CN106188110B - 一种金属-有机骨架功能化荧光材料和制备方法及其应用 - Google Patents
一种金属-有机骨架功能化荧光材料和制备方法及其应用 Download PDFInfo
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Abstract
一种金属‑有机骨架功能化荧光材料和制备方法及其应用,属于荧光检测领域。化学结构式为:[(CH3)2NH2]2[Eu6(μ3‑OH)8(BDC‑NH2)6(H2O)6],以2‑氟苯甲酸作为调节剂,有机配体2‑氨基对苯二甲酸与硝酸铕在N,N‑二甲基甲酰胺(DMF)、硝酸和水的混合溶液中,经由热反应得到八面体结构的荧光材料。所述热反应的反应条件为在玻璃耐压瓶中,120℃,反应时间为20h。用于金属阳离子、阴离子、有机溶剂小分子的荧光检测,可选择性识别Cu2+,Fe3+,Cr2O7 2‑,丙酮。
Description
技术领域
本发明涉及一种金属骨料,设计一种金属-有机骨架材料,应用于金属阳离子,阴离子以及有机溶剂小分子的识别检测,属于荧光检测领域。
背景技术
随着社会的发展,科技的进步。物质检测在生命科学,环境科学,医学以及核工业等众多领域有着越来越重要的作用。在众多的检测方法中,荧光检测由于灵活快捷以及高灵敏度得到了广泛的关注。其中,镧系金属荧光材料具有色泽鲜明,荧光寿命长,从紫外到近红外宽发射范围,以及大的斯托克斯位移的特点。金属-有机骨架材料是通过无机金属离子或簇与有机配体经过化学自组装形成。具有较高的比表面积和孔隙率,可调控的孔道尺寸,其在气体存贮、吸附分离、催化、化学传感以及药物传送等方面拥有广泛应用前景。
镧系金属有机骨架材料继承了金属骨料的高比表面积等特点,同时又具有了镧系金属材料优异的荧光性能。可应用于金属阳离子,阴离子,有机溶剂小分子的识别检测。
发明内容
本发明的目的在于提供一种八面体金属有机骨架功能化荧光材料、制备方法及其应用。
本发明的一种八面体金属有机骨架功能化荧光材料,Eu-BDC-NH2,其特征在于,化学结构式为:[(CH3)2NH2]2[Eu6(μ3-OH)8(BDC-NH2)6(H2O)6],可用于金属阳离子、阴离子、有机溶剂小分子的荧光检测。金属离子选自K+,Hg2+,Mg2+,Mn2+,Ni2+,Cu2+,Fe3+;阴离子选自F-,Cl-,NO2 -,SO4 2-,CO3 2-,HCO3 -,Cr2O7 2-;有机溶剂小分子选自丙酮,二氯甲烷,三氯甲烷,甲醇,乙醇,乙醚,乙酸乙酯。
本发明的一种八面体金属有机骨架功能化荧光材料,其特征在于,晶体属于立方体晶系,空间群为Fm-3m,晶胞参数为: β=96.0160°,α=γ=90°。每个金属铕离子分别与4个μ3-OH的氧原子以及4个羧基上的4个氧原子链接;金属铕离子第九个配位点为水分子;相邻的金属铕离子通过μ3-OH基团和脱质子化的羧酸基团桥连,以双齿化的方式形成12连接的六核簇分子结构单元[Eu6(μ3-OH)8(O2C-)12]。每个六核簇分子结构单元通过阴离子桥接配体BDC-NH2 2-形成一个三维周期性的金属-有机骨材料。
本发明上述所述的八面体金属-有机骨架功能化荧光材料的制备方法,其特征在于,包括以下步骤:
以2-氟苯甲酸作为调节剂,有机配体2-氨基对苯二甲酸与硝酸铕在N,N-二甲基甲酰胺(DMF)、硝酸和水的混合溶液中,经由热反应得到八面体结构的荧光材料。所述热反应的反应条件为在玻璃耐压瓶中,120℃,反应时间为20h。
将所得混合液经过滤或离心得到固体沉淀,用N,N-二甲基甲酰胺,二氯甲烷对固体沉淀进行多次洗涤,以去除孔道内残留的原料和杂质;所得固体产物烘干,得到活化后的材料。
优选,有机配体2-氨基对苯二甲酸:2-氟苯甲酸:硝酸铕:N,N-二甲基甲酰胺(DMF)、3.5摩尔/升硝酸:水用量关系为0.048毫摩尔:0.214毫摩尔:0.0413毫摩尔:2.2毫升:0.1毫升:0.25毫升。
本发明的金属-有机骨架功能化荧光材料作为检测探针,用于多种物质的检测。可用于金属阳离子、阴离子、有机溶剂分子的荧光检测。金属离子选自K+,Hg2+,Mg2+,Mn2+,Ni2+,Cu2+,Fe3+;阴离子选自F-,Cl-,NO2 -,SO4 2-,CO3 2-,HCO3 -,Cr2O7 2-;有机溶剂小分子选自丙酮,二氯甲烷,三氯甲烷,甲醇,乙醇,乙醚,乙酸乙酯。
本发明采用滴定法对特定金属阳离子,阴离子,有机溶剂小分子进行识别检测。配置待检测物质的N,N二甲基甲酰胺溶液,在溶液中加入一定量的金属有机骨架材料,整个体系在10ml离心管中进行,将其置于超声仪中震荡,使其充分分散。其后发现可分别选择性识别Cu2+,Fe3+,Cr2O7 2-,丙酮等。
附图说明
图1晶体结构图;
图2功能化荧光材料Eu-BDC-NH2在不同金属阳离子的DMF溶液中的荧光强度图。
图3功能化荧光材料Eu-BDC-NH2在不同阴离子的DMF溶液中的荧光强度图。
图4功能化荧光材料Eu-BDC-NH2在不同有机溶剂纯溶液中的荧光强度图。
具体实施方式
下面结合实施例对本发明作进一步说明,但本发明并不限于以下实施例。
实施例1
所述材料Eu-BDC-NH2的合成
有机配体2-氨基对苯二甲酸(0.048毫摩尔)、调节剂2-氟苯甲酸(0.214毫摩尔)与硝酸铕(0.0413毫摩尔)在N,N-二甲基甲酰胺(2.2毫升)、硝酸(0.1毫升3.5摩尔/升)和水(0.25毫升)的混合溶液中,120℃加热40h,随后冷却到室温。得到的淡黄色八面晶体用DMF、二氯甲烷溶剂反复多次洗涤,并室温烘干。
实施例2
所述材料Eu-BDC-NH2检测Cu2+、Fe3+
取2mg所述材料Eu-BDC-NH2浸入含有不同金属阳离子M+的DMF溶液中,0.01mol/L,M+(M+=K+,Hg2+,Mg2+,Mn2+,Ni2+,Cu2+,Fe3+),并检测其荧光强度。
实施例3
所述材料Eu-BDC-NH2检测Cr2O7 2-
取2mg所述材料Eu-BDC-NH2浸入含有不同阴离子的DMF溶液中,0.01mol/L,(F-,Cl-,NO2 -,SO4 2-,CO3 2-,HCO3 -,Cr2O7 2-),并检测其荧光强度。
实施例4
所述材料Eu-BDC-NH2检测丙酮
取2mg所述材料Eu-BDC-NH2浸入含有不同有机溶剂的纯溶液中,(丙酮,二氯甲烷,三氯甲烷,甲醇,乙醇,乙醚,乙酸乙酯),并检测其荧光强度。
晶体结构测定:
表1配合物的晶体学数据
Claims (1)
1.一种八面体金属有机骨架功能化荧光材料的应用,Eu-BDC-NH2,八面体金属有机骨架功能化荧光材料化学结构式为:[(CH3)2NH2]2[Eu6(μ3-OH)8(BDC-NH2)6(H2O)6],其特征在于,作为检测探针,用于阴离子的荧光检测;阴离子选自F-,Cl-,NO2 -,SO4 2-,CO3 2-,HCO3 -,Cr2O7 2-;配置待检测物质的N,N二甲基甲酰胺溶液,在溶液中加入金属有机骨架材料,将其置于超声仪中震荡,使其充分分散,即可检测;该应用适用于非诊断与治疗目的。
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