CN110253984A - 一种静电纺纳米纤维膜-织物复合涂层材料及制备方法 - Google Patents

一种静电纺纳米纤维膜-织物复合涂层材料及制备方法 Download PDF

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CN110253984A
CN110253984A CN201910533122.XA CN201910533122A CN110253984A CN 110253984 A CN110253984 A CN 110253984A CN 201910533122 A CN201910533122 A CN 201910533122A CN 110253984 A CN110253984 A CN 110253984A
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fabric
electrostatic spinning
coating material
fiber film
composite coating
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CN110253984B (zh
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王迎
杨云
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Dalian Polytechnic University
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    • A61F13/00—Bandages or dressings; Absorbent pads
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Abstract

本发明公开了一种静电纺纳米纤维膜‑织物复合涂层材料及制备方法。复合涂层材料由三层结构组成。表层是PVP过硫酸盐自由基聚合得到的交联PVPP；中间层为聚偏氟乙烯‑六氟丙烯(PVDF‑HFP)/聚乙烯吡咯烷酮(PVP)无针静电纺纳米纤维膜；底层为织物。表层为功能层，中间层和底层在PVP交联过程中通过PVP自交联及与PVDF‑HFP的互交联复合在一起，共同组成复合涂层材料的支撑层。本发明制备的复合材料可用于功能性医用敷料，还可用于啤酒稳定剂，具备多酚物质吸附及过滤双层功能。

Description

一种静电纺纳米纤维膜-织物复合涂层材料及制备方法
技术领域
本发明属于复合材料制备领域，具体涉及一种加工一种静电纺/织物二元复合材料的制备方法。可应用于纳米材料分析技术和膜材料应用技术领域。
背景技术
随着纺织行业的不断发展以及人们对纺织品综合性能要求的不断提升，多功能复合织物无疑将在织物发展中占据一席之地。其中，近些年来国内外普遍关注的静电纺丝纳米纤维在纺织中的应用也在不断增多，特别是将纳米纤维与传统织物相结合应用于特种产业用材料的报道屡见不鲜。
PVPP由乙烯吡咯烷酮单体在特定条件下交联聚合而成，是一种性质优良的高分子精细化工产品，也是近年兴起的一种新型药用辅料。PVPP主要用作片剂的崩解剂，现已准许用作食品填加剂，作为啤酒、果汁等酿造行业的稳定剂、澄清剂等。
PVPP在国内外啤酒领域广泛运用，作为啤酒胶体稳定剂。过滤后无论多么清凉的啤酒仍含有溶解的分类化合物和蛋白质，这些多酚物质与蛋白质在有氧的条件下形成不可逆的永久聚合物，是造成啤酒混沌的主要原因。PVPP可以有效的除去啤酒中多酚物质，提高啤酒的澄清度，延长啤酒的货架寿命。
目前，啤酒生产中，需要把硅藻土和PVPP混合后定量加入到啤酒中，过滤后PVPP和硅藻土以形成滤饼，作为废物处理。该工艺不需要单独的PVPP过滤设备，但生产成本较高。
发明内容
为了解决以上PVPP作为啤酒稳定剂中的高效使用问题，本发明打破常规PVPP在啤酒稳定剂中以粉末状中间体吸附并以滤饼的形式过滤去除的使用方法，制备一种以静电纺纳米纤维膜-织物过滤材料为支持层，PVPP涂层为功能层的复合材料。
一种静电纺纳米纤维膜-织物复合涂层材料，由表层、中间层、底层组成三层结构，所述表层为交联的聚乙烯吡咯烷酮，为由PVP过硫酸盐自由基聚合得到的交联PVPP涂层，中间层为聚偏氟乙烯-六氟丙烯(PVDF-HFP)/聚乙烯吡咯烷酮(PVP)静电纺纳米纤维膜，优选为无针静电纺得到的聚偏氟乙烯-六氟丙烯(PVDF-HFP)/聚乙烯吡咯烷酮(PVP)无针静电纺纳米纤维膜，底层为织物，所述织物为机织物或无纺布。
作为优选的技术方案，所述聚偏氟乙烯-六氟丙烯/聚乙烯吡咯烷酮静电纺纳米纤维膜的厚度为0.054-0.114mm；所述织物为涤纶、丙纶或锦纶的机织物或无纺布。
本发明还提供一种静电纺纳米纤维膜-织物复合涂层材料的制备方法，包括如下步骤：
(1)将聚偏氟乙烯-六氟丙烯(PVDF-HFP)溶液与聚乙烯吡咯烷酮(PVP)溶液按体积比为(9:1-7:3)混合，得到复合纺丝溶液，再通过静电纺丝方法制备聚偏氟乙烯-六氟丙烯(PVDF-HFP)/聚乙烯吡咯烷酮(PVP)静电纺纳米纤维膜；
所述聚偏氟乙烯-六氟丙烯(PVDF-HFP)溶液的浓度为14-20wt％，所述聚乙烯吡咯烷酮溶液的浓度为6-8wt％；
(2)将步骤(1)得到聚偏氟乙烯-六氟丙烯(PVDF-HFP)/聚乙烯吡咯烷酮(PVP)静电纺纳米纤维膜、织物平行放置，且互相贴合，浸入到含聚乙烯吡咯烷酮(PVP)、引发剂、水的引发体系中，发生聚合(交联)反应，交联结束后，干燥，得到纳米纤维膜-织物复合涂层材料；
所述引发体系中的引发剂为过硫酸铵，聚乙烯吡咯烷酮(PVP)的浓度为5-10wt％，过硫酸铵的浓度为0.5-1wt％，反应的温度为90-95℃，反应的时间为6-8h。
作为优选的技术方案，步骤(1)中所述聚偏氟乙烯-六氟丙烯(PVDF-HFP)溶液和聚乙烯吡咯烷酮(PVP)溶液的溶剂为N-N-二甲基乙酰胺(DMAC)；作为优选的技术方案，步骤(1)中所述静电纺丝方法为无针静电纺丝。
作为优选的技术方案，步骤(1)中所述无针静电纺丝条件为：电压60-80kV，溶液盒速度80-150mm/s，纺丝时间40-120min。
作为优选的技术方案，步骤(1)中所述聚偏氟乙烯-六氟丙烯(PVDF-HFP)/聚乙烯吡咯烷酮(PVP)静电纺纳米纤维膜的厚度为0.054-0.114mm。
作为优选的技术方案，步骤(2)中所述干燥的条件为：40-60℃，干燥2-4h。
作为优选的技术方案，步骤(2)中所述织物为涤纶、丙纶或锦纶的机织物或无纺布。
本发明还提供上文所述的纳米纤维膜-织物复合涂层材料在药物载体、功能性医用敷料、啤酒多酚吸附中的应用。由于具备多酚物质吸附及过滤双层功能，可用于啤酒稳定剂。
作为优选的技术方案，当所述静电纺纳米纤维膜-织物复合涂层材料在啤酒多酚吸附中应用时，所述织物为丙纶的机织物或无纺布。
本发明所述静电纺纳米纤维膜-织物复合涂层材料的表层为功能层，中间层和底层在PVP交联过程中通过PVP自交联及与PVDF-HFP的互交联复合在一起，共同组成复合涂层材料的支撑层。复合涂层材料的表面涂层、纳米纤维互交联的PVPP及织物中纤维表面吸附的PVPP增加了PVPP与吸附材料的接触面积，起到稳定剂的作用，有效的除去啤酒中多酚物质，又起到了对复合涂层材料加固连接的作用。中间层与底层二元织物的复合形成了二级过滤条件。纳米纤维膜中间层为纳米级过滤，织物层为微米级过滤。该复合涂层材料兼具多酚物质吸附及过滤双层功能，缩短了工艺流程，节约了成本。
本发明具有的有益效果是：
1、复合涂层材料由三层组成，表面为PVPP涂层，中间为PVDF-HFP/PVP纳米纤维膜，底层为织物。在过硫酸盐存在的条件下，PVDF-HFP也会产生相应的自由基，发生PVP与PFDF-HFP的互交联反应，形成稳定的结构。利用PVP的自交联及与PVDF-HFP的互交联反应，可以使PVPP将涂层与纳米纤维层、纳米纤维层与织物牢牢连接在一起，提升了材料界面强度，解决了膜易剥离的问题。
2、在啤酒多酚吸附中，复合材料表面涂层及纤维表面固着的PVPP提升了材料的接触面积，起到稳定剂的作用，有效的除去啤酒中多酚物质。中间层与底层二元织物的复合形成了二级过滤条件。纳米纤维层为纳米级过滤，织物层为微米级过滤。该复合材料具备过滤及多酚物质吸附的功能，缩短了工艺流程，节约成本。
3、由于PVPP回收使用过程中需要碱液清洗，啤酒多酚吸附中选用丙纶织物。丙纶织物、PVDF-HFP纳米纤维膜的耐酸碱性好、耐水性好。该复合材料可在酸性、碱性条件下工作，工作寿命较长。
4、PVPP由于其具有生理安全性、吸收液体的能力、能携带并释放药物、水不溶性、络合性等特性，本发明制备的复合材料还可制成柔软又有一定强度的胶带，作为理想的药物载体或外伤包扎敷料。功能层提供载药及吸收液体的能力、中间纳米层耐酸碱，疏水性好，提供产品透气能力、底层为支持层，提供强力和柔软性。
附图说明
图1为实施例1中7:3PVDF-HFP/PVP纳米复合膜的SEM图；
图2为实施例2中9:1PVDF-HFP/PVP纳米复合膜的SEM图；
图3为实施例2中纳米纤维膜-织物复合涂层材料SEM图，其中(a)为正面涂层，(b)为反面织物，(c)为纳米纤维膜与织物界面。
具体实施方式
下述非限定性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。
本发明实施例选用以下材料和设备：
扫描电镜(SEM)：超高分辨热场发射扫描电镜JSM-780DF，日本电子JEDL；
无针静电纺设备：纳米蜘蛛丝静电纺丝机，捷克ELMARCO公司；
强力测试设备：LLY-06E型电子单纤维强力仪，莱州市电子仪器有限公司。测试样品制作过程：剪裁长5cm，宽0.6cm的试样。在温度为20℃，湿度为65％条件下测试；
厚度测试设备：YG141LA型数字式织物厚度仪，莱州市电子仪器有限公司。
实施例1
将PVDF-HFP溶解于DMAC中，得到20wt％的PVDF-HFP溶液。将PVP溶解于DMAC中，得到6wt％的PVP溶液。再将PVDF-HFP溶液与PVP溶液以体积比为7:3混合，制备PVDF-HFP/PVP复合纺丝液。将PVDF-HFP/PVP复合纺丝液在电压80kV，溶液盒速度80mm/s，纺丝时间40min条件下进行无针静电纺丝，得到PVDF-HFP/PVP纳米复合膜。PVDF-HFP/PVP纳米复合膜的断裂强度为4.6202MPa，纳米纤维平均直径为113nm，厚度为0.054mm,SEM如图1所示。将PVDF-HFP/PVP纳米复合膜与涤纶机织物(涤纶：涤纶长丝300DX5，纬纱：涤纶长丝，300DX4；经密：307根/10cm，纬密：122根/10cm，2/2斜纹)，上下平行放置，且相互贴合，四周边缘用模具夹紧后浸入引发体系中引发聚合(交联)反应，引发体系中过硫酸铵的浓度0.5wt％，PVP的浓度5wt％，反应的温度90℃，反应的时间6h，反应结束之后在40℃干燥4h，得到纳米纤维膜-织物复合涂层材料。
实施例2
将PVDF-HFP溶解于DMAC中得到20wt％的PVDF-HFP溶液。将6wt％的PVP溶解于DMAC中，得到PVP溶液。再将PVDF-HFP溶液与PVP溶液以体积比为9:1混合，制备PVDF-HFP/PVP复合纺丝液。PVDF-HFP/PVP复合纺丝液在电压80kV，溶液盒速度80mm/s，纺丝时间40min条件下进行无针静电纺丝，得到PVDF-HFP/PVP纳米复合膜。PVDF-HFP/PVP纳米复合膜的断裂强度为9.1565MPa，纳米纤维平均直径为156nm，厚度为0.114mm，SEM如图2所示。将PVDF-HFP/PVP纳米复合膜与涤纶机织物(经纱：涤纶长丝300DX5，纬纱：涤纶长丝，300DX4；经密：307根/10cm，纬密：122根/10cm，2/2斜纹)，上下平行放置，且相互贴合，四周边缘用模具夹紧后浸入引发体系中引发聚合(交联)反应，引发体系中过硫酸铵的浓度1wt％，PVP的浓度10wt％，反应的温度95℃，反应的时间8h，反应结束之后在40℃干燥4h，得到纳米纤维膜-织物复合涂层材料，其SEM如图3所示，其中(a)为正面涂层，(b)为反面织物，(c)为纳米纤维膜与织物界面。

Claims (10)

1.一种静电纺纳米纤维膜-织物复合涂层材料，其特征在于，由表层、中间层、底层组成三层结构，所述表层为交联的聚乙烯吡咯烷酮，所述中间层为聚偏氟乙烯-六氟丙烯/聚乙烯吡咯烷酮静电纺纳米纤维膜，所述底层为织物，所述织物为机织物或无纺布。
2.根据权利要求1所述的纳米纤维膜-织物复合涂层材料，其特征在于，所述聚偏氟乙烯-六氟丙烯/聚乙烯吡咯烷酮静电纺纳米纤维膜的厚度为0.054-0.114mm；所述织物为涤纶、丙纶或锦纶的机织物或无纺布。
3.一种静电纺纳米纤维膜-织物复合涂层材料的制备方法，其特征在于，包括如下步骤：
(1)将聚偏氟乙烯-六氟丙烯溶液与聚乙烯吡咯烷酮溶液按体积比为9:1-7:3混合，得到复合纺丝溶液，再通过静电纺丝方法制备聚偏氟乙烯-六氟丙烯/聚乙烯吡咯烷酮静电纺纳米纤维膜；
所述聚偏氟乙烯-六氟丙烯溶液的浓度为14-20wt％，所述聚乙烯吡咯烷酮溶液的浓度为6-8wt％；
(2)将步骤(1)制备的聚偏氟乙烯-六氟丙烯/聚乙烯吡咯烷酮静电纺纳米纤维膜、织物平行放置，且互相贴合，浸入到引发体系中，聚合反应后，干燥，得到静电纺纳米纤维膜-织物复合涂层材料；
所述织物为机织物或无纺布；
所述引发体系为含聚乙烯吡咯烷酮、引发剂、水的引发体系，引发剂为过硫酸铵，聚乙烯吡咯烷酮的浓度为5-10wt％，过硫酸铵的浓度为0.5-1wt％，反应的温度为90-95℃，反应的时间为6-8h。
4.根据权利要求3所述的方法，其特征在于，步骤(1)中所述静电纺丝方法为无针静电纺丝。
5.根据权利要求4所述的方法，其特征在于，步骤(1)中所述无针静电纺丝条件为：电压60-80kV，溶液盒速度80-150mm/s，纺丝时间40-120min。
6.根据权利要求3所述的制备方法，其特征在于，步骤(2)中所述织物为涤纶、丙纶或锦纶的机织物或无纺布。
7.根据权利要求3所述的方法，其特征在于，步骤(2)中所述的干燥的条件为：40-60℃干燥2-4h。
8.根据权利要求3所述的方法，其特征在于，步骤(1)中所述聚偏氟乙烯-六氟丙烯溶液和聚乙烯吡咯烷酮溶液的溶剂为N-N-二甲基乙酰胺。
9.权利要求1-2中任意一项所述的静电纺纳米纤维膜-织物复合涂层材料或权利要求2-8中任意一项所述方法得到的静电纺纳米纤维膜-织物复合涂层材料在药物载体、医用敷料、啤酒多酚吸附中的应用。
10.根据权利要求9所述的应用，当所述静电纺纳米纤维膜-织物复合涂层材料在啤酒多酚吸附中应用时，所述织物为丙纶的机织物或无纺布。
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