CN106632933A - 一种芳族聚亚胺多孔材料的机械制备方法 - Google Patents
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Abstract
本发明涉及一种芳族聚亚胺多孔材料的机械制备方法,包括:将均苯三甲醛和芳二胺两种单体置于研钵中,滴加二甲基甲酰胺和乙酸溶液,在室温下研磨1‑4h,然后洗涤、干燥,即得。本发明采用机械合成方法,使得醛基和胺基发生脱水缩合反应生成芳族聚亚胺多孔材料,在气体存储与分离、超级电容器、催化剂载体以及传感器等方面有潜在的应用。
Description
技术领域
本发明属于多孔材料的制备领域,特别涉及一种芳族聚亚胺多孔材料的机械制备方法。
背景技术
多孔材料是一种由相互贯通或封闭的孔洞构成网络结构的材料。根据元素组成和键合方式的不同,多孔材料分为无机、无机-有机杂化和纯有机这三种形式的多孔材料。一般而言,无机孔材料及无机-有机杂化多孔材料,如活性炭、分子筛等,其分子结构不可设计,化学功能不可调。有机多孔材料是新兴的多孔材料,由轻元素组成的有机基元通过共价键连接形成,因此具有骨架组成丰富、修饰性强、稳定性好、比表面积高、孔道结构可调等优点。
芳族聚亚胺交联网络是有机多孔材料中典型代表。这类多孔材料含有大量亚胺或甲亚胺基团,通常由芳二胺和多羰基化合物通过席夫碱反应缩合而成。这种制备方法通常采用溶剂热法,需要高温高压和大量有机溶剂,对设备有一定的要求。同时,该方法的反应时间较长,能耗大。
发明内容
本发明所要解决的技术问题是提供一种芳族聚亚胺多孔材料的机械制备方法,本专利采用机械法合成芳族聚亚胺多孔材料,该方法在室温下机械研磨,使用极少量有机溶剂,具有环保、节能、耗时短等优点。
本发明的一种芳族聚亚胺多孔材料的机械制备方法,包括:
将均苯三甲醛和芳二胺两种单体置于玛瑙研钵中,滴加二甲基甲酰胺和乙酸溶液,在室温下研磨1-4h,然后洗涤除去未反应的原料和低聚物、干燥,即得到芳族聚亚胺多孔材料。
所述均苯三甲醛和芳二胺的摩尔比为2:3。
所述芳二胺为含两个胺基的芳族化合物。
所述芳二胺为1,5-萘二胺、对苯二胺、间苯二胺、2,3-二胺基吡啶、2,6-二胺基吡啶、2,5-二胺基吡啶中的一种。
所述二甲基甲酰胺和乙酸溶液的体积比为1:1。
所述乙酸溶液的浓度为5~7moL/L。
所述芳二胺、二甲基甲酰胺、乙酸溶液的比例为0.75mmol:0.2mL:0.2mL。
所述洗涤为用有机溶剂索氏提取洗涤2-3天。
所述有机溶剂为丙酮、甲醇。
所述干燥为50℃下的真空烘箱中干燥2-3天。
所述得到的芳族聚亚胺多孔材料在气体存储与分离、超级电容器、催化剂载体以及传感器方面的应用。
有益效果
本专利采用机械法合成芳族聚亚胺多孔材料,该方法在室温下机械研磨,使用极少量有机溶剂,具有环保、节能、耗时短等优点;
本发明利用均苯三甲醛和二胺两种单体发生脱水缩合反应生成芳族聚亚胺多孔材料,其在气体存储与分离、超级电容器、催化剂载体以及传感器等方面有潜在的应用。
附图说明
图1为均苯三甲醛和1,5-萘二胺脱水缩合成聚合物的ATR-IR图;
图2为均苯三甲醛和1,5-萘二胺脱水缩合成聚合物的13C-NMR图;
图3为均苯三甲醛和1,5-萘二胺脱水缩合成聚合物的XRD图;
图4为均苯三甲醛和对苯二胺脱水缩合成聚合物的ATR-IR图;
图5为均苯三甲醛和对苯二胺脱水缩合成聚合物的13C-NMR图;
图6为均苯三甲醛和对苯二胺脱水缩合成聚合物的XRD图;
图7为均苯三甲醛和间苯二胺脱水缩合成聚合物的ATR-IR图;
图8为均苯三甲醛和间苯二胺脱水缩合成聚合物的13C-NMR图;
图9为均苯三甲醛和间苯二胺脱水缩合成聚合物的XRD图;
图10为均苯三甲醛和2,3-二胺基吡啶脱水缩合成聚合物的ATR-IR图;
图11为均苯三甲醛和2,3-二胺基吡啶脱水缩合成聚合物的13C-NMR图;
图12为均苯三甲醛和2,3-二胺基吡啶脱水缩合成聚合物的XRD图;
图13为均苯三甲醛和2,6-二胺基吡啶脱水缩合成聚合物的ATR-IR图;
图14为均苯三甲醛和2,6-二胺基吡啶脱水缩合成聚合物的13C-NMR图;
图15为均苯三甲醛和2,6-二胺基吡啶脱水缩合成聚合物的XRD图;
图16为均苯三甲醛和2,5-二胺基吡啶脱水缩合成聚合物的ATR-IR图;
图17为均苯三甲醛和2,5-二胺基吡啶脱水缩合成聚合物的13C-NMR图;
图18为均苯三甲醛和2,5-二胺基吡啶脱水缩合成聚合物的XRD图。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
将均苯三甲醛(81.07mg,0.5mmoL)、1,5-萘二胺(118.65mg,0.75mmoL)两种单体置于玛瑙研钵(75mm内径)中,滴加二甲基甲酰胺和6mol/L乙酸溶液各0.2mL,然后使用研杵在室温下研磨。研磨后,在索氏提取装置中用无水丙酮洗涤48h,以除去未反应的原料和低聚物,最后置于50℃下的真空烘箱中干燥两天,即得到芳族聚亚胺多孔材料。产率为28.5%,BET比表面积为5.7m2/g。
实施例2
将均苯三甲醛(81.07mg,0.5mmoL)、对苯二胺(81.11mg,0.75mmoL)两种单体置于玛瑙研钵(75mm内径)中,滴加二甲基甲酰胺和6mol/L乙酸溶液各0.2mL,然后使用研杵在室温下研磨。研磨后,在索氏提取装置中用无水丙酮洗涤48h,以除去未反应的原料和低聚物,最后置于50℃下的真空烘箱中干燥两天,即得到芳族聚亚胺多孔材料。产率为38.6%,BET比表面积为15.4m2/g。
实施例3
将均苯三甲醛(81.07mg,0.5mmoL)、间苯二胺(81.11mg,0.75mmoL)两种单体置于玛瑙研钵(75mm内径)中,滴加二甲基甲酰胺和6mol/L乙酸溶液各0.2mL,然后使用研杵在室温下研磨。研磨后,在索氏提取装置中用无水丙酮洗涤48h,以除去未反应的原料和低聚物,最后置于50℃下的真空烘箱中干燥两天,即得到芳族聚亚胺多孔材料。产率为41.9%,BET比表面积为30m2/g。
实施例4
将均苯三甲醛(81.07mg,0.5mmoL)、2,3-二胺基吡啶(81.75mg,0.75mmoL)两种单体置于玛瑙研钵(75mm内径)中,滴加二甲基甲酰胺和6mol/L乙酸溶液各0.2mL,然后使用研杵在室温下研磨。研磨后,在索氏提取装置中用无水丙酮洗涤48h,以除去未反应的原料和低聚物,最后置于50℃下的真空烘箱中干燥两天,即得到芳族聚亚胺多孔材料。产率为27.4%,BET比表面积为94m2/g。
实施例5
将均苯三甲醛(81.07mg,0.5mmoL)、2,6-二胺基吡啶(81.75mg,0.75mmoL)两种单体置于玛瑙研钵(75mm内径)中,滴加二甲基甲酰胺和6mol/L乙酸溶液各0.2mL,然后使用研杵在室温下研磨。研磨后,在索氏提取装置中用无水丙酮洗涤48h,以除去未反应的原料和低聚物,最后置于50℃下的真空烘箱中干燥两天,即得到芳族聚亚胺多孔材料。产率为58.8%,BET比表面积为3m2/g。
实施例6
将均苯三甲醛(81.07mg,0.5mmoL)、2,5-二胺基吡啶(81.75mg,0.75mmoL)两种单体置于玛瑙研钵(75mm内径)中,滴加二甲基甲酰胺和6mol/L乙酸溶液各0.2mL,然后使用研杵在室温下研磨。研磨后,在索氏提取装置中用无水丙酮洗涤48h,以除去未反应的原料和低聚物,最后置于50℃下的真空烘箱中干燥两天,即得到芳族聚亚胺多孔材料。产率为54.8%,BET比表面积为81m2/g。
Claims (10)
1.一种芳族聚亚胺多孔材料的机械制备方法,包括:
将均苯三甲醛和芳二胺两种单体置于研钵中,滴加二甲基甲酰胺和乙酸溶液,在室温下研磨1-4h,然后洗涤、干燥,即得到芳族聚亚胺多孔材料。
2.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述均苯三甲醛和芳二胺的摩尔比为2:3。
3.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述芳二胺为含两个胺基的芳族化合物。
4.根据权利要求3所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述芳二胺为1,5-萘二胺、对苯二胺、间苯二胺、2,3-二胺基吡啶、2,6-二胺基吡啶、2,5-二胺基吡啶中的一种。
5.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:二甲基甲酰胺和乙酸溶液的体积比为1:1,其中乙酸溶液的浓度为5~7moL/L。
6.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述芳二胺、二甲基甲酰胺、乙酸溶液的比例为0.75mmol:0.2mL:0.2mL。
7.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述洗涤为用有机溶剂索氏提取洗涤2-3天。
8.根据权利要求7所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述有机溶剂为丙酮、甲醇。
9.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述干燥为50℃下的真空烘箱中干燥2-3天。
10.根据权利要求1所述的一种芳族聚亚胺多孔材料的机械制备方法,其特征在于:所述得到的芳族聚亚胺多孔材料在气体存储与分离、超级电容器、催化剂载体以及传感器方面的应用。
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