CN107417927B - 具有咪唑结构的多孔金属有机框架材料的合成方法 - Google Patents
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Abstract
本发明提供了一种具有咪唑结构的金属有机框架材料的合成方法,是以咪唑、5,6‑二甲基苯并咪唑、四水合醋酸钴为原料,以N,N‑二甲基甲酰胺为溶剂,在室温下搅拌合成金属有机框架;然后经高温碳化,得到具有咪唑结构的多孔金属有机框架材料。本发明具有原料廉价易得,合成工艺简单,反应条件温和,合成成本低,产率高等特点;合成的MOF材料化学稳定性好,密度小,热稳定性好,电化学性能优异,作为超级电容器电极具有很好的应用前景。
Description
技术领域
本发明涉及一种金属有机框架材料的合成,具体涉及一种具有咪唑结构的多孔金属有机框架材料的合成方法,属于金属有机合成技术领域。
背景技术
金属有机框架材料(metal organic frameworks,MOFs)是近十年来发展迅速的一种配位聚合物,具有三维的孔结构,一般以金属离子为连接点,有机配位体支撑构成空间3D延伸,是沸石和碳纳米管之外的又一类重要的新型多孔材料,在催化、储能和分离中都有广泛应用。目前,MOF已成为无机化学、有机化学等多个化学分支的重要研究方向。MOFs具有比表面积大,结构和孔径可调,热稳定性和化学稳定性好,结构有序,孔结构丰富等优点。20世纪90年代中期,第一代MOFs材料被合成出来,孔径和稳定性受到一定限制;1999年,Yaghi等人合成具有三维开放骨架结构的MOF-5,去除孔道中的客体分子后仍然保持骨架完整;2002年,Yaghi科研组合成IRMOF系列材料,实现了MOF材料从微孔到介孔的成功过渡;2008年,Yaghi科研小组合成出上百种ZIF系列类分子筛材料。金属-有机骨架化合物作为新的研究领域,在荧光、磁性、非线性光学、吸附、分离、储氢和催化等诸多方面显示出其独特的物理和化学性能以及潜在的巨大应用价值。
MOFs材料具有较大的孔隙率和比表面积,有利于产生较大的双电层电容。同时这种结构有利于电解质溶液的渗透,电化学过程中电荷的传输和金属活性中心的充分利用,被期望实现较好的速率性能和赝电容性能。
咪唑是分子结构中含有两个间位氮原子的五元芳杂环化合物,咪唑环中的1-位氮原子的未共用电子对参与环状共轭, 咪唑比其他1,3-二唑更容易发生亲电芳香取代反应,并且反应主要在C-4和C-5上进行。咪唑结构中的N原子可与金属离子配位,影响MOFs材料的孔径尺寸与孔道结构,咪唑中的氮原子还可提高MOFs材料的含氮量,增加其比电容。因此将咪唑结构与金属有机框架材料相结合,得到的复合材料应当具有优异的电化学性能,可作为超级电容器电极材料。
发明内容
本发明的目的是提供一种合成成本低廉,合成工艺简单,热稳定性以及化学稳定性良好的具有咪唑结构的多孔金属有机框架材料的合成方法。
一、MOF的合成
以咪唑、5,6-二甲基苯并咪唑、四水合醋酸钴为原料,以N,N-二甲基甲酰胺(DMF)为溶剂,在室温下搅拌合成了多孔金属有机框架材料MOF,其具体工艺为:将咪唑与5,6-二甲基苯并咪唑溶解在N,N-二甲基甲酰胺(DMF)中得溶液;将四水合醋酸钴溶解在DMF中得溶液,再在搅拌下将溶液缓慢滴加到溶液中;滴加完毕后搅拌反应45~48小时,反应结束后,抽滤,产物用DMF洗去未反应的咪唑、5,6-二甲基苯并咪唑以及盐,再用二次蒸馏水洗去DMF,然后用乙醇洗涤;洗涤完成后,于60~70℃真空干燥20~24小时,研磨,获得紫色粉末;然后将紫色粉末置于管式炉中,以2~5℃/分钟的速度升温至600~650℃(温度太低碳化不完全,太高使MOF结构坍塌。),碳化2~2.5h,自然冷却到室温,得到MOF材料。
咪唑与5,6-二甲基苯并咪唑的物质的量为1:1~1:1.05;咪唑与四水合醋酸钴的物质的量比为2:1~2.05:1。
二、MOF的表征
1、FT-IR分析
图1为本发明合成的MOF材料的FT-IR图。2933 cm-1处的峰是咪唑的N-H键的伸缩振动峰,位于1301 cm-1、1081 cm-1和 834 cm-1处的吸收峰是C-N键的伸缩振动峰,位于3024cm-1处的吸收峰是C-H键的振动峰。说明材料成功合成。
2、扫描电镜分析
图2为本发明合成的MOF材料的扫描电镜图。扫描电子显微镜照片表明,MOF材料的颗粒大小不均,无规则形状,且颗粒表面光滑。
3、热重分析
图3为本发明合成的MOF材料的热分析图。热分析图表明,本发明合成的MOF材料热稳定性非常好,200℃之前几乎没有失重,200℃~550℃的失重归结为空腔内的客体分子和孔道中未反应的物质的去除,600℃之后的失重归结为结构的坍塌。
4、X射线粉末衍射分析
图4为本发明合成的MOF材料的X射线粉末衍射图。X射线粉末衍射图表明,MOF材料具有较好的结晶度。
5、循环伏安测试分析
图5为本发明合成的MOF材料煅烧后的循环伏安图。其中图(a)是在0 ~0.4 V的窗口电压下扫描速度由5 mV s-1增加到200 mV s-1(由上至下)的CV曲线。图(a)中存在显著的氧化还原峰,表现出典型的赝电容性能。图(b)是在-1V~0V的窗口电压下扫描速度由5 mVs-1增加到200 mV s-1(由上至下)的CV曲线。由图(b)显示,该材料在-1~0V的窗口内有着类矩形特征出现同时显示出了高的响应电流,充分体现出了该材料的良好双电层电容行为,且在实验测试电位范围内均具备较好的电化学可逆性。
6、恒电流充放电测试分析
图6为本发明合成的MOF材料煅烧后的恒电流充放电的放电曲线图。从图6中可以发现,放电曲线并非呈三角形,在每段曲线中曲线的斜率发生变化出现有一定斜度的“平台”,显示出明显的法拉第反应。
7、交流阻抗测试分析
图7为本发明合成的MOF材料煅烧后的交流阻抗图。在高频区,因为 6 M KOH电解液离子比较容易接近大的孔隙,因而它的阻抗比较小;而在中频区,该水系电解液离子要进入到电极的内部中相对较小的孔隙中去,电解液离子的运动就属于扩散动力学控制,相对于在高频区时,它就很难进入到电极的内部中去,阻抗就会相对的比较大;在低频区,材料的阻抗曲线接近于纯电容性质,阻抗虚部会急剧增加。高频区并没有明显的半圆,这表明该材料有着很小的电荷转移阻抗,但在低频区不是一条特别垂直于实轴的直线,这表明该材料有着一定的内阻。
综上所述,本发明以咪唑,5,6-二甲基苯并咪唑与四水合醋酸钴为原料,以N,N-二甲基甲酰胺(DMF)为溶剂,采用室温搅拌法合成了多孔金属有机框架材料MOF,具有原料廉价易得,合成工艺简单,反应条件温和,合成成本低,产率高等特点;合成的MOF材料化学稳定性好,密度小,热稳定性好,在吸附、气体分离、传感、储能以及催化等领域具有很好的应用前景;将其煅烧后作为超级电容器电极,电化学性能优异。
附图说明
图1为本发明合成的MOF材料的红外光谱图。
图2为本发明合成的MOF材料的扫描电镜图。
图3为本发明合成的MOF材料的热分析图。
图4为本发明合成的MOF材料的X射线粉末衍射图。
图5为本发明合成的MOF材料煅烧后的循环伏安图。
图6为本发明合成的MOF材料煅烧后的恒电流充放电的放电曲线图。
图7为本发明合成的MOF材料煅烧后的交流阻抗图。
具体实施方式
下面通过具体实施例对本发明MOF材料的合成和性能作进一步说明。
将0.068 g (1mol)咪唑,将0.154 g(1.05mol)5,6-二甲基苯并咪唑溶解在10mLN,N-二甲基甲酰胺(DMF)中为溶液,将0.125 g(0.5mol)四水合醋酸钴溶解在2.5 mLDMF中为溶液;在搅拌的条件下向溶液中缓慢滴加溶液;滴加完毕后继续搅拌48小时,反应结束后,抽滤,产物先用DMF洗去未反应的咪唑和5,6-二甲基苯并咪唑以及盐,再用二次蒸馏水洗去DMF,然后用乙醇洗涤。洗涤完成后,65℃左右真空干燥24小时,充分研磨,获得紫色粉末;然后将紫色粉末置于管式炉中,于650℃碳化2小时,得MOF材料。
电化学性能测试,上述制备的MOF材料在0.5 A g-1,1 A g-1,2 A g-1,4 A g-1,6 Ag-1,8A g-1,10 A g-1和20 A g-1的电流密度下比电容值分别为392.86 F g-1,326.00 F g-1,201.20 F g-1,174.59 F g-1,165.90 F g-1,157.80 F g-1,145.08 F g-1,133.76 F g-1,110.75 F g-1,92.78 F g-1。
Claims (4)
1.具有咪唑结构的多孔金属有机框架材料的合成方法,是以咪唑、5,6-二甲基苯并咪唑、四水合醋酸钴为原料,以N,N-二甲基甲酰胺为溶剂,在室温下搅拌合成金属有机框架;然后经高温碳化,得到具有咪唑结构的多孔金属有机框架材料;具体工艺为:将咪唑与5,6-二甲基苯并咪唑溶解在N,N-二甲基甲酰胺中得溶液I;将四水合醋酸钴溶解在DMF中得溶液II,再在搅拌下将溶液II缓慢滴加到溶液I中;滴加完毕后室温搅拌反应45~48小时;反应结束后,抽滤,洗涤,干燥,研磨,获得紫色粉末;然后将紫色粉末置于管式炉中,升温至600~650℃,碳化2~2.5h,自然冷却到室温,得到MOF材料;咪唑与5,6-二甲基苯并咪唑的物质的量为1:1~1:1.05;咪唑与四水合醋酸钴的物质的量比为2:1~2.05:1。
2.如权利要求1所述具有咪唑结构的多孔金属有机框架材料的合成方法,其特征在于:所述洗涤为先用DMF洗去未反应的咪唑、5,6-二甲基苯并咪唑以及盐,再用二次蒸馏水洗去DMF,然后用乙醇洗涤。
3.如权利要求1所述具有咪唑结构的多孔金属有机框架材料的合成方法,其特征在于:所述干燥为于60~70℃真空干燥20~24小时。
4.如权利要求1所述具有咪唑结构的多孔金属有机框架材料的合成方法,其特征在于:管式炉中碳化时升温速度为2~5℃/分钟。
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