CN112608503B - 一种用于碱性电解池的哌啶型阴离子交换膜及其制备方法 - Google Patents
一种用于碱性电解池的哌啶型阴离子交换膜及其制备方法 Download PDFInfo
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
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- XJKSTNDFUHDPQJ-UHFFFAOYSA-N 1,4-diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=C(C=2C=CC=CC=2)C=C1 XJKSTNDFUHDPQJ-UHFFFAOYSA-N 0.000 claims description 11
- 229930184652 p-Terphenyl Natural products 0.000 claims description 11
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000005576 amination reaction Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
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- 238000000034 method Methods 0.000 claims description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种用于碱性电解池的哌啶型阴离子交换膜及其制备方法,属于碱性阴离子交换膜技术领域。本发明首先合成不同取代度的哌啶型三单体聚合物,再直接以聚合物的哌啶酮作为接枝位点对聚合物进行季胺化后获得膜材料并制膜。所制备的膜具有较好的碱稳定性和机械强度,可应用于碱性电解池中。
Description
技术领域
本发明属于碱性阴离子交换膜技术领域,涉及到一种用于碱性电解池的哌啶型阴离子交换膜及其制备方法。
背景技术
随着能源短缺和环境污染等问题日益突出,开发利用新能源迫在眉睫。相比传统的化石燃料而言,氢能是一种可替代的理想能源。它具有高能量密度和零碳排放等优势。在众多制氢方法中,阴离子交换膜电解水(AEMWE)技术具有成本低、环境友好和制氢稳定性高的优点,近年来受到了广泛的关注。
碱性阴离子交换膜是碱性阴离子交换膜电解池的核心部件之一,通常是由含季铵基团的聚合物制备,起到选择性传递氢氧根离子并且分隔两极室的作用。这样的功能就要求碱性阴离子交换膜既有很好的传递氢氧根离子的能力,又能在碱性环境中保持性能的稳定。目前膜材料常用聚砜,聚苯醚等聚合物作为主链,但部分聚合物在碱性环境中会发生降解,存在离子传导率低,吸水溶胀高,尺寸稳定性差、IEC(离子交换容量)不可控的问题。因此寻找具有良好的尺寸稳定性和高电导率的聚合物,是目前关注的热点之一。
发明内容
本发明旨在提高碱性阴离子交换膜的尺寸稳定性和氢氧根传递性能,提供了一种可调离子交换容量的哌啶型阴离子交换膜的制备方法。合成了具有良好碱稳定性和机械性能的哌啶型三单体聚合物,通过控制单体的投料比例来控制取代度,再对聚合物与碘甲烷反应得到季胺化聚合物,并用季胺化聚合物进行铸膜。所制备的膜具有较好的尺寸稳定性和良好的离子传导率,可用于碱性电解池中。
本发明的技术方案:
一种用于碱性电解池的哌啶型阴离子交换膜,哌啶型阴离子交换膜中哌啶型季胺化聚合物的结构如下:
其中:m=0.6~0.9。
一种用于碱性电解池的哌啶型阴离子交换膜的制备方法,步骤如下:
(1)哌啶型三单体聚合物的合成:将对三联苯溶于二氯甲烷中,溶解后加入N-甲基-4哌啶酮和丙酮酸甲酯,在冰浴下逐滴加入三氟乙酸和三氟甲磺酸,1h后撤去冰浴,室温下反应3小时后得到溶液,随后将溶液倒入溶剂A中沉淀,最后用水洗涤至中性,烘箱干燥得到三单体聚合物;
所述的对三联苯与二氯甲烷的w/v,g/mL为16~20%;
所述的对三联苯:N-甲基-4哌啶酮:丙酮酸甲酯的摩尔比为1:1.1:0.1~0.4;
所述的对三联苯与三氟甲磺酸的摩尔比为1:8~9;
所述的对三联苯与三氟乙酸的摩尔比为1:1.3~2;
所述的溶剂A为甲醇、乙醇中的一种;
(2)季胺化聚合物制备:三单体聚合物溶于溶剂B中,溶解后加碘甲烷,最后加入碳酸钾,在60℃下避光反应一段时间;将反应结束后的溶液倒入溶剂C中析出,最后用溶剂C洗涤、过滤、干燥,得到季胺化聚合物;
所述的三单体聚合物:碘甲烷:碳酸钾的摩尔比为:1:1.5~2:0.5~1;
所述的溶剂B为N-甲基吡咯烷酮、二甲基亚砜的一种;
所述的三单体聚合物与溶剂B的w/v,g/mL为4~6%;
所述的析出剂C为丙酮、乙酸乙酯中的一种;
所述的避光反应时间为36~48h;
(3)哌啶型阴离子交换膜的制备:将季胺化聚合物溶于溶剂D中,溶解后离心去除杂质得到铸膜液;再将铸膜液浇铸成膜;将膜浸泡于1mol/L氢氧化钾溶液中24~48h,在去离子水中浸泡至中性,即得哌啶型阴离子交换膜;
所述的溶剂D为N-甲基吡咯烷酮、二甲基亚砜的一种;
所述的铸膜液w/v,g/mL为3~6%;
所述的浇铸法成膜的烘干温度为60~80℃,时间为24~48小时。
步骤(1)中的干燥条件为:温度为60~70℃,时间为24~36h。
步骤(2)中的干燥条件为:温度为50~60C,时间为24小时以上。
本发明的有益效果:
(1)通过改变单体的投料比例,可以制备出不同离子交换容量的阴离子交换膜。
(2)引入第三单体丙酮酸甲酯,可以降低聚合物的刚性,增加其柔韧度。
(3)N-甲基-4-哌啶酮可以直接作为功能化反应位点,反应步骤少,有利于膜内的微相分离,提高了膜的性能。
具体实施方式
以下结合实施案例对本发明做进一步详细的描述,但是本发明的实施方式并不仅限于此。
实施例
哌啶型三单体聚合物的合成:将1.41g(6mmol)对三联苯加入到25mL三口烧瓶中,然后加入8mL二氯甲烷溶液,随后加入0.6928g(6mmol)N-甲基-4-哌啶酮和56μL(0.6mmol)丙酮酸甲酯,机械搅拌一段时间后在冰浴条件下缓慢加入1mL(9.98mmol)三氟乙酸5mL(56.5mmol)三氟甲磺酸,然后反应体系温度逐渐上升到室温。当反应溶液变得高度黏稠时,将反应溶液倒入甲醇中析出聚合物粗品,然后用碳酸钾溶液洗涤至中性,在60℃真空干燥24h得到三单体聚合物材料。
季胺化阴离子交换膜的制备:称取1g(3.08mmol)三单体聚合物材料加入到50mL单口瓶中,然后加入20mL DMSO,溶解后再加入0.4702g(3.3340mmol)碳酸钾和0.7869g(5.5440mmol)碘甲烷,60℃下避光反应48h左右,反应结束后得到的溶液倒入丙酮中析出固体粉末状产物,过滤干燥后用去离子水多次洗涤除去未反应的盐,60℃真空干燥24h得到季铵化聚合物。称取0.12g季铵化聚合物溶解于4mL DMSO中,将铸膜液离心后浇铸在玻璃模具中,60℃干燥48h,得到聚合物膜。将聚合物膜在室温下浸泡于1mol/L的KOH溶液中48h,然后用去离子水反复清洗、浸泡48h至中性,即可得季胺化哌啶型阴离子交换膜。
本实例所得到的阴离子交换膜的结构如下:
m=0.9
经测试表明,本实施例中所制备的季胺化哌啶型阴离子交换膜在30℃时离子传导率为31mS cm-1,吸水率为31%,溶胀度为15%,80℃浸泡于1mol/L的NaOH溶液中552h,电导率保留率为91%,拉伸强度为8.9MPa,膜表现出较好的机械强度和碱稳性能。将膜组装到碱性电解池中进行测试,50℃,2.28V时电流密度达到1164mA/cm2(电解液为1mol/L KOH溶液);电池在运行250h后,电势保持在1.85V左右,体现了优异的稳定性。
Claims (4)
2.权利要求1所述的哌啶型阴离子交换膜的制备方法,其特征在于,步骤如下:
(1)哌啶型三单体聚合物的合成:将对三联苯溶于二氯甲烷中,溶解后加入N-甲基-4哌啶酮和丙酮酸甲酯,在冰浴下逐滴加入三氟乙酸和三氟甲磺酸,1h后撤去冰浴,室温下反应3小时后得到溶液,随后将溶液倒入溶剂A中沉淀,最后用水洗涤至中性,烘箱干燥得到三单体聚合物;
所述的对三联苯与二氯甲烷的w/v,g/mL为16~20%;
所述的对三联苯:N-甲基-4哌啶酮:丙酮酸甲酯的摩尔比为1:1.1:0.1~0.4;
所述的对三联苯与三氟甲磺酸的摩尔比为1:8~9;
所述的对三联苯与三氟乙酸的摩尔比为1:1.3~2;
所述的溶剂A为甲醇、乙醇中的一种;
(2)季胺化聚合物制备:三单体聚合物溶于溶剂B中,溶解后加碘甲烷,最后加入碳酸钾,在60℃下避光反应一段时间;将反应结束后的溶液倒入溶剂C中析出,最后用溶剂C洗涤、过滤、干燥,得到季胺化聚合物;
所述的三单体聚合物:碘甲烷:碳酸钾的摩尔比为:1:1.5~2:0.5~1;
所述的溶剂B为N-甲基吡咯烷酮、二甲基亚砜的一种;
所述的三单体聚合物与溶剂B的w/v,g/mL为4~6%;
所述的析出剂C为丙酮、乙酸乙酯中的一种;
所述的避光反应时间为36~48h;
(3)哌啶型阴离子交换膜的制备:将季胺化聚合物溶于溶剂D中,溶解后离心去除杂质得到铸膜液;再将铸膜液浇铸成膜;将膜浸泡于1mol/L氢氧化钾溶液中24~48h,在去离子水中浸泡至中性,即得哌啶型阴离子交换膜;
所述的溶剂D为N-甲基吡咯烷酮、二甲基亚砜的一种;
所述的铸膜液w/v,g/mL为3~6%;
所述的浇铸法成膜的烘干温度为60~80℃,时间为24~48小时。
3.根据权利要求2所述的制备方法,其特征在于:步骤(1)中的干燥条件为:温度为60~70℃,时间为24~36h。
4.根据权利要求2或3所述的制备方法,其特征在于:步骤(2)中的干燥条件为:温度为50~60C,时间为24小时以上。
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