CN109054808A - 具有荧光传感能力的镁-芳香羧酸多孔配合物及其制备方法和应用 - Google Patents
具有荧光传感能力的镁-芳香羧酸多孔配合物及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一类具有荧光传感能力的镁‑芳香羧酸多孔配合物及其制备方法和应用,该配合物的结构单元为Mga(L1)b(Sol)c(Ac)d(H2O)e,式中L1为脱去羧基上三个氢原子的4,4',4”‑均苯三苯甲酸三价阴离子或脱去羧基上两个氢原子的2,5‑呋喃二羧酸二价阴离子,Sol为N‑甲基乙酰胺或N,N‑二甲基乙酰胺,Ac为乙酰基。本发明以4,4',4”‑均苯三苯甲酸或2,5‑呋喃二羧酸为配体,采用溶剂热法制备得到镁‑芳香羧酸多孔配合物,制备方法简单,所得配合物具有较好的荧光性能,对硝基化合物硝基苯、邻硝基甲苯具有较高的敏感性,为潜在的荧光传感材料。
Description
技术领域
本发明属于主族金属有机配合物技术领域,具体涉及到一类具有荧光传感能力镁-芳香羧酸多孔配合物,以及该配合物的制备方法和应用。
背景技术
配位聚合物是最具有应用前景的一种晶体材料,与一般独立的无机、有机材料相比,配位聚合物将有机配体和无机金属离子两者的特点和性质结合在了一起,使其具有与独立无机、有机材料不同的新奇结构和性能。由于其结构多样性,性质丰富多彩,在气体分子与小分子有机蒸气的吸附与分离、多相催化、多相分离、分子与离子交换、手性识别与分离,分子磁性质、发光与非线性光学性质等方面具有广泛的应用前景,近期引发化学研究者广泛的关注,正迅速发展并成为材料、能源和生命科学交叉领域中的研究热点。
发明内容
本发明所要解决的技术问题在于提供一种可作为荧光传感材料的镁-芳香羧酸多孔配合物,并为该配合物提供一种制备方法和新的应用。
解决上述技术问题所采用的技术方案是:该配合物的结构单元为Mga(L1)b(Sol)c(Ac)d(H2O)e,式中L1为脱去三个羧基上氢原子的4,4',4”-均苯三苯甲酸三价阴离子,Sol为N-甲基乙酰胺,Ac为乙酰基,a为9、b为8、c为12、d为6、e为6,该配合物属于三方晶系,R-3空间群,晶胞参数a为b为 c为α为90°,β为90°,γ为120°;或者式中L1为脱去两个羧基上氢原子的2,5-呋喃二羧酸二价阴离子,Sol为N,N-二甲基乙酰胺,Ac为乙酰基,a为2、b为2、c为1、d为1、e为0,该配合物属于四方晶系,I4/mmm空间群,晶胞参数a为b为c为α为90°,β为90°,γ为90°。
上述配合物的结构单元Mga(L1)b(Sol)c(Ac)d(H2O)e中,L1为脱去三个羧基上氢原子的4,4',4”-均苯三苯甲酸三价阴离子,Sol为N-甲基乙酰胺,Ac为乙酰基,a为9、b为8、c为12、d为6、e为6时,该配合物的制备方法为:将4,4',4”-均苯三苯甲酸、4,4'-联吡啶、六水合硝酸镁按摩尔比为1:1~1.5:2~2.5加入N-甲基乙酰胺与乙醇体积比为4~4.5:1的混合液中,搅拌均匀,密封,90~100℃恒温静置反应7天,制备成镁-芳香羧酸多孔配合物。
上述配合物的结构单元Mga(L1)b(Sol)c(Ac)d(H2O)e中,L1为脱去两个羧基上氢原子的2,5-呋喃二羧酸二价阴离子,Sol为N,N-二甲基乙酰胺,Ac为乙酰基,a为2、b为2、c为1、d为1、e为0,该配合物的制备方法为:将2,5-呋喃二羧酸、六水合硝酸镁按摩尔比为1:2~2.5加入N,N-二甲基乙酰胺与蒸馏水体积比为6~6.5:1的混合液中,搅拌均匀,密封,120~130℃恒温静置反应12天,制备成镁-芳香羧酸多孔配合物。
本发明配合物可作为荧光传感器用于检测硝基苯或邻硝基甲苯。
本发明的镁-芳香羧酸多孔配合物采用荧光光谱仪进行了测试,测试结果表明,其对硝基苯和邻硝基甲苯都具有高度敏感性,随着加入硝基苯溶液和邻硝基甲苯溶液浓度的增大,其荧光发射强度逐渐降低,当加入的硝基苯达到一定值时配合物就会发生荧光猝灭;而对硝基甲烷的敏感性却不高,可以被开发成具有环保意义的荧光传感器来检测环境中的硝基苯和邻硝基甲苯,同时排除硝基甲烷的干扰。
附图说明
图1是实施例1制备的镁-芳香羧酸多孔配合物的晶体结构图。
图2是实施例1制备的镁-芳香羧酸多孔配合物的三维结构图。
图3是实施例2制备的镁-芳香羧酸多孔配合物的晶体结构图。
图4是实施例2制备的镁-芳香羧酸多孔配合物的三维结构图。
图5是实施例1制备的镁-芳香羧酸多孔配合物对硝基苯(NB)的荧光光谱图。
图6是实施例1制备的镁-芳香羧酸多孔配合物对邻硝基甲苯(2-NT)的荧光光谱图。
图7是实施例1制备的镁-芳香羧酸多孔配合物对硝基甲烷(NM)的荧光光谱图。
图8是实施例2制备的镁-芳香羧酸多孔配合物对硝基苯(NB)的荧光光谱图。
图9是实施例2制备的镁-芳香羧酸多孔配合物对邻硝基甲苯(2-NT)的荧光光谱图。
图10是实施例2制备的镁-芳香羧酸多孔配合物对硝基甲烷(NM)的荧光光谱图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
以制备结构单元为Mga(L1)b(Sol)c(Ac)d(H2O)e的镁-芳香羧酸多孔配合物为例,其中L1为脱去三个羧基上氢原子的4,4',4”-均苯三苯甲酸三价阴离子,Sol为N-甲基乙酰胺,Ac为乙酰基,a为9、b为8、c为12、d为6、e为6,具体制备方法如下:
将0.026g(0.1mmol)Mg(NO3)2·6H2O、0.021g(0.05mmol)4,4',4”-均苯三苯甲酸、0.008g(0.05mmol)4,4'-联吡啶加入2.5mL N-甲基乙酰胺与乙醇体积比为4:1的混合液中,搅拌均匀,密封,90℃恒温静置反应7天后,自然冷却至室温,制备成镁-芳香羧酸多孔配合物,根据Mg计算产率约为46%。
所制备的镁-芳香羧酸多孔配合物的单晶结构如图1所示,属于三方晶系,R-3空间群,晶胞参数a为b为c为α为90°,β为90°,γ为120°,其独立单元中存在三个晶体学独立的Mg(II)离子、8/3个4,4',4”-均苯三苯甲酸配体分子、两个由溶剂分子N-甲基乙酰胺分解得到的Ac-以及一个配位H2O分子。Mg1、Mg2均采取六配位模式形成空间变形八面体结构。与Mg1配位的六个氧原子中有五个4,4',4”-均苯三苯甲酸配体的羧基氧原子(O16,O17A,O19,O20,O21),另外一个为Ac-氧原子(O12),其中Mg1-O键长范围为与Mg2配位的六个氧原子分别为:四个来自于4,4',4”-均苯三苯甲酸配体的羧基氧原子(O13,O14,O18A,O21)、一个Ac-氧原子(O11)、一个配位H2O分子中的氧原子(O9),其中Mg2-O键长范围为Mg3与四个来自于4,4',4”-均苯三苯甲酸配体中的氧原子(O1,O7C,O5,O15B)配位形成空间变形四面体的结构,其中Mg3-O键长范围为由图2可见,所制备的镁-芳香羧酸多孔配合物为2-重穿插的空间三维阴离子骨架结构。
实施例2
以制备结构单元为Mga(L1)b(Sol)c(Ac)d(H2O)e的镁-芳香羧酸多孔配合物为例,其中L1为脱去两个羧基上氢原子的2,5-呋喃二羧酸二价阴离子,Sol为N,N-二甲基乙酰胺,a为2、b为2、c为1、d为1、e为0,Ac为乙酰基,具体制备方法如下:
将0.026g(0.1mmol)Mg(NO3)2·6H2和0.008g(0.05mmol)2,5-呋喃二羧酸加入3.5mL N,N-二甲基乙酰胺与蒸馏水体积比为6:1的混合液中,搅拌均匀,密封,120℃恒温静置反应12天,制备成镁-芳香羧酸多孔配合物,根据Mg计算产率约为38%。所制备的镁-芳香羧酸多孔配合物的单晶结构如图3所示,属于四方晶系,I4/mmm空间群,晶胞参数a为b为c为 α为90°,β为90°,γ为90°,其独立单元中存在两个独立的Mg(II)离子、两个2,5-呋喃二羧酸配体分子以及一个Ac-分子(由溶剂分子N,N-二甲基乙酰胺分子加热分解而来)。Mg1通过六配位的变形八面体模式与四个2,5-呋喃二羧酸配体羧基氧原子O2、O2B、O2B、O2C以及两个Ac-分子上的O1、O1A原子配位。Mg2同样采用六配位的变形八面体配位模式与三个来自于2,5-呋喃二羧酸配体羧基氧原子O3A、O3B、O3D及两个Ac-分子上的O1、O1A原子配位。由图4可见,所制备的镁-芳香羧酸多孔配合物为三维网络结构。
实施例3
实施例1和2制备的配合物在检测硝基苯和对硝基甲苯中的应用
采用PELS55荧光光谱仪进行实施例1和2制备的镁-芳香羧酸多孔配合物对硝基苯(NB)、邻硝基甲苯(2-NT)、硝基甲烷(NM)的荧光猝灭研究,结果见图5~10。
由图5可见,随着加入NB溶液浓度的增大,实施例1制备的配合物的荧光发射强度逐渐降低。当加入的NB溶液的浓度达到5000ppm时,配合物发生荧光猝灭。经计算,该镁-芳香羧酸多孔配合物在上述浓度下对硝基苯的猝灭率KSV(KSV=I0-I/I0(I0为不加硝基化合物溶液时各化合物溶液的荧光强度,I为加入硝基化合物溶液浓度为M时对应的荧光强度))可达96.02%。由图6可见,随着加入2-NT溶液浓度的增大,实施例1制备的配合物的荧光发射强度逐渐降低,且在8000ppm时未达到完全猝灭。经计算,该配合物在上述浓度下对邻硝基甲苯的猝灭率KSV为84.98%。由图7可见,随着加入NM溶液浓度的增大,实施例1制备的配合物的荧光发射强度小幅度逐渐降低,且在8000ppm时均不能达到猝灭。经计算,该配合物在上述浓度下对硝基甲烷的猝灭率KSV仅为11.76%。上述实验结果表明,实施例1制备的镁-芳香羧酸多孔配合物可以被开发成具有环保意义的荧光传感器来检测环境中的硝基苯和邻硝基甲苯,同时排除硝基甲烷的干扰。
由图8可见,随着加入NB溶液浓度的增大,实施例2制备的配合物的荧光发射强度逐渐降低。当加入的NB溶液的浓度达到8000ppm时,配合物发生荧光猝灭。经计算,该镁-芳香羧酸多孔配合物在上述浓度下对硝基苯的猝灭率KSV(KSV=I0-I/I0(I0为不加硝基化合物溶液时各化合物溶液的荧光强度,I为加入硝基化合物溶液浓度为M时对应的荧光强度))可达96.61%。由图9可见,随着加入2-NT溶液浓度的增大,实施例2制备的配合物的荧光发射强度逐渐降低,且在8000ppm时未达到完全猝灭。经计算,该配合物在上述浓度下对邻硝基甲苯的猝灭率KSV为72.08%。由图10可见,随着加入NM溶液浓度的增大,实施例2制备的配合物的荧光发射强度小幅度逐渐降低,且在8000ppm时均不能达到猝灭。经计算,该配合物在上述浓度下对硝基甲烷的猝灭率KSV仅为20.48%。上述实验结果表明,实施例2制备的镁-芳香羧酸多孔配合物可以被开发成具有环保意义的荧光传感器来检测环境中的硝基苯和邻硝基甲苯,同时排除硝基甲烷的干扰。
Claims (5)
1.一类具有荧光传感能力的镁-芳香羧酸多孔配合物,其特征在于:该配合物的结构单元为Mga(L1)b(Sol)c(Ac)d(H2O)e;
式中L1为脱去三个羧基上氢原子的4,4',4”-均苯三苯甲酸三价阴离子,Sol为N-甲基乙酰胺,Ac为乙酰基,a为9、b为8、c为12、d为6、e为6,其属于三方晶系,R-3空间群,晶胞参数a为b为c为 α为90°,β为90°,γ为120°;
或者L1为脱去两个羧基上氢原子的2,5-呋喃二羧酸二价阴离子,Sol为N,N-二甲基乙酰胺,Ac为乙酰基,a为2、b为2、c为1、d为1、e为0,其属于四方晶系,I4/mmm空间群,晶胞参数a为b为c为 α为90°,β为90°,γ为90°。
2.一种权利要求1的镁-芳香羧酸多孔配合物的制备方法,该配合物的结构单元为Mg9(L1)8(Sol)12(Ac)6(H2O)6,式中L1为脱去三个羧基上氢原子的4,4',4”-均苯三苯甲酸三价阴离子,Sol为N-甲基乙酰胺,Ac为乙酰基,其特征在于:将4,4',4”-均苯三苯甲酸、4,4'-联吡啶、六水合硝酸镁按摩尔比为1:1~1.5:2~2.5加入N-甲基乙酰胺与乙醇体积比为4~4.5:1的混合液中,搅拌均匀,密封,90~100℃恒温静置反应7天,制备成镁-芳香羧酸多孔配合物。
3.一种权利要求1的镁-芳香羧酸多孔配合物的制备方法,该配合物的结构单元为Mg2(L1)2(Sol)(Ac),式中L1为脱去两个羧基上氢原子的2,5-呋喃二羧酸二价阴离子,Sol为N,N-二甲基乙酰胺,Ac为乙酰基,其特征在于:将2,5-呋喃二羧酸、六水合硝酸镁按摩尔比为1:2~2.5加入N,N-二甲基乙酰胺与蒸馏水体积比为6~6.5:1的混合液中,搅拌均匀,密封,120~130℃恒温静置反应12天,制备成镁-芳香羧酸多孔配合物。
4.权利要求1所述的具有荧光传感能力的镁-芳香羧酸多孔配合物在检测硝基苯中的用途。
5.权利要求1所述的具有荧光传感能力的镁-芳香羧酸多孔配合物在检测邻硝基甲苯中的用途。
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