CN114134702B - 基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法 - Google Patents

基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法 Download PDF

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CN114134702B
CN114134702B CN202111154095.9A CN202111154095A CN114134702B CN 114134702 B CN114134702 B CN 114134702B CN 202111154095 A CN202111154095 A CN 202111154095A CN 114134702 B CN114134702 B CN 114134702B
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任改焕
田璐璐
卢东旭
刘春晖
张盼
李博
任帅领
李伟涛
何建新
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Abstract

本发明公开了一种基于硫基‑烯光化学反应的无氟静电纺防水透湿膜的制备方法，包括以下步骤：步骤1、以N,N‑二甲基乙酰胺(DMAc)、丙酮为溶剂配置硅基聚氨酯/聚甲基丙烯酸甲酯(Si‑PU/PMMA)纺丝液，添加2,4,6,8‑四甲基‑2,4,6,8四环硅氧烷(TMTVSi)、正十八硫醇作为疏水剂和交联剂，2,2‑二甲基‑2‑苯基苯乙酮(DMPA)为光催化剂，通过静电纺丝工艺制备出疏水纤维膜，本发明中的静电纺防水透湿膜经紫外光照处理后，纤维间形成化学交联结构，从而减小防水透湿膜的最大孔径提高其耐水性，同时化学交联结构能显著增大纤维间的摩擦力提高其机械性能，满足其在防护服装领域中的应用要求。

Description

基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法
技术领域
本发明属于静电纺丝功能材料领域，涉及一种基于烯烃-疏基点击反应的无氟防水透湿膜制备方法。
背景技术
防水透湿膜是指水在一定压力下不浸入内部，而人体散发的汗液却能以水蒸气的形式传导到外界，从而避免汗液积聚冷凝在体表与衣物之间，保持人体的舒适，它是一种高技术、独具特色的功能性膜。静电纺丝技术制备的纳米纤维膜在空间上具有一定厚度，呈网状结构。静电纺纳米纤维具有纤维直径小、孔径小、孔隙率高以及孔道连通性好等特点，纤维与纤维之间存在微孔，可以有效的传递水蒸气分子，而外界的液态水滴由于直径远大于纤维之间的孔径而被阻止进入，因此具有良好的防水透湿性能，在制备防水透湿功能膜领域具有巨大的应用优势。含氟材料具有低表面能和高疏水性的特征而成为制备防水透湿膜的主要选择，但是，大多数含氟材料分解后会产生全氟辛烷磺酰基化合物，它是一种极难降解的有机污染物，具有长期生物积累性以及远距离迁移性，对人体健康和生态环境具有潜在的威胁。
发明内容
本发明的目的在于提供基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：
基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，包括一下步骤：
步骤1、以N,N-二甲基乙酰胺(DMAc)、丙酮为溶剂配置硅基聚氨酯/聚甲基丙烯酸甲酯(Si-PU/PMMA)纺丝液，添加2,4,6,8-四甲基-2,4,6,8-四乙烯基环四硅氧烷(TMTVSi)、正十八硫醇作为疏水剂和交联剂，2,2-二甲基-2-苯基苯乙酮(DMPA)为光催化剂，通过静电纺丝工艺制备出疏水纤维膜；
步骤2、对纤维膜进行紫外线照射，引发疏基-烯烃的原位聚合反应，形成化学交联，调控纤维膜的孔结构，增强纤维膜的防水性并提高其力学性能，获得静电纺防水透湿膜。
作为本发明的进一步技术方案，所述纺丝液中Si-PU/PMMA的质量分数为5-30%。
作为本发明的进一步技术方案，所述纺丝液中TMTVSi占Si-PU/PMMA质量分数为1-30%。
作为本发明的进一步技术方案，所述纺丝液中正十八硫醇占Si-PU/PMMA质量分数为5-50%。
作为本发明的进一步技术方案，所述静电纺丝电压为5-50 kV，接收距离为5-30cm，纺丝液的供液速度为0.5-10 ml/h，所得纤维膜的厚度为5-100 μm。
作为本发明的进一步技术方案，对纤维膜进行紫外光照射时采用的紫外光波长为200-500 nm，处理时间为0.1-120 min。
作为本发明的进一步技术方案，静电纺丝过程中接收基材为涤纶布(300T)。
作为本发明的进一步技术方案，制备出的防水透湿膜耐水压≥50 kPa，透湿率≥7kg·m-2·d-1，断裂强力≥7 MPa。
与现有技术相比，本发明的有益效果是：（1）本发明中的静电纺防水透湿膜经紫外光照处理后，纤维间形成化学交联结构，从而减小防水透湿膜的最大孔径提高其耐水性，同时化学交联结构能显著增大纤维间的摩擦力提高其机械性能，满足其在防护服装领域中的应用要求。
（2）本发明中的静电纺防水透湿膜采用无氟材料制备，在实际应用中不会对环境产生破坏，避免对穿着者的身体健康造成损害。
附图说明
图1为本发明制备的防水透湿膜的扫描电镜图片。
图2为本发明中所涉及的巯基-烯光化学反应。
图3为反应物(TMTVSi和硫醇)在紫外线照射之前(底部)和之后(顶部)的红外光谱。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
请参阅图1-3所示，实施例1：
基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，步骤如下：
1）以DMAc、丙酮为溶剂，质量比为6:4，Si-PU/PMMA的质量分数为12%，正十八硫醇质量为Si-PU/PMMA质量的15%，正十八硫醇质量为Si-PU/PMMA质量的20%，DMPA为正十八硫醇和TMTVSi质量的0.5%配置纺丝液。通过静电纺丝方法在涤纶布(300T)上制备疏水纤维膜，纺丝电压为25 kV，纺丝距离为18 cm，供液速度为8 ml/h，所得疏水纤维膜的厚度为80μm。
2）采用紫外光波长为362 nm的紫外光源辐射30 min，引发疏基-烯烃点击反应，使聚合物相互键合交联成网状结构，增强纤维膜的耐水性与结构稳定性，获得具备优异防水、透湿及力学性能的防水透湿膜，耐水压值为50.4 kPa，透湿量为8.9 kg·m-2·d-1，断裂强力为7.6 MPa。
实施例2
基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，步骤如下：
1）以DMAc、丙酮为溶剂，质量比为6:4，Si-PU/PMMA的质量分数为12%，正十八硫醇质量为Si-PU/PMMA质量的30%，正十八硫醇质量为Si-PU/PMMA质量的20%，DMPA为正十八硫醇和TMTVSi质量的0.5%配置纺丝液。通过静电纺丝方法在涤纶布(300T)上制备疏水纤维膜，纺丝电压为25 kV，纺丝距离为18 cm，供液速度为8 ml/h，所得疏水纤维膜的厚度为80μm。
2）采用紫外光波长为362 nm的紫外光源辐射30 min，引发疏基-烯烃点击反应，使聚合物相互键合交联成网状结构，增强纤维膜的耐水性与结构稳定性，获得具备优异防水、透湿及力学性能的防水透湿膜，耐水压值为64.43 kPa，透湿量为7.8kg·m-2·d-1，断裂强力为10.04 MPa。
实施例3
基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，步骤如下：
1）以DMAc、丙酮为溶剂，质量比为6:4，Si-PU/PMMA的质量分数为12%，正十八硫醇质量为Si-PU/PMMA质量的30%，正十八硫醇质量为Si-PU/PMMA质量的20%，DMPA为正十八硫醇和TMTVSi质量的0.5%配置纺丝液。通过静电纺丝方法在涤纶布(300T)上制备疏水纤维膜，纺丝电压为25 kV，纺丝距离为18 cm，供液速度为8 ml/h，所得疏水纤维膜的厚度为80μm。
2）采用紫外光波长为362 nm的紫外光源辐射30 min，引发疏基-烯烃点击反应，使聚合物相互键合交联成网状结构，增强纤维膜的耐水性与结构稳定性，获得具备优异防水、透湿及力学性能的防水透湿膜，耐水压值为68.54 kPa，透湿量为7.04kg·m-2·d-1，断裂强力为11.75 MPa。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何附图标记视为限制所涉及的权利要求。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。

Claims (8)

1.基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，包括一下步骤：
步骤1、以N,N-二甲基乙酰胺(DMAc)、丙酮为溶剂配置硅基聚氨酯/聚甲基丙烯酸甲酯(Si-PU/PMMA)纺丝液，添加2,4,6,8-四甲基-2,4,6,8-四乙烯基环四硅氧烷、正十八硫醇作为疏水剂和交联剂，2,2-二甲基-2-苯基苯乙酮(DMPA)为光催化剂，通过静电纺丝工艺制备出疏水纤维膜；
步骤2、对纤维膜进行紫外线照射，引发疏基-烯烃的原位聚合反应，形成化学交联，调控纤维膜的孔结构，增强纤维膜的防水性并提高其力学性能，获得静电纺防水透湿膜。
2.根据权利要求1所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，所述纺丝液中Si-PU/PMMA的质量分数为5-30%。
3.根据权利要求1所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，所述纺丝液中TMTVSi占Si-PU/PMMA质量分数为1-30%。
4.根据权利要求1所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，所述纺丝液中正十八硫醇占Si-PU/PMMA质量分数为5-50%。
5.根据权利要求1所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，所述静电纺丝电压为5-50 kV，接收距离为5-30 cm，纺丝液的供液速度为0.5-10ml/h，所得纤维膜的厚度为5-100 μm。
6.根据权利要求1所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，对纤维膜进行紫外光照射时采用的紫外光波长为200-500 nm，处理时间为0.1-120 min。
7.根据权利要求1所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，静电纺丝过程中接收基材为涤纶布。
8.根据权利要求2所述的基于疏基-烯光反应的无氟静电纺防水透湿膜的制备方法，其特征在于，制备出的防水透湿膜耐水压≥50 kPa，透湿率≥7 kg·m-2·d-1，断裂强力≥7MPa。
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