CN112742222A - 一种pvc脂肪族两性离子交换膜的制备方法 - Google Patents
一种pvc脂肪族两性离子交换膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种两性离子交换膜的制备方法及其应用。所述分离膜按照如下方法制备:将聚氯乙烯(PVC)溶解在N,N‑二甲基乙酰胺溶解在圆底烧瓶中混合均匀,获得制备基膜的溶液;使用循环水真空泵对获得的溶液进行抽滤,除去溶液中掺杂的不溶性杂质;将抽滤后的溶液进行抽真空,然后将溶液涂覆于玻璃板上,置于平板加热器上进行烘干,获得聚氯乙烯基膜;将基膜浸泡在三亚乙基四胺中8‑24小时,取出,用去离子水冲洗,获得季铵化膜;将季铵化膜浸泡到3‑氯‑2‑羟基丙磺酸钠溶液中,浸泡12小时,取出烘干,获得两性离子交换分离膜。本发明所需原料易得,价格低廉,制备过程简单,仅需要简单的浸泡,省去了现有技术的电沉积、层层自组装复杂过程以及采用静电吸附改性膜表面的改性层脱落的问题。
Description
技术领域
本发明属于分离膜技术领域,涉及一种PVC脂肪族两性阴离子膜的制备方法。
背景技术
近几十年来,电渗析(ED)技术已广泛应用于海水淡化水的回收。离子交换膜(AEMs)作为电渗析装置的核心部件,在决定海水淡化性能方面起着重要作用。近年来,聚砜、聚醚砜、聚苯乙烯等聚合物作为膜合成的基材得到了广泛的研究。但离子膜的性能仍存在一些需要解决的问题,如价格昂贵、性能不稳定等导致膜的运行性能不良。因此,开发低成本、稳定性强的离子膜是ED发展过程中的一个重要挑战。其中,一种切实可行的低成本离子膜的制备方法就是将功能单体接枝到低成本聚合物的主链上制备离子交换膜。此外,芳香族的AEMs由于其主链上固有的芳香烃与疏水性,在ED过程中有机污染物易附着在膜表面或其基体内部,导致膜过滤阻力增加及膜寿命降低。本发明所述的两性离子交换膜是一种既含有碱性基团又含有酸性基团的离子交换膜,该离子交换膜表面的电荷性质可以根据其所处理溶液性质的改变而改变,因为其既能够用作阳离子交换膜又能够用作阴离子交换膜,所以两***换膜具有可调性。
Journal of Membrane Science(2016,490,301-310)提出了一种利用聚多巴胺改性商业阴膜的方法制备出一种两性离子交换膜。由于多巴胺在空气环境中就会转化为聚多巴胺,聚多巴胺具有很好的吸附粘附作用而有两性的性质,由SO4 2-/Cl-体系的电渗析实验,可以实现较好的多价离子选择性分离。但该方法面临着改性层脱落,以及原料较贵的问题,不适合未来的膜制备的大范围的工业化推广。
Electrochimica Acta(2015,174,1113-1121)Tang etal采用两步法分别对聚氯乙烯进行氯甲基化以及胺基化制备了一种聚氯乙烯两性离子交换膜,离子交换通量可达3.6meq/g,但离子膜制备过程复杂;Wang etal.以十二烷基苯磺酸钠(SDBS)、腐殖酸钠和牛血清白蛋白(BAS)为污染物典型代表,考察了污染物对不同离子交换膜在ED运行过程中的污染情况,结果表明膜表面有机物的粘附程度主要决定于膜表面亲疏水性以及与膜表面与污染物的之间的静电斥力、π-π共轭作用强度,膜表面亲水性越强,抗污染能力越好,脂肪族离子膜的抗污染能力优于芳香族离子膜。
本发明利用成本低廉、易得的原料以及简单的手段便可以充分满足膜法离子分离的要求,对于今后的工业化有很大的指导意义。
发明内容
本发明的目的是提供一种PVC脂肪族两性离子交换膜的制备方法,解决了现有技术中存在的芳香族离子膜的易污染性能以及降低工艺成本的问题。
本发明采用的技术方案是:
本发明提供一种PVC脂肪族两性离子交换膜,所述分离膜按照如下方法制备:
(1)将聚氯乙烯与N,N-二甲基乙酰胺混合均匀,获得制备基膜的溶液。
(2)将步骤(1)所得溶液利用循环水真空泵进行抽滤,去除溶液中的不溶性杂质。
(3)将步骤(2)所得溶液置于真空箱中进行抽真空除泡。
(4)将步骤(3)所得的溶液涂覆于玻璃板上,置于平板加热器上进行烘干(优选烘干温度为60℃,时间为8h),在所述的玻璃板上获得聚氯乙烯基膜。
(5)室温下,取下步骤(4)玻璃板上获得的膜,浸泡在质量浓度50-100%(优选70%)的三亚乙基四胺溶液中8-24h,取出,去离子水冲洗,获得季铵化膜。
(6)将步骤(5)所获得的季铵化后的膜浸泡到3-氯-2羟基丙磺酸钠溶液中,50-90℃(优选60℃)浸泡8-48h(优选12h),取出烘干,获得一种PVC脂肪族两性离子交换膜。
进一步,步骤(4)中所述涂覆厚度为60-120μm,优选80μm。
进一步,步骤(4)中所述烘干温度为60℃,时间为8h。
进一步,步骤(5)中所述三亚乙基四胺的质量浓度优选为70%。
与当前技术相比本发明的有益效果在于:本发明制备过程简单,仅需要简单的浸泡,省去了现有技术的电沉积、层层自组装复杂过程以及采用静电吸附改性膜表面的改性层脱落的问题。同时,膜基本性能指标如离子交换容量,机械强度等都与未改性之前相差无几。
附图说明
图1是本发明膜阻测试装置图;
图2是本发明离子交换膜的傅里叶红外测试图;
图3是本发明离子交换膜的电镜(SEM)扫描图;
图4是本发明离子交换膜的膜阻(Rn)以及离子通量(IEC)变化图;
图5是本发明作为阴离子交换膜的电渗析测试图;
图6是本发明作为阳离子交换膜的电渗析测试图;
图7是本发明离子交换膜的抗污染实验膜两侧电压趋势图;
图8是本发明离子交换膜的膜电流效率变化趋势图;
具体实施方式
说明本发明方法完整的步骤:
实施例1
将PVC粉末加入到N,N-二甲基乙酰胺中,加热到60℃,溶解得到溶液,将PVC溶液进行真空脱泡,倾倒在玻璃板上,用厚度为80μm的刮刀刮涂成湿膜,于60℃平板加热器上干燥蒸发出溶剂,得到PVC膜。取下PVC膜剪裁成合适的大小并浸泡在60℃的100mL70%三亚乙基四胺水溶液中,分别反应2h以后取出两张膜,一张浸泡在0.5molNaCl中,另一张浸泡在3-氯-2-羟基丙磺酸钠溶液中12h得到离子交换膜Q-1。
实施例2
将上述实例1中在三亚乙基四胺的浸泡时间改为3h,其他步骤不变,得到离子交换膜Q-2。
实施例3
将上述实例1中在三亚乙基四胺的浸泡时间改为4h,其他步骤不变,得到离子交换膜Q-3。
下面结合附图和具体实施方式对本发明进行详细说明:
从图2的SEM图中可以看出QPVC膜层表面与横断面致密均一,无孔洞裂纹。对实施例中制备的QPVC离子膜进行膜阻(Rn)红外以及吸水率等的考察,如图4所示,随着PVC膜在三乙烯四胺溶液中浸泡时间的延长IEC逐渐增加,Rn逐渐降低。这是由于浸泡时间越长,接枝到PVC主链上的季胺盐官能团越多,离子交换通量增加,且亲水性越强的季胺盐能够提供的更多的离子传输通道,使膜面电阻降低。为了考察实施例合成的QPVC膜的抗污染效果,进行污染实验,如图2所示,电极为银电极,污染实验膜面积为7.065cm2,阳离子膜为德国FKB阳膜,以安徽合肥科佳高新技术有限公司提供的商业膜JAM-II-05为离子膜参考进行对比,实验以0.8g/L十二烷基苯磺酸钠为典型污染物代表,NaCl电解液初始浓度为0.05mol/L,淡室中加入SDBS污染物,浓度为0.8g/L,设定电流密度为15mA/cm2。采用Ag-AgCl电极测量膜两侧电压随时间的变化情况。
如图7所示,与商业膜相比,Q-2和Q-3离子膜两侧电压随时间的变化较小,在720min内无明显的转变时间出现,呈现出良好的抗污染能力。对实施例1合成的阴离子膜进行电渗析实验,电极为银电极,电渗析实验膜面积7.05cm2,阳膜都为为德国FKB阳膜,以以安徽合肥科佳高新技术有限公司提供的商业膜JAM-II-05为参考对比,原液初始浓度为0.5mol/LNaCl,中加入0.8mol/LSDBS,以0.3g/LNa2SO4为极液,电流维持在0.3A,进行电渗析实验,图5-6可以看出,在淡室存在污染物的情况下,商业膜JAM-II-05经电渗析200min后,淡室中电导率下降24.69%,说明电渗析过程中离子膜受到严重污染;而QPVC膜仅下降9.4%,说明该离子膜具有优异的抗污染性能。
当测试两性离子交换膜的阴离子交换膜性能时,由图5可以看出浸泡三亚乙基四胺后与3-氯-2-羟基丙磺酸钠反应12h后的膜电导率-时间的变化趋势,三种膜在其进料与出料两侧的溶液电导率变化都比较大,其分离效果较好。且一定程度随着浸泡三亚乙基四氨时间的加长而效果增强,主要是随PVC与三亚乙基四氨反应时间的增加使其反应程度也不断提高导致连接到PVC膜上的氨基在不断增加进而导致随着浸泡三亚乙基四氨时间的加长而分离效果增强。
图8所示为本次实验所制备的浸泡在三亚乙基四胺中的三份膜样的电流效率。其中浸泡时间为2h的膜其电流效率为11.99%,浸泡时间为3h的膜其电流效率为30.05%,浸泡时间为4h的膜其电流效率为34.05%,由图8可知,三种膜的电流效率随浸泡时间的加长电流效率随之上升,主要因随浸泡时间的加长,离子膜的膜阻变小,电流效率随之上升,因此,本发明对于离子交换膜应用的节能具有重要意义。
Claims (7)
1.一种PVC脂肪族两性离子交换膜,所述分离膜按如下方法制备:
(1)将聚氯乙烯与N,N-二甲基乙酰胺混合均匀,获得制备基膜的溶液。
(2)将步骤(1)所得溶液利用循环水真空泵进行抽滤,去除溶液中的不溶性杂质。
(3)将步骤(2)所得溶液置于真空箱中进行抽真空除泡。
(4)将步骤(3)所得的溶液涂覆于玻璃板上,置于平板加热器上进行烘干,在所述的玻璃板上获得聚氯乙烯基膜。
(5)室温下,取下步骤(4)玻璃板上获得的膜,浸泡在质量浓度50-100%的三亚乙基四胺溶液中8-24h,取出,去离子水冲洗,获得季铵化膜。
(6)将步骤(5)所获得的季铵化后的膜浸泡到3-氯-2羟基丙磺酸钠溶液中,50-90℃浸泡8-48h,取出烘干,获得一种PVC脂肪族两性离子交换膜。
2.如权利要求1所述PVC脂肪族两性离子交换膜,其特征在于步骤(1)所述加热溶解得到浓度为5-50wt%的溶液。
3.如权利要求1所述PVC脂肪族两性离子交换膜,其特征在于步骤(4)所述溶液涂覆厚度为60-120μm。
4.如权利要求1所述PVC脂肪族两性离子交换膜,其特征在于步骤(4)所述烘干温度为60℃,加热时间为6-12h。
5.如权利要求1所述PVC脂肪族两性离子交换膜,其特征在于步骤(5)所述将膜浸泡在质量浓度50-100%的三亚乙基四胺溶液中8-48h,取出,用去离子水冲洗干净,获得季铵化膜。
6.如权利要求1所述PVC脂肪族两性离子交换膜,其特征在于步骤(6)所述将所获得的季铵化后的膜浸泡到3-氯-2羟基丙磺酸钠溶液中,50-90℃浸泡8-48h,取出烘干,获得一种PVC脂肪族两性离子交换膜。
7.一种权利要求1所述所述PVC脂肪族两性离子交换膜在水处理中的应用。
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CN114405286A (zh) * | 2021-12-08 | 2022-04-29 | 华东理工大学 | 一种离子交联型两性离子交换膜、制备方法及其在选择性电渗析中的用途 |
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CN113998762A (zh) * | 2021-11-04 | 2022-02-01 | 广东工业大学 | 一种带磁体的电渗析污水处理装置和电渗析污水处理方法 |
CN113998762B (zh) * | 2021-11-04 | 2023-02-28 | 广东工业大学 | 一种带磁体的电渗析污水处理装置和电渗析污水处理方法 |
CN114405286A (zh) * | 2021-12-08 | 2022-04-29 | 华东理工大学 | 一种离子交联型两性离子交换膜、制备方法及其在选择性电渗析中的用途 |
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