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CN118814359A - 一种微米/纳米波浪卷曲纤维膜的制备方法 - Google Patents

一种微米/纳米波浪卷曲纤维膜的制备方法 Download PDF

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CN118814359A
CN118814359A CN202410842055.0A CN202410842055A CN118814359A CN 118814359 A CN118814359 A CN 118814359A CN 202410842055 A CN202410842055 A CN 202410842055A CN 118814359 A CN118814359 A CN 118814359A
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鞠敬鸽
于君
张甜甜
韩佳呈
张妍
王永澄
孙颖
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Tiangong University
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Tianjin Polytechnic University
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43825—Composite fibres
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4391—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece characterised by the shape of the fibres
    • D04H1/43918—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece characterised by the shape of the fibres nonlinear fibres, e.g. crimped or coiled fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

本发明涉及一种微米/纳米波浪卷曲纤维膜的制备方法，包括以下两个步骤：(1)纺丝液配置：将非相容高弹性聚合物和低弹性聚合物以一定质量比溶于溶剂中共混制备纺丝液；(2)静电纺丝：以特制粗糙板作为接收基材，一步静电纺丝技术制备纤维体纳米尺度卷曲(纳米波浪)、膜体微米尺度凹凸(微米波浪)的微米/纳米波浪卷曲纤维膜。本发明制得的微米/纳米波浪卷曲纤维膜具有优异力学性能，且卷曲纤维堆叠形成的高孔隙率及膜体凹凸形成的高粗糙度，为高精度、低阻力膜分离等领域有广阔的应用前景；此外，其制备技术可控、简便，为卷曲纤维宏量化生产提供了可能。

Description

一种微米/纳米波浪卷曲纤维膜的制备方法
技术领域
本发明涉及一种微米/纳米波浪卷曲纤维膜的制备方法，属于卷曲微纳纤维制备技术领域。
背景技术
卷曲微纳纤维，又称波浪微纳纤维，是一种在纤维轴向具有螺旋或弯曲结构的微米或纳米尺度的纤维材料，因其独特的结构特征，使得其具有高比表面积大、高孔隙率、优异机械性能等优势，在吸附、催化、传感、过滤和生物医学等领域具有广泛的应用前景。
静电纺丝技术是能够连续生产微纳纤维的有效手段之一，因设备简单、工艺可控等优势，成为近年来学术界和工业界共同的关注热点。但传统静电纺丝技术在强电场和高速滚筒的双重作用下，制备出的微纳纤维多为伸直状态，收集所得膜材料中纤维呈现紧密沉积状态，阻碍了静电纺丝纳米纤维膜在一些特定领域中的推广和应用。
目前，研究学者通过对静电纺丝技术的改进，实现了卷曲纤维的制备：(1)复合原料：通过力学性能差异或导电性能差异的两种或多种高分子材料，分别通过各自的熔体(或溶液)管道，在同轴、并列等纺丝针头处形成复合熔体流(或溶液流)喷出，从而制成卷曲微纳纤维；(2)装置改进：通过在静电纺丝装置底部引入两根不锈钢针头的储液腔，其在纺丝过程中不断旋转，形成螺旋卷曲纳米纤维，或在纺丝区域引入电场干扰装置，纤维丝在飞行过程中随电场的扭曲发生卷曲，得到卷曲纳米纤维；(3)工艺控制：通过在高湿度环境下进行纺丝，通过高湿诱导实现静电纺纤维的原位自卷曲成型。然而，在实际生产过程中，方法(1)需要采用并列或同轴喷头，纺丝过程和卷曲结构的成形难以控制；方法(2)中收集装置只有两根不锈钢针式喷头，不能批量化得到螺旋卷曲纳米纤维，且外加电场的引入同时会影响纺丝过程的稳定性，也不利于大量化的制备；方法(3)中需要在纺丝过程中引入高湿环境，不利于溶剂的挥发，且提高了高静电压击穿的风险，也可能对设备造成损坏。综上所述，现有技术在纤维形貌控制、结构调控和大规模制备方面仍然存在一些挑战，可控、简便的制备技术仍有待研发。
发明内容
本发明提供了一种微米/纳米波浪卷曲纤维膜的制备方法，以特制粗糙板作为接收基材，结合高弹性聚合物独特的回弹性和力学性能共混低弹性聚合物，通过非相容共混聚合物力学性能差异，基于“惯停曲化”效应，一步静电纺丝技术制备出微米/纳米波浪卷曲纤维膜。
一种微米/纳米波浪卷曲纤维膜，其特征在于，包括以下步骤：
(1)纺丝液配置：将非相容高弹性聚合物和低弹性聚合物以质量比为10：1-1：10溶于溶剂中共混，制备质量分数为5-40wt％的纺丝液；
(2)静电纺丝：以特制粗糙板作为接收基材，通过一步静电纺丝技术，在电压5-60kV、接收距离5-100cm的纺丝参数下，制备纤维体纳米尺度卷曲(纳米波浪)、膜体微米尺度凹凸(微米波浪)的微米/纳米波浪卷曲纤维膜；
所述高弹性聚合物为热塑性聚氨酯弹性体、聚烯烃热塑性弹性体的一种或以上，所述低弹性聚合物为聚苯乙烯、芳纶、聚偏二氟乙烯、偏氟乙烯-六氟丙烯共聚物、聚酰亚胺、聚砜、聚对苯二甲酸乙二醇酯的一种或以上；
所述纺丝液中所用溶剂为N,N-二甲基甲酰胺、N，N-二甲基乙酰胺、氯仿、二甲基亚砜、环己烷、异丁醇、二氯甲烷、甲苯、乙酸乙酯的一种或以上；
所述特制粗糙板为导电接收板，其材质可为铝制、铜制等金属材质或不锈钢等合金材质，其表面有深度为20-500μm的凹槽，凹槽为多边形或圆形，多边形外接圆直径或圆直径为10-3000μm；
所述纤维体直径为100-1500nm，纳米尺度卷曲的卷曲度为5-80％；
所述膜体厚度为5-300μm，微米尺度凹凸的粗糙度为5-300μm。
优选的，步骤(1)中所述非相容高弹性聚合物和低弹性聚合物的质量比为8：1-1：5，所述纺丝液质量分数为10-30wt％。
优选的，步骤(2)中所述静电纺丝参数为电压20-40kV、接收距离10-30cm。
优选的，步骤(2)中特制粗糙板中凹槽深度为100-300μm，多边形外接圆直径或圆直径为100-1000μm。
本发明与现有的技术相比，具有以下优点及突出效果：
(1)仅需借助特制粗糙板即可实现微米/纳米波浪卷曲纤维膜的制备，为微米/纳米波浪卷曲纤维膜的可控、宏量制备提供了可能；
(2)由于高弹性聚合物和低弹性聚合物的共混纺丝，结合微米/纳米波浪卷曲形态，所制备复合纤维膜具有独特的力学性能，断裂强度和断裂伸长率均呈现显著优势，且卷曲纤维堆叠形成的高孔隙率及膜体凹凸形成的高粗糙度，为高精度、低阻力膜分离等领域有广阔的应用前景。
附图说明
图1为微米/纳米波浪卷曲纤维膜的制备流程图。
图2为非相容PVDF-HFP/TPU纺丝液在表面有直径为900μm、深度为200μm的圆形凹槽特制粗糙板上制备的微米/纳米波浪卷曲纤维膜的电镜图。
图3为非相容PVDF-HFP/TPU纺丝液在光滑接收板上制备的纳米纤维膜的电镜图。
图4为PVDF-HFP纺丝液在表面有直径为900μm、深度为200μm的圆形凹槽特制粗糙板上制备的纳米纤维膜电镜图。
图5为非相容PMIA/TPU纺丝液在表面有直径为900μm、深度为200μm的圆形凹槽特制粗糙板上制备的微米/纳米波浪卷曲纤维膜的电镜图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
(1)纺丝液配置：将非相容高弹性聚合物热塑性聚氨酯弹性体(TPU)和低弹性聚合物偏氟乙烯-六氟丙烯共聚物(PVDF-HFP)以质量比为1：2溶于溶剂N，N-二甲基甲酰胺(DMF)中共混，室温下磁力搅拌6h，制备质量分数为18wt％的纺丝液，静置除掉气泡待用；
(2)静电纺丝：以表面有深度为200μm、直径为900μm圆形凹槽的不锈钢特制粗糙板作为接收基材，通过一步静电纺丝技术，在电压30kV、接收距离18cm的纺丝参数下，制备出平均直径为0.28μm的纳米纤维膜，且纤维体纳米尺度卷曲(纳米波浪)、膜体微米尺度凹凸(微米波浪)，膜体粗糙度14.79μm。
实施例2
(1)纺丝液配置：将非相容高弹性聚合物热塑性聚氨酯弹性体(TPU)和低弹性聚合物芳纶(PMIA)以质量比为1：1溶于溶剂N，N-二甲基甲酰胺(DMF)中共混，室温下磁力搅拌6h，制备质量分数为18wt％的纺丝液，静置除掉气泡待用；
(2)静电纺丝：以表面有深度为150μm、直径为1200μm圆形凹槽的不锈钢特制粗糙板作为接收基材，通过一步静电纺丝技术，在电压28kV、接收距离15cm的纺丝参数下，制备出平均直径为0.21μm的纳米纤维膜，且纤维体纳米尺度卷曲(纳米波浪)、膜体微米尺度凹凸(微米波浪)，膜体粗糙度11.62μm。
对比例1
(1)纺丝液配置：将非相容高弹性聚合物热塑性聚氨酯弹性体(TPU)和低弹性聚合物偏氟乙烯-六氟丙烯共聚物(PVDF-HFP)以质量比为1：2溶于溶剂N，N-二甲基甲酰胺(DMF)中共混，室温下磁力搅拌6h，制备质量分数为18wt％的纺丝液，静置除掉气泡待用；
(2)静电纺丝：以光滑不锈钢板作为接收基材，通过一步静电纺丝技术，在电压30kV、接收距离18cm的纺丝参数下，制备出平均直径为0.29μm的纳米纤维膜，且纤维体和膜体均无卷曲现象，膜体粗糙度3.01μm。
对比例2
(1)纺丝液配置：将单一低弹性聚合物偏氟乙烯-六氟丙烯共聚物(PVDF-HFP)溶于溶剂N，N-二甲基甲酰胺(DMF)中，室温下磁力搅拌6h，制备质量分数为18wt％的纺丝液，静置除掉气泡待用；
(2)静电纺丝：以表面有深度为200μm、直径为900μm圆形凹槽的不锈钢特制粗糙板作为接收基材，通过一步静电纺丝技术，在电压30kV、接收距离18cm的纺丝参数下，制备出平均直径为0.32μm的纳米纤维膜，且纤维体呈现纳米尺度微小卷曲、膜体呈现微米尺度凹凸，膜体粗糙度12.87μm。

Claims (1)

1.一种微米/纳米波浪卷曲纤维膜的制备方法，其特征在于，包括以下步骤：
(1)纺丝液配置：将非相容高弹性聚合物和低弹性聚合物以质量比为10：1-1：10溶于溶剂中共混，制备质量分数为5-40wt％的纺丝液；
(2)静电纺丝：以特制粗糙板作为接收基材，通过一步静电纺丝技术，在电压5-60kV、接收距离5-100cm的纺丝参数下，制备纤维体纳米尺度卷曲(纳米波浪)、膜体微米尺度凹凸(微米波浪)的微米/纳米波浪卷曲纤维膜；
所述高弹性聚合物为热塑性聚氨酯弹性体、聚烯烃热塑性弹性体的一种或以上，所述低弹性聚合物为聚苯乙烯、芳纶、聚偏二氟乙烯、偏氟乙烯-六氟丙烯共聚物、聚酰亚胺、聚砜、聚对苯二甲酸乙二醇酯的一种或以上；
所述纺丝液中所用溶剂为N，N-二甲基甲酰胺、N，N-二甲基乙酰胺、氯仿、二甲基亚砜、环己烷、异丁醇、二氯甲烷、甲苯、乙酸乙酯的一种或以上；
所述特制粗糙板为导电接收板，其材质可为铝制、铜制等金属材质或不锈钢等合金材质，其表面有深度为20-500μm的凹槽，凹槽为多边形或圆形，多边形外接圆直径或圆直径为10-3000μm；
所述纤维体直径为100-1500nm，纳米尺度卷曲的卷曲度为5-80％；
所述膜体厚度为5-300μm，微米尺度凹凸的粗糙度为5-300μm。
CN202410842055.0A 2024-06-27 2024-06-27 一种微米/纳米波浪卷曲纤维膜的制备方法 Pending CN118814359A (zh)

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