CN112516806A - 静电纺丝纤维膜的制备方法 - Google Patents

静电纺丝纤维膜的制备方法 Download PDF

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CN112516806A
CN112516806A CN202011083006.1A CN202011083006A CN112516806A CN 112516806 A CN112516806 A CN 112516806A CN 202011083006 A CN202011083006 A CN 202011083006A CN 112516806 A CN112516806 A CN 112516806A
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spinning
electrostatic spinning
mineralized
spinning solution
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黄衡
刘戈
陈承
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Ningbo Fotile Kitchen Ware Co Ltd
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Abstract

一种静电纺丝纤维膜的制备方法，其特征在于包括以下步骤：①纺丝液的制备：将聚合物树脂、添加剂及矿化材料溶解在溶剂中配制成纺丝液；②静电纺丝矿化纳米纤维膜的制备：将基底安装在静电纺丝设备的接收装置上，将步骤①得到的纺丝液脱泡后注入静电纺丝装置中，经静电纺丝和空气固化后，在凝固浴中固化成形，得到矿化的静电纺丝纤维膜。将矿化材料与静电纺丝纳米纤维结合，比表面增大，进水经过膜时能充分矿化，提高矿化效率；矿化材料固定在纳米纤维上，不存在脱落的风险，饮用水时更安全。

Description

静电纺丝纤维膜的制备方法
技术领域
本发明涉及一种纤维过滤膜的制备方法，应用于水净化装置上。
背景技术
为了提高水质，净水器中纳滤\反渗透膜滤芯的占有比例不断提升，导致水中的大量矿化物质被截留，不利于身体健康。为了矿化水质，目前市场上大多使用矿化水龙头、矿化储水桶等方式，达到矿化水的目的。矿化水龙头在使用过程中，水与水龙头接触时间较短，导致水质矿化效果差，达不到矿化水质的目的；矿化储水桶的存在，通过水浸泡时间的延长提高矿化效果，但是储水桶的存在，带来了水质污染的风险。
静电纺丝用于制备纤维膜越来越多，可以参考申请号为201610881964.0的中国发明专利申请公开《超疏水静电纺丝聚二甲基硅氧烷膜及其制备方法和应用》(申请公布号为CN 106334462 A)；还可以参考申请号为201710456146.0的中国发明专利申请公开《一种纳米结构符合超滤膜制备的新方法》(申请公布号为CN107081078A)。
如何将矿化和静电纺丝结合起来，制作出具有矿化功能的纤维膜，以提高水质的矿化水平，一直是本领域技术人员的研究课题。
发明内容
本发明所要解决的技术问题是针对上述的技术现状而提供一种将矿化材料与纤维膜融为一体成型的静电纺丝矿化纳米纤维膜的制备方法。
本发明解决上述技术问题所采用的技术方案为：1、一种静电纺丝纤维膜的制备方法，其特征在于包括以下步骤：
①纺丝液的制备：将5～20wt％的聚合物树脂、0～10wt％的添加剂和0～5wt％的矿化材料溶解在65～95wt％的溶剂中配制成纺丝液，各组分之和为100wt％；
②静电纺丝矿化纳米纤维膜的制备：将基底安装在静电纺丝设备的接收装置上，将步骤①得到的纺丝液脱泡后注入静电纺丝装置中，经静电纺丝和空气固化后，在凝固浴中固化成形，得到矿化的静电纺丝纤维膜。
作为优选，步骤①中所述的聚合物树脂为聚砜、聚醚砜、聚丙烯腈、聚偏氟乙烯、聚乳酸、聚丙烯或聚酰亚胺中的至少一种；
作为优选，步骤①中所述溶剂为N,N-二甲基乙酰胺、水、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、丙酮和二甲基亚砜中的至少一种。
作为优选，步骤①中所述添加剂为聚乙烯吡咯烷酮、聚乙二醇、氯化钾、溴化锂、氯化钠、氯化锂或硝酸锂中的至少一种；
作为优选，步骤①中所述矿化材料为木鱼石、沸石、麦饭石或扇贝壳中的至少一种，粒径为0.1～0.4μm。
作为优选，步骤②中所述的基底可以采用无纺布或编织管。
作为优选，所述的无纺布材质为涤纶、丙纶、锦纶或腈纶中的至少一种。
作为优选，步骤②中所述凝固浴为水或溶剂的水溶液。
作为优选，步骤②中所述静电纺丝条件如下：
纺丝电压为10～30KV，负压为3～10KV，溶液推进速度为0.5～3ml/h，纺丝温度为15～50℃，纺丝相对湿度为40～80％，接收装置转速为100～250rpm，接收距离10～20cm，纺丝针头的摆动速率为100～350cm/min。
作为优选，步骤②中所述基底在安装到静电纺丝设备之前，先对其进行预处理，该预处理：室温下无纺布在纺丝液的溶剂中浸渍0.5～5min。
与现有技术相比，本发明的优点在于：将矿化材料与静电纺丝纳米纤维结合，比表面增大，进水经过膜时能充分矿化，提高矿化效率；矿化材料固定在纳米纤维上，不存在脱落的风险，饮用水时更安全；纳米纤维膜的孔隙率高，比表面积大，通量大，压降小，有利于水顺利穿透过膜表面。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1
1)将涤纶无纺布在DMAc中浸泡2min。
2)纺丝液的制备
将氯化钾(KCl)和聚乙二醇(PEG)溶解于N,N-二甲基乙酰胺(DMAc)，加入聚醚砜(PES)和麦饭石(0.3μm)，在一定温度下搅拌，溶解完全后即得到纺丝液；
其中，纺丝液中KCl、PEG、DMAc、PES、麦饭石的质量分数为2％、2％、83％、10％、3％；
3)将步骤2)制得的纺丝液脱泡后置于静电纺丝设备中，将无纺布置于接收辊上，作为纳米纤维接收器，在以下条件下纺丝：静电纺丝温度为28℃，湿度为70％，正高压为17KV，负压为5KV，纺丝液速度为0.9mL/h，接收辊速度为180rpm，接收距离为10cm，针头摆动速率为150cm/min，纺丝2h后浸入凝固浴(纯水，45℃)中固化成形，取出烘干得矿化纳米纤维膜。
经测试，所得矿化纳米纤维膜的纤维平均直径为0.68μm，孔隙率为75％，纯水经过膜后TDS为925mg/L。
实施例2
1)将涤纶无纺布在DMAc中浸泡2min。
2)纺丝液的制备
将氯化钾(KCl)溶解于N,N-二甲基乙酰胺(DMAc)，加入聚醚砜(PES)和麦饭石(0.2μm)，在一定温度下搅拌，溶解完全后即得到纺丝液；
其中，纺丝液中KCl、DMAc、PES、麦饭石的质量分数为2％、84％、11％、3％；
3)将步骤2)制得的纺丝液脱泡后置于静电纺丝设备中，将无纺布置于接收辊上，作为纳米纤维接收器，在以下条件下纺丝：静电纺丝温度为32℃，湿度为75％，正高压为17KV，负压为5KV，a液速度为1.2mL/h，接收辊速度为200rpm，接收距离为10cm，针头摆动速率为160cm/min，纺丝2h后浸入凝固浴(纯水，40℃)中固化成形，取出烘干得矿化纳米纤维膜。
经测试，所得矿化纳米纤维膜的纤维平均直径为0.65μm，孔隙率为77％，纯水经过膜后TDS为1003mg/L。
实施例3
1)将锦纶无纺布在DMAc中浸泡1min。
2)纺丝液的制备
将氯化锂(LiCl)溶解于N,N-二甲基乙酰胺(DMAc)中，加入聚醚砜(PES)、麦饭石(0.3μm)，在一定温度下搅拌，溶解完全后即得到纺丝液；
其中，纺丝液中LiCl、DMAc、PES、麦饭石的质量分数为3％、80％、12％、5％；
3)将步骤2)制得的纺丝液脱泡后置于静电纺丝设备中，将无纺布置于接收辊上，作为纳米纤维接收器，在以下条件下纺丝：静电纺丝温度为28℃，湿度为70％，正高压为23KV，负压为5KV，纺丝液速度为1.0mL/h，接收辊速度为200rpm，接收距离为15cm，针头摆动速率为200cm/min，纺丝1.5h后浸入凝固浴(纯水，45℃)中固化成形，取出烘干得矿化纳米纤维膜。
经测试，所得矿化纳米纤维膜的纤维平均直径为0.76μm，孔隙率为79％，纯水经过膜后TDS为1162mg/L；
实施例4
1)将丙纶无纺布在DMAc中浸泡5min。
2)纺丝液的制备
将氯化钾(LiCl)和聚乙二醇(PEG)溶解于N,N-二甲基乙酰胺(DMAc)中，加入聚乳酸(PLA)麦饭石(0.3μm)，在一定温度下搅拌，溶解完全后即得到纺丝液；
其中，纺丝液中KCl、PEG、DMAc、PLA、麦饭石的质量分数为3％、5％、77％、12％、3％；
3)将步骤2)制得的纺丝液脱泡后置于静电纺丝设备中，将无纺布置于接收辊上，作为纳米纤维接收器，在以下条件下纺丝：静电纺丝温度为35℃，湿度为80％，正高压为25KV，负压为5KV，纺丝液速度为1.5mL/h，接收辊速度为250rpm，接收距离为15cm，针头摆动速率为200cm/min，纺丝1h后浸入凝固浴(纯水，40℃)中固化成形，取出烘干得矿化纳米纤维膜。
经测试，所得矿化纳米纤维膜的纤维平均直径为0.75μm，孔隙率为79％，纯水经过膜后TDS为1063mg/L。

Claims (10)

1.一种静电纺丝纤维膜的制备方法，其特征在于包括以下步骤：
①纺丝液的制备：将5～20wt％的聚合物树脂、0～10wt％的添加剂和0～5wt％的矿化材料溶解在65～95wt％的溶剂中配制成纺丝液，各组分之和为100wt％；
②静电纺丝矿化纳米纤维膜的制备：将基底安装在静电纺丝设备的接收装置上，将步骤①得到的纺丝液脱泡后注入静电纺丝装置中，经静电纺丝和空气固化后，在凝固浴中固化成形，得到矿化的静电纺丝纤维膜。
2.根据权利要求1所述的制备方法，其特征在于步骤①中所述的聚合物树脂为聚砜、聚醚砜、聚丙烯腈、聚偏氟乙烯、聚乳酸、聚丙烯或聚酰亚胺中的至少一种。
3.根据权利要求1所述的制备方法，其特征在于步骤①中所述溶剂为N,N-二甲基乙酰胺、水、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、丙酮和二甲基亚砜中的至少一种。
4.根据权利要求1所述的制备方法，其特征在于步骤①中所述添加剂为聚乙烯吡咯烷酮、聚乙二醇、氯化钾、溴化锂、氯化钠、氯化锂或硝酸锂中的至少一种。
5.根据权利要求1所述的制备方法，其特征在于步骤①中所述矿化材料为木鱼石、沸石、麦饭石或扇贝壳中的至少一种，粒径为0.1～0.4μm。
6.根据权利要求1所述的制备方法，其特征在于步骤②中所述的基底采用无纺布或编织管。
7.根据权利要求6所述的制备方法，其特征在于所述的无纺布材质为涤纶、丙纶、锦纶或腈纶中的至少一种。
8.根据权利要求1所述的制备方法，其特征在于步骤②中所述凝固浴为水或溶剂的水溶液。
9.根据权利要求1所述的制备方法，其特征在于步骤②中所述静电纺丝条件如下：
纺丝电压为10～30KV，负压为3～10KV，溶液推进速度为0.5～3ml/h，纺丝温度为15～50℃，纺丝相对湿度为40～80％，接收装置转速为100～250rpm，接收距离10～20cm，纺丝针头的摆动速率为100～350cm/min。
10.根据权利要求1所述的制备方法，其特征在于步骤②中所述基底在安装到静电纺丝设备之前，先对其进行预处理，该预处理：室温下无纺布在纺丝液的溶剂中浸渍0.5～5min。
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