CN116159446B - 一种分子筛/聚酰胺混合基质膜 - Google Patents
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 55
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000004952 Polyamide Substances 0.000 title claims abstract description 28
- 229920002647 polyamide Polymers 0.000 title claims abstract description 28
- 239000004941 mixed matrix membrane Substances 0.000 title claims abstract description 12
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 16
- 229920002492 poly(sulfone) Polymers 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 238000001728 nano-filtration Methods 0.000 claims description 3
- 238000001223 reverse osmosis Methods 0.000 claims description 3
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
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- 239000012528 membrane Substances 0.000 abstract description 32
- 230000004907 flux Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 239000012071 phase Substances 0.000 description 29
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 14
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 description 14
- 238000007598 dipping method Methods 0.000 description 14
- 229940018564 m-phenylenediamine Drugs 0.000 description 14
- 239000011159 matrix material Substances 0.000 description 10
- 238000012695 Interfacial polymerization Methods 0.000 description 9
- 239000008346 aqueous phase Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000007654 immersion Methods 0.000 description 7
- 238000000108 ultra-filtration Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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Abstract
本发明提供了一种分子筛共混的聚酰胺混合基膜,其通过双分子筛的掺杂使得混合基质膜中的分子筛掺杂量得到提升,且整个膜材料形成不亲水‑低亲水‑高亲水的三层结构,提升了混合基质膜的通量。
Description
技术领域
本发明涉及一种膜材料,具体涉及一种分子筛共混的聚酰胺混合基膜。
技术背景
聚酰胺类的反渗透膜及纳滤膜在海水淡化领域得到广泛研究和应用,其一般通过界面聚合形成。在聚酰胺膜中添加无机颗粒是改进膜性能的重要研究方向,目前热门的掺杂物主要是分子筛、二氧化硅、碳纳米管、二氧化钛、纳米银颗粒等。其中分子筛其具有规整的孔道结构便于水分子的通过使其成为较为集中的聚酰胺掺杂研究热点。
其中,对于聚酰胺膜混合基质膜而言,分子筛掺杂量的增加可以大幅度提升膜的通量水平,但是当分子筛掺杂量提升的同时,小粒径的分子筛颗粒之间便会相互团聚,从而造成孔缺陷,反而降低了膜的分离水平,所以膜通量水平和膜分离水平导致了分子筛的掺杂量一般不会太高,一般而言,水相或油相中分子筛的掺杂量不会高于0.5wt%。另一方面,为提升膜的亲水性,现有技术公开了在基底层中掺杂无机颗粒以提高膜的亲水性,但是聚酰胺膜在应用过程中一般是基底层面向原水侧,基底层中亲水性的提高减缓了水分子在贯穿膜的驱动力。因此,如何改良聚酰胺混合基质膜以最大程度提升膜的通量是一个亟待解决的技术问题。
针对上述技术问题,本发明提供了一种分子筛共混的聚酰胺混合基膜,其通过双分子筛的掺杂使得混合基质膜中的分子筛掺杂量得到提升,且整个膜材料形成不亲水-低亲水-高亲水的三层结构,提升了混合基质膜的通量。
为实现上述目的,本发明提供了一种分子筛/聚酰胺混合基质膜,其包括基底和依附在基底上的聚酰胺层,所述聚酰胺层含有嵌在基底层上的介孔分子筛和贯穿在聚酰胺层的微孔分子筛。
作为优选技术方案,所述介孔分子筛为MCM-41、MCM-48或SBA-15分子筛,硅铝比为4-50,粒径为200-500nm。
作为优选技术方案,所述介孔分子筛经过官能团、离子液体或聚合物修饰。
作为优选技术方案,所述微孔分子筛为NaA分子筛,硅铝比为1,粒径为50-800nm。
本发明还提供了一种分子筛/聚酰胺混合基质膜的制备方法,其分别将介孔分子筛和微孔分子筛与聚合形成聚酰胺层的水相单体溶液、油相单体溶液混合,并将基底分别与所述水相单体溶液和油相单体溶液接触以聚合形成聚酰胺层。
作为优选技术方案,所述的基底为纤维素、聚酯、聚丙烯腈、聚砜、聚偏氟乙烯或聚四氟乙烯中的一种。
作为优选技术方案,所述水相溶液中介孔介孔分子筛的质量分数为0.001-0.5%。
作为优选技术方案,所述油相溶液中微孔介孔分子筛的质量分数为0.002-1%。
作为优选技术方案,基底与所述水相单体溶液接触后静置2-5分钟、
本发明制备的混合基质膜在纳滤、反渗透水处理中的应用。
本发明利用分子筛在水相、油相中混合形成的混合基质膜中分子筛与聚酰胺层位置的不同,创造性的提出将将介孔分子筛和微孔分子筛与聚合形成聚酰胺层的水相单体溶液、油相单体溶液混合,从而使得界面聚合过程中水相单体溶液中介孔分子筛嵌在基底上,而油相单体溶液中的微孔分子筛贯穿在聚酰胺层中,从而形成互补干扰的双分子筛层结构,显著提升了混合基质层中的通量。而且,基底、介孔分子筛和微孔分子筛的亲水性依次提高,使得整个膜材料形成不亲水-低亲水-高亲水的三层结构,且介孔分子筛的孔径也大于微孔分子筛,更利于水分子的通过,提升了水分子在贯穿膜结构过程中的驱动力。
具体实施方式
实施例1
(1)将硅铝比为50的Al-MCM-41混合于含有间苯二胺的水相单体溶液中,溶液中Al-MCM-41含量为0.2wt%,间苯二胺含量为0.5wt%;将硅铝比为1的NaA混合于含有均苯三甲酰氯的油相单体溶液中,溶液中NaA含量为0.5wt%,均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置2min;
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
对比例1
(1)将硅铝比为50的Al-MCM-41混合于含有间苯二胺的水相单体溶液中,溶液中Al-MCM-41含量为0.7wt%,间苯二胺含量为0.5wt%;制备含有均苯三甲酰氯的油相单体溶液中,溶液中均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置2min;
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
对比例2
(1)制备含有间苯二胺的水相单体溶液中,溶液中间苯二胺含量为0.5wt%;将硅铝比为1的NaA混合于含有均苯三甲酰氯的油相单体溶液中,溶液中NaA含量为0.7wt%,均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置2min;
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
对比例3
(1)将硅铝比为1的NaA混合于含有间苯二胺的水相单体溶液中,溶液中NaA含量为0.2wt%,间苯二胺含量为0.5wt%;将硅铝比为1的NaA混合于含有均苯三甲酰氯的油相单体溶液中,溶液中NaA含量为0.5wt%,均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置2min;
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
对比例4:
(1)将硅铝比为50的Al-MCM-41混合于含有间苯二胺的水相单体溶液中,溶液中Al-MCM-41含量为0.2wt%,间苯二胺含量为0.5wt%;将硅铝比为50的Al-MCM-41混合于含有均苯三甲酰氯的油相单体溶液中,溶液中Al-MCM-41含量为0.5wt%,均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置2min;
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
对比例5
(1)将硅铝比为1的NaA混合于含有间苯二胺的水相单体溶液中,溶液中NaA含量为0.2wt%,间苯二胺含量为0.5wt%;将硅铝比为50的Al-MCM-41混合于含有均苯三甲酰氯的油相单体溶液中,溶液中Al-MCM-41含量为0.5wt%,均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置2min;
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
对比例6
(1)将硅铝比为50的Al-MCM-41混合于含有间苯二胺的水相单体溶液中,溶液中Al-MCM-41含量为0.2wt%,间苯二胺含量为0.5wt%;将硅铝比为1的NaA混合于含有均苯三甲酰氯的油相单体溶液中,溶液中NaA含量为0.5wt%,均苯三甲酰氯含量为1wt%;
(2)将自购的聚砜平板超滤膜作为基底先浸入水相单体溶液中,浸渍时间为180s,浸渍结束取出后将基底静置10s后马上进行步骤(3);
(3)然后将基底继续浸渍于油相单体溶液中,继续浸渍120s以实现界面聚合,浸渍结束后将膜取出置于60℃烘箱内干燥10min形成混合基质膜。
将上述混合基质膜用2000ppm的氯化钠水溶液在1.5MPa压力、25℃下测试渗透性能,结果如下表所示
表1不同混合基质膜的渗透性能参数
尽管已经结合实施方案说明和描述了本发明,但对于本领域的技术人员将显而易见的是,在不背离如所附权利要求限定的本发明的精神和范围的情况下,可以进行各种修改和变化。
Claims (9)
1.一种分子筛/聚酰胺混合基质膜在纳滤、反渗透水处理中的应用,所述分子筛/聚酰胺混合基质膜包括基底和依附在基底上的聚酰胺层,所述聚酰胺层含有嵌在基底层上的介孔分子筛和贯穿在聚酰胺层的微孔分子筛;所述分子筛/聚酰胺混合基质膜是通过如下方法制备:分别将介孔分子筛和微孔分子筛与聚合形成聚酰胺层的水相单体溶液、油相单体溶液混合,并将基底分别与所述水相单体溶液和油相单体溶液接触以聚合形成聚酰胺层;所述介孔分子筛硅铝比为4-50,所述微孔分子筛硅铝比为1。
2.根据权利要求1所述的应用,其特征在于所述介孔分子筛为MCM-41、MCM-48或SBA-15分子筛。
3.根据权利要求1所述的应用,其特征在于所述微孔分子筛为NaA分子筛。
4.根据权利要求1所述的应用,其特征在于所述介孔分子筛粒径为200-500nm。
5.根据权利要求1所述的应用,其特征在于所述介孔分子筛经过官能团、离子液体或聚合物修饰;粒径为50-800nm。
6.根据权利要求5所述的应用,其特征在于所述的基底为纤维素、聚酯、聚丙烯腈、聚砜、聚偏氟乙烯或聚四氟乙烯中的一种。
7.根据权利要求5所述的应用,其特征在于所述水相溶液中介孔介孔分子筛的质量分数为0.001-0.5%。
8.根据权利要求5所述的应用,其特征在于所述油相溶液中微孔介孔分子筛的质量分数为0.002-1%。
9.根据权利要求5所述的应用,其特征在于基底与所述水相单体溶液接触后静置2-5分钟。
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