CN108385273A - 一种亲/疏水性可调控的薄膜静电纺丝制备方法 - Google Patents
一种亲/疏水性可调控的薄膜静电纺丝制备方法 Download PDFInfo
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Abstract
本发明涉及一种亲/疏水性可调控的薄膜静电纺丝制备方法。将聚合物/偶极子的混合溶液利用静电纺丝技术制备高质量的复合薄膜,通过调控静电纺丝工艺中的电场强度和方向,来精确控制偶极子在薄膜中的取向程度和旋转方向,从而精确调控了制备的复合薄膜表面的亲疏水性能。本发明为亲水/疏水薄膜的制备提供了一种简单有效的制备方法。
Description
技术领域
本发明涉及高分子材料领域,特别涉及一种亲水/疏水性可调控的聚合物薄膜的静电纺丝制备方法
背景技术
随着人们对固体的表面性能越来越关注,润湿性就是其中最大的关注点,而固体表面疏水性及接触角大于150°的超疏水表面更是研究人员的关注点。这种超疏水界面材料可以用于石油管道的输送;用于微量注射器针尖;防水和防污处理;在远洋轮船的防污、防腐等方面有广泛的应用。经由前人的各方面研究表明超疏水表面可由两种方式来实现,一是微观表面结构,即表面粗糙度,即仿生方法,二是在表面修饰低表面能物质。经过长时间的研究,目前有很多制备超疏水界面的方法,例如刻蚀法,其包括等离子体刻蚀,光刻蚀,化学刻蚀法(CN103409754A);溶胶-凝胶法(CN103102082A);模板法(CN103881120A)等。但是现如今存在的这些方法有许多的弊端,例如其操作方式繁琐复杂,且传统的方法制备的材料其接触角角度固定,导致其应用领域受到一定的限制,由此,如果能发明一种薄膜亲疏水性可精确调控的制备方法一定有广阔的应用领域和研究价值。
发明内容
本发明的目的在于提供一种亲/疏水性能可调控的薄膜材料制备方法。本发明所用原料均是常规材料,均可通过商用渠道获得。
本发明的一种亲水/疏水性能可调控的聚合物薄膜的静电纺丝制备方法包括以下步骤:(1)纺丝液的制备,将聚合物偶极分子聚合物溶解在有机溶剂中。(2)复合膜的制备,将其纺丝液吸入静电纺丝装置中,在一定电压下进行静电纺丝法制备薄膜。
步骤(1)中所述的聚合物可以是聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯、聚乙烯吡咯烷酮、聚苯乙烯、聚甲醛、聚碳酸酯,聚酯,聚丙乙烯、尼龙610等聚酰胺类,非极性聚烯烃类高分子聚合物等。
步骤(1)中所述聚合物的分子量在5000~2000000,优选为15000~1500000。
步骤(1)中所述共轭偶极分子聚合物是一端带有疏水基团且带有偶极子结构的共轭聚合物。符合其结构的分子式如下:
步骤(1)中所述静电纺丝工艺中的电压在2000.00~50000.00伏,最优选为5000~23000伏。
步骤(1)中所述溶剂可以是乙酸丁酯、乙酸乙酯、三聚甲烷、二甲基甲酰胺、氯苯、甲苯、乙醇、乙醚等有机溶剂。
步骤(1)中所述带有偶极子结构共轭高分子聚合物质量浓度在0.01~10.0%,优选为0.05~0.50%。
步骤(1)中所述的聚合物浓度可以是0.50%-30.00%,最优选为1.00~5.00%。
本发明是利用简单的静电纺丝技术,制备出聚合物/共轭偶极子复合膜,利用偶极子聚合物的特殊结构来实现对薄膜疏水性能的精确调控。本发明的复合膜材料可在常规的疏水材料的应用领域上进行调控其疏水性能来实现扩大其应用领域范围的效果。
本发明的方法与现有的技术相比创新点在于:(1)与常用的刻蚀法,溶胶-凝胶法及模板法相比本发明采用的静电纺丝技术,设备价格经济,工艺简单,适用范围广泛。(2)本发明思想新颖,通过电场对共轭偶极子的极化作用,利用偶极子在电场下的一致取向行为,亲水基团/疏水基团向薄膜表面取向,实现了复合薄膜表面亲疏水性能的有效精确调控。
附图说明
图1:本发明的静电纺丝方法实验设备装置图。1,高压电源;2,注射泵;3,接收装置;4,注射器。
图2:本发明实施例1中制备的PMMA/DR1复合薄膜的接触角数据曲线图。
图3:本发明实施例2中制备的POM/DR19复合薄膜的接触角数据曲线图。
图4:本发明实施例:3中制备的PVP/DR98复合薄膜的接触角数据曲线图。
图5:本发明实施例4中制备的PS/DR1复合薄膜的接触角数据曲线图。
图6:本发明实施例5中制备的PC/DR19复合薄膜的接触角数据曲线图。
图7:本发明实施例6中制备的PS/DR1复合薄膜的接触角数据曲线图。
图8:本发明实施例7中制备的PMMA/DR1复合薄膜的接触角数据曲线图。
图9本发明实施例中的DR1即分散红1结构式。
图10:本发明实施例中的DR19即分散红19结构式。
图11:本发明实施例中的DR98即分散红98结构式。
具体实施方法:为了更清楚地说明本发明,列举如下的实施例,但其对本发明的范围无任何限制。
实施例1:将聚甲基丙烯酸甲酯(poly(methylmethacrylate),PMMA)与分散红1(disperse red 1,DR1)溶解在乙酸丁酯(n-Butyl acetate,BTA)中,配制成含有1.1%聚甲基丙烯酸甲酯及0.075%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
将所制备的PMMA/DR1复合薄膜用接触角测试仪进行接触角的测试表征,图2为测试5次的结果。
实施例2:将聚甲醛(polyformaldehyde),POM,)与分散红19(disperse red 1,DR19)溶解在二甲基甲酰胺(N,N-Dimethylformamide,DMF)中,配制成含有1.5%聚甲醛及0.09%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
将所制备的POM/DR19复合薄膜用接触角测试仪进行接触角的测试表征,图3为测试5次的结果。
实施例3:将聚乙烯吡咯烷酮(poly(vinyl pyrrolidone),PVP)与分散红98(disperse red 1,DR98)溶解在氯苯(Chlorobenzene)中,配制成含有2.0%聚乙烯吡咯烷酮及0.10%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
将所制备的PVP/DR98复合薄膜用接触角测试仪进行接触角的测试表征,图4为测试5次的结果。
实施例4:将聚苯乙烯(poly(styrene),PS,Wm=8000)与分散红1(disperse red 1,DR1)溶解在甲苯(methylbenzene)中,配制成含有1.75%聚苯乙烯及0.08%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
将所制备的PS/DR1复合薄膜用接触角测试仪进行接触角的测试表征,图5为测试5次的结果。
实施例5:将聚碳酸酯(Poly(carbonate),PC,Wm=130000)分散红19(disperse1,DR19) 溶解在三氯甲烷(Trichloromethane)中,配制成含有3.0%聚碳酸酯及0.10%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
将所制备的PC/DR19复合薄膜用接触角测试仪进行接触角的测试表征,图6为测试5次的结果。
实施例6:将聚苯乙烯(poly(styrene),PS,Wm=8000)与分散红1(disperse red 1,DR1)溶解在甲苯(methylbenzene)中,配制成含有2.50%聚苯乙烯及0.09%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,将高压电源与的输出输入端调转在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
所制备的复合薄膜呈现亲水状态。
将所制备的PS/DR1复合薄膜用接触角测试仪进行接触角的测试表征,图7为测试5次的结果。
实施例7:将聚甲基丙烯酸甲酯(poly(methylmethacrylate),PMMA,Wm=8000)与分散红1(disperse red 1,DR1)溶解在乙酸丁酯(n-Butyl acetate,BTA)中,配制成含有1.1%聚甲基丙烯酸甲酯及0.075%DR1的纺丝溶液,将其放置于装有直径为0.6mm针头的静电纺丝装置中,设置固定喷射速度为0.3ml/h,给料距离为12cm,将高压电源的输出输入端调转,同样在不同的工作电场强度,在室温下进行静电纺丝。采用贴有锡纸的玻璃基底接收制备出的薄膜。
所制备的复合薄膜呈现亲水性能。
将所制备的PMMA/DR1复合薄膜用接触角测试仪进行接触角的测试表征,图8为测试5次的结果。
Claims (10)
1.一种亲/疏水性能可调控的薄膜静电纺丝制备方法。
2.其特征在于,包括以下步骤:
分别称取一定量的聚合物、偶极分子和溶剂,在同一个样品瓶中搅拌溶解。
3.将配置好的混合液采用静电纺丝工艺制备高质量的聚合物薄膜。
4.根据权利要求1所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述聚合物可以是聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯、聚乙烯吡咯烷酮、聚苯乙烯、聚甲醛、聚碳酸酯,聚酯,聚丙乙烯、尼龙610等聚酰胺类,非极性聚烯烃类高分子聚合物等。
5.根据权利要求1、2所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述聚合物的分子量在5000~2000000,优选为15000~1500000。
6.根据权利要求1所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述偶极分子为分子两端分别连接有亲水和疏水基团的发色团分子,更优选地如下几种结构的分子,其结构如下所示:
其中,M代表的共轭基团可以是:或-CH=CH-或-N=N-
D代表的基团可以是:-NO2或-CN
A代表的基团可以表达为:其中n可以为0、1、2或3
B代表的基团可以是:-OH或-HSO3。
7.根据权利要求1所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述静电纺丝工艺中的电压在2000.00~50000.00伏,最优选为5000~23000伏。
8.根据权利要求1所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述溶剂可以是乙酸丁酯、乙酸乙酯、三聚甲烷、二甲基甲酰胺、氯苯、甲苯、乙醇、乙醚等有机溶剂中的一种或多种。
9.根据权利要求1所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述带有偶极子结构共轭高分子质量浓度在0.01~10.0%,优选为0.05~0.50%。
10.根据权利要求1所述的一种亲/疏水性能可调控的聚合物/偶极子复合薄膜的静电纺丝制备方法,其特征在于:所述的聚合物浓度可以是0.50~30.00%,最优选为1.00~5.00%。
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