系统能源消耗增加，造成了环境中不必要的热散失和热输入，因此需要制备出具有良好隔热性能的薄膜使玻璃具有良好隔热性，达到节能效果。
车辆在雨天高速行驶中，落下的雨水和超车时飞溅起来的水花附在挡风玻璃的外面，驾驶员只能看清雨刷扫过的部分，且雨刷也不能及时刷去雨水，很容易造成事故的发生。
疏水表面作为具有特殊浸润性表面的一种，可用来防水、防雾、防雪、防尘等。目前，制备疏水性表面的方法是在具有粗糙结构的表面上涂布低表面能物质，如硅化物、氟化物等，进行表面修饰。但是这种方法工序复杂，费时费力，难以制备出大面积的超疏水薄膜，这些都限制了它们的广泛实际应用。
发明内容
基于背景技术存在的技术问题，本发明提出了一种改性聚酯母料及疏水隔热双向拉伸聚酯薄膜，是在聚酯母料生产过程中加入聚羟基氟硅油进行共聚改性，从而在聚酯链段上引入氟硅原子，降低聚酯表面能，提高聚酯疏水性；将该聚酯用于薄膜生产，所得薄膜具有优异的超疏水性能。
本发明提出的一种改性聚酯母料，是将聚羟基氟硅油、对苯二甲酸、乙二醇、催化剂、气凝胶混合，进行酯化反应和缩聚反应后得到的。
本发明中，是采用直接酯化法聚酯生产工艺，其制备过程包括酯化反应和缩聚反应。
优选地，所述酯化反应的温度为220～240℃、反应压力为0.2～0.4MPa；所述缩聚反应的温度为270～285℃、反应压力为真空度≤100Pa。
优选地，所述对苯二甲酸和乙二醇的摩尔比为1.2～1.7：1；所述聚羟基氟硅油的用量为对苯二甲酸质量的4～10％；所述气凝胶的用量为理论得到的聚酯质量的2000～3500ppm。
优选地，所述聚羟基氟硅油为硅羟基封端的低分子量聚(甲基-3,3,3－三氟丙基硅氧烷)流体。
优选地，所述气凝胶为疏水性二氧化硅气凝胶，其粒径为2～3.5μm。
上述疏水性二氧化硅气凝胶具有多孔非晶结构，孔隙率和比表面积大，导热率低，具有保温隔热效果。
优选地，所述催化剂为锑系催化剂，优选为三氧化二锑、醋酸锑、乙二醇锑中的一种或一种以上；所述催化剂的用量以锑元素计，为对苯二甲酸质量的0.02～0.04％。
本发明还提出了上述改性聚酯母料的制备方法，包括以下步骤：
S1、将气凝胶分散到适量的乙二醇中，得气凝胶分散液；
S2、将对苯二甲酸、剩余的乙二醇、催化剂、气凝胶分散液、聚羟基氟硅油加入到反应釜中，升温进行酯化反应，然后再升温进行缩聚反应。
本发明还提出了一种疏水隔热双向拉伸聚酯薄膜，包括上表层、芯层和下表层；所述上表层和下表层是由以下质量百分比的原料组成的：聚酯切片20～40％、上述改性聚酯母料60～80％；所述芯层原料为膜级聚酯切片。
本发明还提出了上述疏水隔热双向拉伸聚酯薄膜的制备方法，步骤如下：将聚酯切片和改性聚酯母料进行混合，得到混合料，将其作为三层共挤薄膜中的上表层和下表层成分；将膜级聚酯切片作为芯层成分；将上述原料经预结晶、干燥后，采用三层共挤制得膜片，再将膜片进行纵横向双向拉伸、牵引收卷、分切包装，制成疏水隔热双向拉伸聚酯薄膜。
优选地，所述纵横向拉伸温度为90～105℃，纵横向拉伸倍率为3.5～4.2。
与现有技术相比，本发明的有益效果体现在以下几个方面：
1.本发明在聚酯母料生产过程中加入聚羟基氟硅油进行共聚改性，从而在聚酯链段上引入氟硅原子，降低了聚酯的表面能，提高了聚酯的疏水性。
2.本发明制备的聚酯薄膜具有优异的超疏水性能，添加的疏水二氧化硅气凝胶作为抗粘粒子，在聚酯薄膜表面构筑了微纳米双尺寸的结构，同时由于其多孔非晶结构，孔隙率、比表面积大，导热率低，具有保温隔热效果；且将二氧化硅气凝胶先预分散到二元醇原料中制成分散液，以分散液的方式加入并进行酯化反应，能够提高二氧化硅气凝胶在体系中的分散性。
3.本发明制备的聚酯薄膜具有性能优异、制备工艺简单、易于实现工业化生产等优点，可用于薄膜外包装制品的防水防污，也可用于医用薄膜制品防污防菌领域中。
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
一种改性聚酯母料的制备：
S1、将SiO2气凝胶分散到适量乙二醇中，配制质量浓度为12％的气凝胶分散液，其中SiO2气凝胶粒子平均粒径中值d(50)为3.0μm；
S2、将对苯二甲酸、乙二醇、乙二醇锑催化剂、气凝胶分散液、聚羟基氟硅油(硅羟基封端的低分子量聚(甲基-3,3,3－三氟丙基硅氧烷)流体)加入到反应釜中；控制反应体系中n(对苯二甲酸)：n(乙二醇)＝1.2：1，m(聚羟基氟硅油)＝4％m(对苯二甲酸)，m(SiO2气凝胶)为理论得到的聚酯质量的2000ppm，乙二醇锑催化剂用量以锑元素计，为m(对苯二甲酸)的0.02％；将反应体系升温，在220～225℃、0.2MPa下进行酯化反应，待出水量达到要求时，放至常压；然后在270～275℃、真空度≤100Pa下进行缩聚反应。反应完毕充氮气挤出、切粒、干燥，得到改性聚酯母粒。
实施例2
一种改性聚酯母料的制备：
S1、将SiO2气凝胶分散到适量乙二醇中，配制质量浓度为12％的气凝胶分散液，其中SiO2气凝胶粒子平均粒径中值d(50)为3.0μm；
S2、将对苯二甲酸、乙二醇、乙二醇锑催化剂、气凝胶分散液、聚羟基氟硅油(硅羟基封端的低分子量聚(甲基-3,3,3－三氟丙基硅氧烷)流体)加入到反应釜中；控制反应体系中n(对苯二甲酸)：n(乙二醇)＝1.5：1，m(聚羟基氟硅油)＝7％m(对苯二甲酸)，m(SiO2气凝胶)为理论得到的聚酯质量的2800ppm，乙二醇锑催化剂用量以锑元素计，为m(对苯二甲酸)的0.03％；将反应体系升温，在230～235℃、0.3MPa下进行酯化反应，待出水量达到要求时，放至常压；然后在275～280℃、真空度≤100Pa下进行缩聚反应。反应完毕充氮气挤出、切粒、干燥，得到改性聚酯母粒。
实施例3
一种改性聚酯母料的制备：
S1、将SiO2气凝胶分散到适量乙二醇中，配制质量浓度为12％的气凝胶分散液，其中SiO2气凝胶粒子平均粒径中值d(50)为3.0μm；
S2、将对苯二甲酸、乙二醇、乙二醇锑催化剂、气凝胶分散液、聚羟基氟硅油(硅羟基封端的低分子量聚(甲基-3,3,3－三氟丙基硅氧烷)流体)加入到反应釜中；控制反应体系中n(对苯二甲酸)：n(乙二醇)＝1.7：1，m(聚羟基氟硅油)＝10％m(对苯二甲酸)，m(SiO2气凝胶)为理论得到的聚酯质量的3500ppm，乙二醇锑催化剂用量以锑元素计，为m(对苯二甲酸)的0.04％；将反应体系升温，在235～240℃、0.4MPa下进行酯化反应，待出水量达到要求时，放至常压；然后在280～285℃、真空度≤100Pa下进行缩聚反应。反应完毕充氮气挤出、切粒、干燥，得到改性聚酯母粒。
实施例4
一种聚酯薄膜，包括上表层、芯层和下表层；所述芯层的原料为芯层原料为膜级聚酯切片；上表层和下表层的原料均为：聚酯切片20％、实施例1中制备的改性聚酯母料80％。
上述聚酯薄膜的制备如下：将聚酯切片和改性聚酯母料进行混合，得到混合料，将其作为三层共挤薄膜中的上表层和下表层成分；将膜级聚酯切片作为芯层成分；将上述原料经预结晶、干燥后，采用三层共挤制得膜片，再将膜片进行纵横向双向拉伸、牵引收卷、分切包装，制成疏水隔热双向拉伸聚酯薄膜；其中，纵向拉伸温度为100～103℃、纵向拉伸倍率为4.1，横向拉伸温度为103～105℃，纵横向拉伸倍率为4.0。
实施例5
与实施例4相比，区别仅在于改性聚酯母料的添加比例不同；具体如下：上表层和下表层的原料为：聚酯切片30％、实施例1中制备的改性聚酯母料70％。
实施例6
与实施例4相比，区别仅在于改性聚酯母料的添加比例不同；具体如下：上表层和下表层的原料为：聚酯切片40％、实施例1中制备的改性聚酯母料60％。
实施例7
与实施例4相比，区别仅在于改性聚酯母料的选择不同，是采用实施例2中制备的改性聚酯母料。
实施例8
与实施例4相比，区别仅在于改性聚酯母料的选择不同，是采用实施例3中制备的改性聚酯母料。
对比例1
与实施例4相比，区别仅在于：采用未改性的普通聚酯抗粘母料替代改性聚酯母料。
对实施例4-8和对比例1制得的双向拉伸聚酯薄膜进行性能测试，测试结果如下：
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)
1.一种改性聚酯母料，其特征在于，是将聚羟基氟硅油、对苯二甲酸、乙二醇、催化剂、气凝胶混合，进行酯化反应和缩聚反应后得到的。
2.根据权利要求1所述的改性聚酯母料，其特征在于，所述酯化反应的温度为220～240℃、反应压力为0.2～0.4MPa；所述缩聚反应的温度为270～285℃、反应压力为真空度≤100Pa。
3.根据权利要求1或2所述的改性聚酯母料，其特征在于，所述对苯二甲酸和乙二醇的摩尔比为1.2～1.7：1；所述聚羟基氟硅油的用量为对苯二甲酸质量的4～10％；所述气凝胶的用量为理论得到的聚酯质量的2000～3500ppm。
4.根据权利要求1-3任一项所述的改性聚酯母料，其特征在于，所述聚羟基氟硅油为硅羟基封端的低分子量聚(甲基-3,3,3－三氟丙基硅氧烷)流体。
5.根据权利要求1-4任一项所述的改性聚酯母料，其特征在于，所述气凝胶为疏水性二氧化硅气凝胶，其粒径为2～3.5μm。
6.根据权利要求1-5任一项所述的改性聚酯母料，其特征在于，所述催化剂为锑系催化剂，优选为三氧化二锑、醋酸锑、乙二醇锑中的一种或一种以上；所述催化剂的用量以锑元素计，为对苯二甲酸质量的0.02～0.04％。
7.一种如权利要求1-6任一项所述的改性聚酯母料的制备方法，其特征在于，包括以下步骤：
S1、将气凝胶分散到适量的乙二醇中，得气凝胶分散液；
S2、将对苯二甲酸、剩余的乙二醇、催化剂、气凝胶分散液、聚羟基氟硅油加入到反应釜中，升温进行酯化反应，然后再升温进行缩聚反应。
8.一种疏水隔热双向拉伸聚酯薄膜，其特征在于，包括上表层、芯层和下表层；所述上表层和下表层是由以下质量百分比的原料组成的：聚酯切片20～40％、权利要求1-6任一项所述的改性聚酯母料60～80％；所述芯层原料为膜级聚酯切片。
9.根据权利要求8所述的疏水隔热双向拉伸聚酯薄膜的制备方法，其特征在于，步骤如下：将聚酯切片和改性聚酯母料进行混合，得到混合料，将其作为三层共挤薄膜中的上表层和下表层成分；将膜级聚酯切片作为芯层成分；将上述原料经预结晶、干燥后，采用三层共挤制得膜片，再将膜片进行纵横向双向拉伸、牵引收卷、分切包装，制成疏水隔热双向拉伸聚酯薄膜。
10.根据权利要求9所述的疏水隔热双向拉伸聚酯薄膜的制备方法，其特征在于，所述纵横向拉伸温度为90～105℃，纵横向拉伸倍率为3.5～4.2。
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