CN109157990B - 一种交联季铵化聚苯胺单价选择性阳离子交换膜及其制备方法 - Google Patents
一种交联季铵化聚苯胺单价选择性阳离子交换膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种交联季铵化聚苯胺单价选择性阳离子交换膜及其制备方法,所述交联季铵化聚苯胺单价选择性阳离子交换膜包括阳离子交换膜和在阳离子交换膜界面采用苯胺与氧化剂氧化聚合后,所得聚合物与季铵化试剂反应制得的季铵化聚苯胺,所述阳离子交换膜为基膜,季铵化聚苯胺为活性层。本发明中交联季铵化聚苯胺活性层,增加膜的致密性的同时改变基膜的表面荷电性,从而达到单价阳离子选择性分离。
Description
技术领域
本发明属于分离膜材料技术领域,涉及应用于水处理领域的膜材料研制,具体涉及一种交联季铵化聚苯胺单价选择性阳离子交换膜及其制备方法。
背景技术
随着工业进步和社会发展,水污染亦日趋严重,成了世界性的头号环境治理难题。水处理技术因此得到充分关注,按处理方法的不同,有生物化学法如活化污泥法,生物结层法,混合生物法等;物理化学法,如粒质过滤法,活化炭吸附法,化学沉淀法,膜滤/析法等。其中电渗析因其水回收率高、设备使用寿命长和运行成本低,同时对于非同性离子、甚至同性离子之间的分离具有不可代替的巨大优势成为水处理技术中的一个重要的分支。其中离子交换膜作为电渗析的核心组件尤为重要。
由于化工生产的进步以及水产品等级要求的提高,对于具有特殊分离能力的离子交换膜的需求也日益高涨。单价选择性离子交换膜是在离子交换膜的选择性基础上研究发展起来的,它能够将电性相同、电荷量不同的单价和多价离子进行选择性分离。其主要的分离原理就是利用孔径的筛分作用和静电排斥作用。其中,静电排斥就是利用在膜表面引入一层带有不同电荷的改性层,该改性层能对电解质溶液中的离子进行排斥,其所带电荷越多则排斥力越大。孔径的筛分是在膜表面引入一层致密的改性层使膜的结构更加致密,半径较大的离子就更加难以通过。
单价离子选择性电渗析技术在水处理领域拥有诸多方面的优势和巨大的应用前景,但国内外应用实例却相对较少。其主要发展瓶颈在于高性能单价选择性分离膜的缺乏。因此开发高性能单价阳离子选择性分离膜刻不容缓。
发明内容
针对现有技术存在的上述技术问题,本发明的目的在于提供一种交联季铵化聚苯胺单价选择性阳离子交换膜及其制备方法,它是基于交联季铵化聚苯胺活性层,增加膜的致密性的同时改变基膜的表面荷电性,进而制备出相应的单价阳离子选择性分离膜。
所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于包括基膜和位于基膜界面上的活性层,在界面采用苯胺单体与氧化剂氧化聚合后,所得聚合物与季铵化试剂反应制得的季铵化聚苯胺,所述季铵化聚苯胺为活性层;所述季铵化试剂的结构通式为X-(CH2)n-X,所述X为Cl、Br或I,n表示0~18的整数;所述季铵化试剂优选为1,2-二溴乙烷、1,3-二溴丙烷或1,4-二溴丁烷。
所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于氧化剂为氯化铁、过硫酸铵或重铬酸钾。
所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜的制备方法,其特征在于季铵化试剂溶于有机溶剂中作为季铵溶液,阳离子交换膜作为基膜;基膜表面用苯胺单体溶液浸泡后取出,使用滤纸吸干基膜表面的液体后,将所述基膜浸入氧化剂溶液中进行氧化聚合反应,苯胺单体与氧化剂在基膜表面发生氧化聚合反应生成聚苯胺活性层,再将基膜取出干燥后,放入季铵溶液中浸泡反应,最后将基膜从季铵溶液中取出并用纯净水反复冲洗,即得所述交联季铵化聚苯胺单价选择性阳离子交换膜。
所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜的制备方法,其特征在于氧化剂溶液中,溶剂为水,氧化剂的浓度为0.1~10 mol/L,所述氧化剂为氯化铁;所述基膜浸入氧化剂溶液中反应的时间为5~300min。
所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜的制备方法,其特征在于基膜表面用苯胺单体溶液浸泡的时间为5~300min;所述苯胺单体溶液中,溶剂为乙醇,苯胺单体的浓度为0.1~10 mol/L。
所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜的制备方法,其特征在于季铵溶液中,季铵化试剂的质量浓度为0.1~100 g/L,有机溶剂为乙醇;基膜放入季铵溶液中浸泡反应的时间为1~50h。
通过采用上述技术,与现有技术相比,本发明的有益效果如下:
本发明的交联季铵化聚苯胺单价选择性阳离子交换膜,它是通过在基膜表面使用苯胺与氧化剂氧化聚合然后与两端为卤代的不同链长烷烃反应生成的季铵化聚苯胺活性层制备得到;聚苯胺有着良好的稳定性,季铵化改性在提高了荷正电性的同时实现了聚苯胺之间的交联进一步增加了它的稳定性与致密性,保证了所制得的单价选择性阳离子交换膜的稳定性与选择性,其制备过程中通过调节制备步骤中反应条件,如苯胺单体组分料液浓度、操作时间、操作温度等,就可以有效控制聚苯胺层厚度与荷正电性大小,使得到的单价阳离子选择性分离膜具有单多价阳离子选择性分离的性能。
附图说明
图1 为实施例1得到的交联季铵化聚苯胺单价选择性阳离子交换膜的表面扫描电镜图;
图2 为实施例1得到的交联季铵化聚苯胺单价选择性阳离子交换膜的断面扫描电镜图;
图3为本发明的测试装置结构示意图;
图中:1-第一电极室,2-淡室,3-浓室,4-第二电极室,5-第一阴离子交换膜,6-单价选择性阳离子交换膜,7-第二阴离子交换膜,8-阳极,9-阴极,10-料液口。
具体实施方式
下面结合具体实施例对本发明作进一步说明,但本发明的保护范围并不限于此。
实施例 1
使用商业阳离子交换膜作为基膜,所述商业阳离子交换膜购自日本德山曹达公司,型号为CM-1。
将基膜表面用1 mol/L的苯胺单体溶液浸泡60min,取出基膜使用滤纸吸干表面多余溶液,然后浸泡1 mol/L的氯化铁溶液60min,苯胺单体在氯化铁作用下在基膜表面发生氧化聚合反应生成聚苯胺活性层,然后将其置于60℃加热器上干燥,再将膜放入5g/L的1,2-二溴乙烷溶液中浸泡反应6 h(1,2-二溴乙烷溶液的溶剂为乙醇),最后从1,2-二溴乙烷溶液中取出基膜用纯水反复冲洗,得到交联季铵化聚苯胺单价选择性阳离子交换膜,放入纯水中保存。
本实施例制备交联季铵化聚苯胺单价选择性阳离子交换膜的表面扫描电镜图和断面扫描电镜图分别如图1和图2所示,苯胺单体在氯化铁氧化剂作用下在基膜表面发生氧化聚合反应生成球状聚苯胺相互堆积,再经过季铵化改性形成一层薄而致密的活性皮层,由于聚苯胺本身的致密性与季铵化改性后的荷正电性,多价离子的传输受到阻碍,通量下降。
将所得交联季铵化聚苯胺单价选择性阳离子交换膜产品,进行单多价阳离子选择性电渗析实验,电渗析实验的测试装置结构如图3所示,包括电极室,电极室的左右两端分别为阳极8和阴极9,第一阴离子交换膜5、单价选择性阳离子交换膜6和第二阴离子交换膜7设置于电极室内并将电极室分隔为第一电极室1、淡室2、浓室3和第二电极室4,第一电极室1、淡室2、浓室3和第二电极室4顶部均设有料液口10。上述第一阴离子交换膜5和第二阴离子交换膜7均购自日本德山曹达公司,型号为CM-1。单价选择性阳离子交换膜6为本实施例制得的交联季铵化聚苯胺单价选择性阳离子交换膜产品。
测试步骤如下:实验以Na+/Mg2+水溶液为测试体系,将Na+/Mg2+水溶液分别加入淡室2与浓室3(Na+/Mg2+水溶液中,Na+和Mg2+初始浓度均为0.05 mol/L),在第一电极室1和第一电极室4中分别加入0.05 mol/L的Na2SO4水溶液,然后向阳极8和阴极9施加0.1A的恒流直流电,淡室2内的Na+、Mg2+会在电场力的作用下透过单价选择性阳离子交换膜6进入浓室3,而由于单价选择性阳离子交换膜对于多价离子的阻碍作用其通量将小于单价离子的通量,一小时后取淡室2的溶液利用离子色谱分析Na+和Mg2+的浓度,并计算Na+、Mg2+的通量(,其中Ji为通量,C0为初始浓度,C1为最终浓度,t为时间),以及Na+相对Mg2+选择性透过值(,其中S为选择性透过值,JNa为Na+的通量,JMg为Mg2+的通量)。
计算结果如下:聚苯胺能够增加基膜的致密度,而1,2-二溴乙烷可以引入相反电荷的同时进一步提高膜的稳定性。计算得钠离子的通量为,要远高于镁离子的通量。本实施例制得的交联季铵化聚苯胺单价选择性阳离子交换膜产品的选择性透过值达到3.14,而基膜的选择性透过值却低于1.0。第一阴离子交换膜5和第二阴离子交换膜7为基膜。
实施例 2
上述实例1中的步骤不变,改变1,2-二溴乙烷溶液为1,4-二溴丁烷溶液。施例2改性膜的钠镁离子的通量为,本实施例制得的交联季铵化聚苯胺单价选择性阳离子交换膜产品的选择性透过值达到3.52。得到了较好的选择性。
实施例 3
本说明书所述的内容仅仅是对发明构思实现形式的列举,本发明的保护范围不应当被视为仅限于实施例所陈述的具体形式,本发明的保护范围也仅仅于本领域技术人员根据本发明构思所能够想到的等同技术手段。
Claims (5)
1.一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于包括基膜和位于基膜界面上的活性层,在界面采用苯胺单体与氧化剂氧化聚合后,所得聚合物与季铵化试剂反应制得的季铵化聚苯胺,所述季铵化聚苯胺为活性层;
所述季铵化试剂的结构通式为X-(CH2)n-X,所述X为Cl、Br或I,n表示1~18的整数;所述季铵化试剂为1,2-二溴乙烷、1,3-二溴丙烷或1,4-二溴丁烷;
所述的季铵化聚苯胺单价选择性阳离子交换膜,用于Na+和Mg2+之间的分离;
所述交联季铵化聚苯胺单价选择性阳离子交换膜的制备方法如下:季铵化试剂溶于有机溶剂中作为季铵溶液,阳离子交换膜作为基膜;基膜表面用苯胺单体溶液浸泡后取出,使用滤纸吸干基膜表面的液体后,将所述基膜浸入氧化剂溶液中进行氧化聚合反应,苯胺单体与氧化剂在基膜表面发生氧化聚合反应生成聚苯胺活性层,再将基膜取出干燥后,放入季铵溶液中浸泡反应,最后将基膜从季铵溶液中取出并用纯净水反复冲洗,即得所述交联季铵化聚苯胺单价选择性阳离子交换膜。
2.根据权利要求1所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于氧化剂为氯化铁、过硫酸铵或重铬酸钾。
3.根据权利要求1所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于氧化剂溶液中,溶剂为水,氧化剂的浓度为0.1~10 mol/L,所述氧化剂为氯化铁;所述基膜浸入氧化剂溶液中反应的时间为5~300min。
4.根据权利要求1所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于基膜表面用苯胺单体溶液浸泡的时间为5~300min;所述苯胺单体溶液中,溶剂为乙醇,苯胺单体的浓度为0.1~10 mol/L。
5.根据权利要求1所述的一种交联季铵化聚苯胺单价选择性阳离子交换膜,其特征在于季铵溶液中,季铵化试剂的质量浓度为0.1~100 g/L,有机溶剂为乙醇;基膜放入季铵溶液中浸泡反应的时间为1~50h。
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