CN113293508A - 一种复合纤维膜及其制备方法和应用 - Google Patents

一种复合纤维膜及其制备方法和应用 Download PDF

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CN113293508A
CN113293508A CN202110408598.8A CN202110408598A CN113293508A CN 113293508 A CN113293508 A CN 113293508A CN 202110408598 A CN202110408598 A CN 202110408598A CN 113293508 A CN113293508 A CN 113293508A
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solution
layer
component
fiber membrane
composite fiber
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许瞳
孟海涛
白杰
李春萍
徐薇
徐广然
柳欢
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Inner Mongolia University of Technology
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Abstract

本发明属于纤维膜技术领域。本发明提供了一种复合纤维膜，包含疏水层、转移层和亲水层；疏水层原料为聚偏氟乙烯和/或聚四氟乙烯；转移层原料包含重量比为1∶9～11的A组分和B组分；亲水层原料包含重量比为1∶9～11的C组分和B组分；A组分为聚乙烯吡咯烷酮或聚乙二醇；B组分为聚苯胺、聚醚砜、聚乳酸或醋酸纤维素；C组分为2‑甲基丙烯酰氧乙基磷酸胆碱或聚[(2‑甲基丙烯酰氧基)乙基]二甲基[3‑磺丙基]氢氧化铵。本发明还提供了一种复合纤维膜的制备方法和应用。本发明的复合纤维膜具有良好的单向水运输性能；在40℃下，水分蒸发速率为0.3～0.67g/h。

Description

一种复合纤维膜及其制备方法和应用
技术领域
本发明涉及纤维膜技术领域，尤其涉及一种复合纤维膜及其制备方法和应用。
背景技术
液体的单向运输在众多生理和物理过程中必不可少，例如生物体排汗、细胞膜的液体传输、海水脱盐、燃料电池内部电解质膜两侧液体定向流动等。近年来，液体单向运输受到越来越广泛的关注和研究。复合纤维膜具有亲水/疏水差异，使得复合纤维膜具有特殊的单向透过性能。目前，单向水运输的复合纤维膜的研究较少，并且存在稳定性较差、不能完全实现单向水运输、能耗高、工艺复杂等不足。
因此，研究开发一种能耗低、工艺简单、提高水的运输速率和稳定性的复合纤维膜，具有重要的应用价值。
发明内容
本发明的目的是针对现有技术的不足提供一种复合纤维膜及其制备方法。本发明的复合纤维膜具有良好的单向水运输性能和吸汗排湿功能。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种复合纤维膜，包含疏水层、转移层和亲水层；
所述疏水层原料为聚偏氟乙烯和/或聚四氟乙烯；
所述转移层原料包含重量比为1∶9～11的A组分和B组分；
所述亲水层原料包含重量比为1∶9～11的C组分和B组分；
所述A组分为聚乙烯吡咯烷酮或聚乙二醇；
所述B组分为聚苯胺、聚醚砜、聚乳酸或醋酸纤维素；
所述C组分为2-甲基丙烯酰氧乙基磷酸胆碱或聚[(2-甲基丙烯酰氧基)乙基]二甲基[3-磺丙基]氢氧化铵；
所述亲水层在复合纤维膜的最上层或最下层。
本发明还提供了一种所述的复合纤维膜的制备方法，包含如下步骤：
1)将疏水层溶液、转移层溶液、亲水层溶液独立顺次进行加热处理、超声处理，得到三种纺丝溶液；
2)对三种纺丝溶液独立进行静电纺丝，得到纤维膜；
3)将交联剂、光引发剂、单体和氯化钠溶液形成的水凝胶溶液和纤维膜进行交联反应，即得复合纤维膜；
作为优选，步骤1)所述疏水层溶液包含重量比为1∶9～11的疏水层原料和溶剂；所述转移层溶液包含重量比为1∶9～11的转移层原料和N，N-二甲基甲酰胺；所述亲水层溶液包含重量比为1∶9～11的亲水层原料和溶剂。
作为优选，所述疏水层溶液中，溶剂包含重量比为2～4∶6～8的丙酮和N，N-二甲基甲酰胺；所述亲水层溶液中，溶剂包含重量比为1∶8～10的六氟异丙醇和N，N-二甲基甲酰胺。
作为优选，步骤1)所述加热处理的温度为18～60℃，时间为15～26h，所述加热处理在搅拌条件下进行。
作为优选，步骤1)所述超声处理的温度为18～60℃，时间为0.3～1.5h，超声处理的频率为30～50kHz。
作为优选，步骤2)所述静电纺丝中，针头内径为0.3～0.5mm，针头外径为0.6～0.8mm；推注速度为0.4～1.5mL/h，针头和接收滚筒之间的距离为12～20cm；针头平移速度为280～320mm/min，针头平移行程为480～520mm。
作为优选，步骤2)所述静电纺丝的时间为5～60min，温度为20～30℃，电压为12～18kV。
作为优选，步骤3)所述交联剂为N，N-亚甲基双丙烯酰胺，所述交联剂和单体的质量比为1∶94～104；所述单体与亲水层原料中的C组分的种类和质量均相同；所述单体在水凝胶溶液中的质量浓度为9.4～10.4％；所述光引发剂为2-羟基-2-甲基-1-苯基-1-丙酮，所述光引发剂在水凝胶溶液中的质量浓度为1～5％；所述氯化钠溶液中，氯化钠的摩尔浓度为0.5～1.5mol/L。
作为优选，步骤3)所述交联反应在紫外光下进行，所述紫外光的波长为350～380nm，所述交联反应的时间为10～30min。
本发明还提供了一种所述的复合纤维膜在单向水运输中的应用。
本发明的有益效果为：
本发明的复合纤维膜具有三层结构，分别为疏水层、亲水层和转移层，三层纤维膜通过静电力的作用结合在一起，再采用紫外光照射的方式，对亲水层进行交联，得到本发明的复合纤维膜。本发明提供的复合纤维膜具有良好的单向水运输性能；在40℃下，水分蒸发速率为0.3～0.67g/h。
附图说明
图1为实施例1的复合纤维膜的水运输试验图；
图2为实施例2的复合纤维膜的上表面和下表面润湿过程图，其中，(A)为上表面，(B)为下表面；
图3为实施例2的复合纤维膜的动态水接触角演变图；
图4为实施例2的复合纤维膜在40℃下的水分蒸发试验图。
具体实施方式
本发明提供了一种复合纤维膜，包含疏水层、转移层和亲水层；
所述疏水层原料为聚偏氟乙烯和/或聚四氟乙烯；
所述转移层原料包含重量比为1∶9～11的A组分和B组分；
所述亲水层原料包含重量比为1∶9～11的C组分和B组分；
所述A组分为聚乙烯吡咯烷酮或聚乙二醇；
所述B组分为聚苯胺、聚醚砜、聚乳酸或醋酸纤维素；
所述C组分为2-甲基丙烯酰氧乙基磷酸胆碱或聚[(2-甲基丙烯酰氧基)乙基]二甲基[3-磺丙基]氢氧化铵；
所述亲水层在复合纤维膜的最上层或最下层。
本发明所述转移层的原料优选包含重量比为1∶10的A组分和B组分；所述亲水层的原料优选包含重量比为1∶10的C组分和B组分。
本发明还提供了一种所述的复合纤维膜的制备方法，包含如下步骤：
1)将疏水层溶液、转移层溶液、亲水层溶液独立顺次进行加热处理、超声处理，得到三种纺丝溶液；
2)对三种纺丝溶液独立进行静电纺丝，得到纤维膜；
3)将交联剂、光引发剂、单体和氯化钠溶液形成的水凝胶溶液和纤维膜进行交联反应，即得复合纤维膜；
步骤1)所述疏水层溶液包含重量比为1∶9～11的疏水层原料和溶剂；所述转移层溶液包含重量比为1∶9～11的转移层原料和N，N-二甲基甲酰胺；所述亲水层溶液包含重量比为1∶9～11的亲水层原料和溶剂。
本发明步骤1)所述疏水层溶液优选包含重量比为1∶10的疏水层原料和溶剂；所述溶剂优选包含丙酮和N，N-二甲基甲酰胺，所述丙酮和N，N-二甲基甲酰胺的重量比优选为2～4∶6～8，进一步优选为3∶7。
本发明步骤1)所述转移层溶液优选包含重量比为1∶10的转移层原料和N，N-二甲基甲酰胺；所述亲水层溶液优选包含重量比为1∶10的亲水层原料和溶剂；所述溶剂优选包含六氟异丙醇和N，N-二甲基甲酰胺，所述六氟异丙醇和N，N-二甲基甲酰胺的重量比优选为1∶8～10，进一步优选为1∶9。
本发明步骤1)所述加热处理的温度优选为18～60℃，进一步优选为25～50℃；更优选为35～45℃；所述加热处理的时间优选为15～26h，进一步优选为18～24h，更优选为20～22h；所述加热处理优选在搅拌条件下进行。
本发明步骤1)所述超声处理的温度优选为18～60℃，进一步优选为25～50℃，更优选为35～45℃；所述超声处理的时间优选为0.3～1.5h，进一步优选为0.5～1h；所述超声处理的频率优选为30～50kHz，进一步优选为35～45kHz。
本发明步骤2)所述静电纺丝中，针头内径优选为0.3～0.5mm，进一步优选为0.4mm；针头外径优选为0.6～0.8mm，进一步优选为0.7mm；推注速度优选为0.4～1.5mL/h，进一步优选为0.8～1.2mL/h；针头和接收滚筒之间的距离优选为12～20cm，进一步优选为15～18cm；接收滚筒的转速优选为30～50r/min，进一步优选为40r/min；接收装置优选采用铝箔包覆在接收滚筒上；针头平移速度优选为280～320mm/min，进一步优选为290～310mm/min，更优选为300mm/min；针头平移行程优选为480～520mm，进一步优选为490～510mm，更优选为500mm。
本发明步骤2)所述静电纺丝的时间优选为5～60min，进一步优选为15～45min，更优选为25～35min；所述静电纺丝的温度优选为20～30℃，进一步优选为23～27℃；所述静电纺丝的电压优选为12～18kV，进一步优选为14～16kV；所述静电纺丝的相对湿度优选为30～40％，进一步优选为35％。
本发明将亲水层溶液、疏水层溶液和转移层溶液，按照特定的纺丝顺序顺次的进行静电纺丝，纺丝完第一层结构后，换装溶液纺织第二层结构，纺织完第二层结构后，换装溶液纺织第三层结构，全部纺织结束后，三层结构通过静电力的作用结合在一起，得到纤维膜；本发明的纺丝顺序为亲水层、疏水层、转移层，或者亲水层、转移层、疏水层，或者疏水层、转移层、亲水层，或者转移层、疏水层、亲水层。
本发明步骤3)所述交联剂优选为N，N-亚甲基双丙烯酰胺，所述交联剂和单体的质量比优选为1∶94～104，进一步优选为1∶97～102，更优选为1∶99；所述单体优选与亲水层原料中的C组分的种类和质量均相同；所述单体在水凝胶溶液中的质量浓度优选为9.4～10.4％，进一步优选为9.7～10.2％，更优选为9.9％；所述光引发剂优选为2-羟基-2-甲基-1-苯基-1-丙酮，所述光引发剂在水凝胶溶液中的质量浓度优选为1～5％，进一步优选为3～4％；所述氯化钠溶液中，氯化钠的摩尔浓度优选为0.5～1.5mol/L，进一步优选为1mol/L。
本发明步骤3)所述交联反应优选在紫外光下进行，所述紫外光的波长优选为350～380nm，进一步优选为360～370nm，更优选为365nm；所述交联反应的时间优选为10～30min，进一步优选为20min；所述交联反应优选将水凝胶溶液滴加在纤维膜的亲水层上，水凝胶溶液和纤维膜的亲水层在紫外光下发生交联反应。
本发明中，交联反应结束后优选进行洗涤和干燥，所述洗涤的试剂优选为水，所述洗涤的次数优选为2～5次，更优选为3～4次，所述干燥的温度优选为30～50℃，进一步优选为35～45℃，更优选为40℃。
本发明还提供了一种所述的复合纤维膜在单向水运输中的应用。
下面结合实施例对本发明提供的技术方案进行详细的说明，但是不能把它们理解为对本发明保护范围的限定。
实施例1
将100g聚偏氟乙烯加入到300g丙酮和700gN，N-二甲基甲酰胺的混合溶剂中，得到疏水层溶液；将10g聚乙烯吡咯烷酮和100g聚苯胺加入到1100gN，N-二甲基甲酰胺中，得到转移层溶液；将10g 2-甲基丙烯酰氧乙基磷酸胆碱和100g聚苯胺加入到110g六氟异丙醇和990gN，N-二甲基甲酰胺的混合溶剂中，得到亲水层溶液。
将疏水层溶液、转移层溶液、亲水层溶液分别独立的在40℃，搅拌的条件下溶解20h，然后在40℃、40kHz频率下超声处理1h，得到疏水层纺丝溶液、转移层纺丝溶液、亲水层纺丝溶液。
对亲水层纺丝溶液进行静电纺丝处理：采用20mL的注射器，针头内径0.41mm，针头外径0.71mm，针头的推注速度0.8mL/h，针头和接收滚筒的距离为16cm，接收滚筒的转速为40r/min，针头平移速度为300mm/min，针头平移行程为500mm。静电纺丝的电压12kV，温度为25℃，时间为30min，相对湿度为35％。
亲水层纺丝结束后，换装转移层纺丝溶液进行纺丝处理：纺丝电压为16kV，针头和接收滚筒的距离为17cm，针头的推注速度0.6mL/h，其他条件与亲水层纺丝处理相同。
转移层纺丝结束后，换装疏水层纺丝溶液进行纺丝处理：纺丝电压为13kV，针头和接收滚筒的距离为18cm，针头的推注速度1.2mL/h，其他条件与亲水层纺丝处理相同。亲水层纺丝结束后，得到由上到下为疏水层、转移层、亲水层的纤维膜。
配制水凝胶溶液：氯化钠水溶液的浓度为1mol/L，2-甲基丙烯酰氧乙基磷酸胆碱10g，N，N-亚甲基双丙烯酰胺0.1g，2-甲基丙烯酰氧乙基磷酸胆碱在水凝胶溶液中的质量浓度为10％，2-羟基-2-甲基-1-苯基-1-丙酮在水凝胶溶液中的质量浓度为3％。将配制好的水凝胶溶液滴加在纤维膜上的亲水层表面，滴加完成后在360nm的紫外光下交联20min，交联结束后使用去离子水洗涤3次，然后在40℃下干燥，即得复合纤维膜。
实施例1的复合纤维膜在40℃下，水分蒸发速率为0.67g/h。
图1为实施例1的复合纤维膜的水运输试验图。
实施例2
将100g聚偏四氟乙烯加入到200g丙酮和700gN，N-二甲基甲酰胺的混合溶剂中，得到疏水层溶液；将10g聚乙二醇和90g聚醚砜加入到900gN，N-二甲基甲酰胺中，得到转移层溶液；将10g聚[(2-甲基丙烯酰氧基)乙基]二甲基[3-磺丙基]氢氧化铵和90g聚乳酸加入到90g六氟异丙醇和810gN，N-二甲基甲酰胺的混合溶剂中，得到亲水层溶液。
将疏水层溶液、转移层溶液、亲水层溶液分别独立的在20℃，搅拌的条件下溶解24h，然后在20℃、30kHz频率下超声处理1.5h，得到疏水层纺丝溶液、转移层纺丝溶液、亲水层纺丝溶液。
对疏水层纺丝溶液进行静电纺丝处理：采用20mL的注射器，针头内径0.3mm，针头外径0.6mm，针头的推注速度0.6mL/h，针头和接收滚筒的距离为17cm，接收滚筒的转速为32r/min，针头平移速度为280mm/min，针头平移行程为480mm。静电纺丝的电压14kV，温度为25℃，时间为10min，相对湿度为35％。
疏水层纺丝结束后，换装转移层纺丝溶液进行纺丝处理：纺丝电压为13kV，针头和接收滚筒的距离为18cm，针头的推注速度0.8mL/h，其他条件与疏水层纺丝处理相同。
转移层纺丝结束后，换装亲水层纺丝溶液进行纺丝处理：纺丝电压为12kV，针头和接收滚筒的距离为18cm，针头的推注速度0.9mL/h，其他条件与疏水层纺丝处理相同。亲水层纺丝结束后，得到由上到下为亲水层、转移层、疏水层的纤维膜。
配制水凝胶溶液：氯化钠水溶液的浓度为0.7mol/L，聚[(2-甲基丙烯酰氧基)乙基]二甲基[3-磺丙基]氢氧化铵9.7g，N，N-亚甲基双丙烯酰胺0.1g，聚[(2-甲基丙烯酰氧基)乙基]二甲基[3-磺丙基]氢氧化铵在水凝胶溶液中的质量浓度为9.7％，2-羟基-2-甲基-1-苯基-1-丙酮在水凝胶溶液中的质量浓度为1.5％。将配制好的水凝胶溶液滴加在纤维膜上的亲水层表面，滴加完成后在350nm的紫外光下交联30min，交联结束后使用去离子水洗涤2次，然后在35℃下干燥，即得复合纤维膜。
图2为采用8μL的墨滴对实施例2的复合纤维膜进行上表面和下表面的润湿过程图。
图3为实施例2的复合纤维膜的动态水接触角演变图。
图4为实施例2的复合纤维膜中取长宽均为2cm的复合纤维膜片，在40℃烘箱内的水分蒸发试验图；由图4可知，40℃下，复合纤维膜的水分蒸发速率为0.582g/h。
实施例3
将100g聚偏氟乙烯加入到400g丙酮和700gN，N-二甲基甲酰胺的混合溶剂中，得到疏水层溶液；将10g聚乙烯吡咯烷酮和110g醋酸纤维素加入到1200gN，N-二甲基甲酰胺中，得到转移层溶液；将10g 2-甲基丙烯酰氧乙基磷酸胆碱和110g醋酸纤维素加入到120g六氟异丙醇和1200gN，N-二甲基甲酰胺的混合溶剂中，得到亲水层溶液。
将疏水层溶液、转移层溶液、亲水层溶液分别独立的在50℃，搅拌的条件下溶解15h，然后在50℃、50kHz频率下超声处理0.5h，得到疏水层纺丝溶液、转移层纺丝溶液、亲水层纺丝溶液。
对转移层纺丝溶液进行静电纺丝处理：采用20mL的注射器，针头内径0.47mm，针头外径0.78mm，针头的推注速度1.4mL/h，针头和接收滚筒的距离为18cm，接收滚筒的转速为48r/min，针头平移速度为320mm/min，针头平移行程为520mm。静电纺丝的电压17kV，温度为27℃，时间为50min，相对湿度为35％。
转移层纺丝结束后，换装疏水层纺丝溶液进行纺丝处理：纺丝电压为15kV，针头和接收滚筒的距离为15cm，针头的推注速度1.2mL/h，其他条件与转移层纺丝处理相同。
疏水层纺丝结束后，换装亲水层纺丝溶液进行纺丝处理：纺丝电压为14kV，针头和接收滚筒的距离为17cm，针头的推注速度1.2mL/h，其他条件与转移层纺丝处理相同。亲水层纺丝结束后，得到由上到下为亲水层、疏水层、转移层的纤维膜。
配制水凝胶溶液：氯化钠水溶液的浓度为1.5mol/L，2-甲基丙烯酰氧乙基磷酸胆碱10.3g，N，N-亚甲基双丙烯酰胺0.1g，2-甲基丙烯酰氧乙基磷酸胆碱在水凝胶溶液中的质量浓度为10.3％，2-羟基-2-甲基-1-苯基-1-丙酮在水凝胶溶液中的质量浓度为5％。将配制好的水凝胶溶液滴加在纤维膜上的亲水层表面，滴加完成后在370nm的紫外光下交联12min，交联结束后使用去离子水洗涤4次，然后在47℃下干燥，即得复合纤维膜。
实施例3的复合纤维膜在40℃下，水分蒸发速率为0.5g/h。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种复合纤维膜，其特征在于，包含疏水层、转移层和亲水层；
所述疏水层原料为聚偏氟乙烯和/或聚四氟乙烯；
所述转移层原料包含重量比为1∶9～11的A组分和B组分；
所述亲水层原料包含重量比为1∶9～11的C组分和B组分；
所述A组分为聚乙烯吡咯烷酮或聚乙二醇；
所述B组分为聚苯胺、聚醚砜、聚乳酸或醋酸纤维素；
所述C组分为2-甲基丙烯酰氧乙基磷酸胆碱或聚[(2-甲基丙烯酰氧基)乙基]二甲基[3-磺丙基]氢氧化铵；
所述亲水层在复合纤维膜的最上层或最下层。
2.权利要求1所述的复合纤维膜的制备方法，其特征在于，包含如下步骤：
1)将疏水层溶液、转移层溶液、亲水层溶液独立顺次进行加热处理、超声处理，得到三种纺丝溶液；
2)对三种纺丝溶液独立进行静电纺丝，得到纤维膜；
3)将交联剂、光引发剂、单体和氯化钠溶液形成的水凝胶溶液和纤维膜进行交联反应，即得复合纤维膜；
步骤1)所述疏水层溶液包含重量比为1∶9～11的疏水层原料和溶剂；所述转移层溶液包含重量比为1∶9～11的转移层原料和N，N-二甲基甲酰胺；所述亲水层溶液包含重量比为1∶9～11的亲水层原料和溶剂。
3.根据权利要求2所述的制备方法，其特征在于，所述疏水层溶液中，溶剂包含重量比为2～4∶6～8的丙酮和N，N-二甲基甲酰胺；所述亲水层溶液中，溶剂包含重量比为1∶8～10的六氟异丙醇和N，N-二甲基甲酰胺。
4.根据权利要求2或3所述的制备方法，其特征在于，步骤1)所述加热处理的温度为18～60℃，时间为15～26h，所述加热处理在搅拌条件下进行。
5.根据权利要求4所述的制备方法，其特征在于，步骤1)所述超声处理的温度为18～60℃，时间为0.3～1.5h，超声处理的频率为30～50kHz。
6.根据权利要求5所述的制备方法，其特征在于，步骤2)所述静电纺丝中，针头内径为0.3～0.5mm，针头外径为0.6～0.8mm；推注速度为0.4～1.5mL/h，针头和接收滚筒之间的距离为12～20cm；针头平移速度为280～320mm/min，针头平移行程为480～520mm。
7.根据权利要求6所述的制备方法，其特征在于，步骤2)所述静电纺丝的时间为5～60min，温度为20～30℃，电压为12～18kV。
8.根据权利要求6或7所述的制备方法，其特征在于，步骤3)所述交联剂为N，N-亚甲基双丙烯酰胺，所述交联剂和单体的质量比为1∶94～104；所述单体与亲水层原料中的C组分的种类和质量均相同；所述单体在水凝胶溶液中的质量浓度为9.4～10.4％；所述光引发剂为2-羟基-2-甲基-1-苯基-1-丙酮，所述光引发剂在水凝胶溶液中的质量浓度为1～5％；所述氯化钠溶液中，氯化钠的摩尔浓度为0.5～1.5mol/L。
9.根据权利要求8所述的制备方法，其特征在于，步骤3)所述交联反应在紫外光下进行，所述紫外光的波长为350～380nm，所述交联反应的时间为10～30min。
10.权利要求1所述的复合纤维膜在单向水运输中的应用。
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