CN105879700A - 一种晶须掺混复合反渗透膜的制备方法 - Google Patents
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Abstract
本发明公开了一种晶须掺混和聚乙烯醇(PVA)预处理制备复合反渗透膜的方法。其主要技术特性在于：将晶须加入聚合物铸膜液中，以无纺布为支撑层采用非溶剂相转化法制备晶须掺混基膜，然后用含有PVA和离子液体放水溶液预涂基膜表面，最后在经过预处理的基膜表面进行间苯二胺和均苯三甲酰氯的原位界面聚合，得到复合反渗透膜。采用此方法制备的复合反渗透膜采具有极高的机械强度；其功能层更为致密、均匀，与基膜结合的更紧密，不易脱落；复合反渗透膜的截留率更高，使用寿命延长。
Description
技术领域
本发明涉及一种反渗透膜的制备方法，具体为晶须掺混和固定化处理制备复合反渗透膜的方法，属于分离膜制造领域。
背景技术
反渗透是水质净化和脱盐的较优方法，广泛用于苦咸水淡化、海水淡化、水质净化、食品饮料、医疗制药、石油化工、锅炉补给等领域。目前，商品反渗透膜均为平板复合膜，是由基膜和其表面的脱盐层组成。基膜是以无纺布为底基的超滤膜，起增加机械强度的作用；脱盐层一般是通过在支撑膜表面的原位界面聚合得到的超薄致密层。在反渗透膜的生产过程中，基膜表面的亲水性影响脱盐层的均匀度和致密性，从而影响反渗透膜的脱盐率和使用寿命。
晶须是一种新型增强填料。晶须以单晶形式生长成的一种纤维，其直径非常小(微米数量级)，具有高强度、高模量和高伸长率等优点。晶须的强度远高于其他短切纤维，主要用作复合材料的增强体，用于制造高强度复合材料。
发明内容
为了改善现有反渗透膜的脱盐率、延长其使用寿命，本发明公开一种晶须掺混和固定化处理制备复合反渗透膜的方法，提出了一种新型反渗透复合膜的制备工艺。主要制膜步骤如下：
(1)晶须-聚合物混合溶液的制备
将聚合物、有机溶剂和制孔剂按一定比例配制成聚合物铸膜液；将晶须加入铸膜液中，搅拌均匀后静置脱泡。
(2)复合反渗透膜基膜的制备
将含有晶须的铸膜液涂于无纺布上，再浸入凝固浴中使聚合物分相，用去离子水多次冲洗，即采用非溶剂相转化法得到复合反渗透膜的基膜。
(3)复合反渗透膜基膜的预处理
基膜晾干后，在其表面涂敷含有一定浓度的PVA和离子液体的水溶液，干燥。
(4)复合反渗透膜的制备
在预处理好的基膜表面涂敷间苯二胺水溶液，恒温恒湿环境下干燥后；再涂敷均苯三甲酰氯的正己烷溶液，制得复合反渗透膜。
PVA和离子液体可降低基膜的表面张力，增加间苯二胺水溶液在膜表面的附着力，使间苯二胺在膜表面分布的更为均匀。另外，聚乙烯醇(PVA)含有大量羟基，可与某些晶须结合形成离子键，离子键的形成增加了PVA与基膜的结合牢度。采用PVA和离子液体预处理后，反渗透膜的脱盐层更为致密、均匀，截留率也更高。
所述步骤(1)、(2)晶须是指碳化硅、碳化钽、氮化硅、碳纤维、纳米纤维素晶须中的一种或几种，优选为：碳化硅晶须。聚合物是指聚砜、聚醚砜和聚偏氟乙烯中的一种或几种。
所述步骤(1)中，晶须的浓度为0.2wt％-10wt％。
所述步骤(3)中，离子液体的浓度为1wt％-10wt％；PVA的浓度为1wt％-10wt％。
所述步骤(4)中，复合反渗透膜致密层由间苯二胺和均苯三甲酰氯经原位界面聚合而成。
与传统反渗透膜相比，其优点是：
(1)晶须的加入增强了复合反渗透膜的机械强度；
(2)基膜经过PVA和离子液体预浸液处理后，基膜表面的亲水性增加，从而使界面聚合后的脱盐层更为致密、均匀，复合反渗透膜的截留率更高。
附图说明
附图(图1)为本发明复合反渗透膜的结构示意图。其中，1为无纺布支撑层，2为聚合物层，3为脱盐层，4为晶须。
具体实施方式
下面结合实施例对本发明方案做进一步具体说明。
实施例1
将浓度为0.2wt％的碳化硅加入聚合物铸膜液中，溶解脱泡后，制得含有晶须的铸膜液；将此铸膜液均匀地涂于无纺布上，采用非溶剂相转化法制得复合反渗透膜基膜；在基膜表面预涂含有5wt％的离子液体和1wt％PVA的水溶液，干燥后，涂敷间苯二胺水溶液；干燥后，再在表面涂敷均苯三甲酰氯的正己烷溶液，制得复合反渗透膜。
实施例2
将浓度为1wt％的氮化硅加入聚合物铸膜液中，溶解脱泡后，制得含有晶须的铸膜液；将此铸膜液均匀地涂于无纺布上，采用非溶剂相转化法制得复合反渗透膜基膜；在基膜表面预涂含有10wt％的离子液体和5wt％PVA的水溶液，干燥后，涂敷间苯二胺水溶液；干燥后，再在表面涂敷均苯三甲酰氯的正己烷溶液，制得复合反渗透膜。
实施例3
将浓度为10wt％的纳米纤维素晶须加入聚合物铸膜液中，溶解脱泡后，制得含有晶须的铸膜液；将此铸膜液均匀地涂于无纺布上，采用非溶剂相转化法制得复合反渗透膜基膜；在基膜表面预涂含有5wt％的离子液体和10wt％PVA的水溶液，干燥后，涂敷间苯二胺水溶液；干燥后，再在表面涂敷均苯三甲酰氯的正己烷溶液，制得复合反渗透膜。
对照组1
将聚合物铸膜液均匀地涂于无纺布上，采用非溶剂相转化法制得复合反渗透膜基膜；干燥后，涂敷间苯二胺水溶液；干燥后，再在表面涂敷均苯三甲酰氯的正己烷溶液，制得复合反渗透膜。
取实施例1-3和对照组1制得的相同面积的膜片，测试：(1)测试水通量，(2)测试氯化钠截留率，(3)测试抗张强度。截留性能测试时，操作压力为1.55MPa，测试系统温度为25℃。实验结果见表1。
表1 膜片的水通量、截留率和抗张强度
由表1可知，在同样的测试条件下，以本发明方法实施例和对照组制得的复合反渗透膜的膜片，其测试水通量变化率是20.73％，氯化钠截留率变化率是1.14％，抗张强度变化率是8.17％。以上结果说明本发明制备的晶须掺混和反渗透膜基膜表面经预浸液处理制备复合反渗透膜优于未添加晶须和基膜未进行预浸液处理制备的复合反渗透膜，可替代未添加晶须和基膜未进行预浸液处理制备的反渗透膜使用。
Claims (4)
1.一种晶须掺混和聚乙烯醇(PVA)预处理制备复合反渗透膜的方法，该方法是将晶须加入聚合物铸膜液中，以无纺布为支撑层，采用非溶剂相转化法制备晶须掺混基膜，用含有1wt％-10wt％的PVA和1wt％-10wt％的离子液体水溶液预涂基膜表面，然后在预处理后基膜表面进行间苯二胺和均苯三甲酰氯原位界面聚合，制得复合反渗透膜。
2.如权利要求1所述的一种晶须掺混复合反渗透膜，其特征在于基膜中含有晶须。晶须是指碳化硅、碳化钽、氮化硅、碳纤维、纳米纤维素晶须中的一种或几种，优选为：碳化硅晶须。聚合物是指聚砜、聚醚砜和聚偏氟乙烯中的一种或几种。晶须的浓度为0.2wt％-10wt％。
3.如权利要求1和2所述，采用一种晶须掺混和PVA预处理制备复合反渗透膜的方法，其特征在于：用含有PVA和离子液体的水溶液预处理基膜表面。其中，PVA的浓度为1wt％-10wt％，离子液体的浓度为1wt％-10wt％。
4.如权利要求1和2所述，一种晶须掺混和PVA预处理制备复合反渗透膜的方法，其特征在于：复合反渗透膜致密层由间苯二胺和均苯三甲酰氯经原位界面聚合而成。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126850A (zh) * | 2017-05-23 | 2017-09-05 | 中国石油大学(华东) | 一种聚磺酰胺纳滤或反渗透复合膜及其制备方法 |
| CN111054214A (zh) * | 2018-10-16 | 2020-04-24 | 天津天元新材料科技有限公司 | 一种复合反渗透膜的制备方法 |
| CN111841346A (zh) * | 2020-07-21 | 2020-10-30 | 浙江奥氏环境科技有限公司 | 一种反渗透膜的制备方法 |
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