CN105481900A - 一种用于金属离子污染物检测的过渡金属-有机框架材料 - Google Patents
一种用于金属离子污染物检测的过渡金属-有机框架材料 Download PDFInfo
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Abstract
本发明涉及一种发光金属有机框架在金属离子污染物检测中的应用。本发明合成的发光金属有机框架可以作为荧光传感材料用于金属离子污染物的检测。其荧光强度随着金属离子污染物浓度的增加而逐渐发生变化。因而,在金属离子污染物检测和识别中具有潜在的应用。
Description
技术领域
本发明涉及一种发光金属有机框架在金属离子污染物检测中的应用。
技术背景
随着人类社会的发展,科学技术在给人们带来高品质生活的同时,也产生了一系列负面因素,其中当属环境污染问题最为严重。有毒重金属如铜、铁、铅等,作为工业生产过程中所排放的物质,由于大部分可以转化为可溶性阳离子而存在于水体、土壤当中,并通过食物链等途径直接或间接被人体吸收,从而对人类健康和地球自然生态环境造成巨大的危害。现有的检测技术如如原子光谱法、电化学分析法、X射线荧光光谱法等检测手段都存在检测仪器价格昂贵,分析步骤繁琐冗长等缺点,不能满足现场快速检测的需要。因此,为了保护生态环境和人类的健康,开发出高效、快速、准确的能够用于环境和生物检测的探测材料变得越来越重要。
发光金属有机框架化合物,是一类孔隙率高、比表面积大、孔结构可控、化学性质稳定和制备过程简单的新型多孔晶态发光材料。最近研究表明,该类材料在荧光传感检测方面具有检测速度快、灵敏度高、选择性好等优点,成为新一代的理想发光传感材料。发光金属有机框架材料作为新一代固态发光材料,其组成中的金属单元、有机配体单元以及客体分子等都可以作为发光的来源,并且这些组成单元可选择的范围广,通过有机地组合不同的组分单元,可以实现金属有机框架材料不同的发光性能。文献上有关用金属配合物来检测和识别金属离子污染物的报道还很少。我们选择以苯环为中心,并引入多配位点的羧基基团和极性酰胺基团,使配体不仅能以多种灵活的配位方式与金属离子键合形成多孔的发光金属有机框架材料,而且可以通过利用酰胺基团与客体分子之间的相互作用引起金属有机框架材料的发光行为变化的特性,实现对客体分子的选择性识别和检测。基于以上分析我们探究了以二-(3,5-二羧基苯基)对苯二甲酰胺作为有机配体与金属锰离子构筑的发光金属有机配合物在金属离子污染物检测中的应用。
发明内容
本发明的目的在于探究了一种发光金属有机框架在金属离子污染物检测中的应用,从而为实现快速、简便、灵敏地检测环境中金属离子污染物提供了实验基础。
为实现上述目的,本发明采用下述技术方案:
本发明采用溶剂热法制备了二-(3,5-二羧基苯基)对苯二甲酰胺(H4L)和MnSO4形成的发光金属有机配合物,其具体制备过程为:
将MnSO4、H4L配体、邻菲罗啉、DMF和水的混合物置于聚四氟乙烯内胆中,在85℃下恒温反应3天,然后自然冷却至室温,过滤,所得产物用DMF洗涤,室温干燥,得到块状晶体。
采用以上方法制备了一种发光金属有机框架。
本发明的发光金属有机框架对金属离子污染物,如Ag+,Na+,Ni2+,Co2+,Pb2+,Zn2+,Ba2+,Ca2+,Mg2+,Al3+,Cu2+和Fe3+等进行了荧光传感研究。
本发明的金属有机框架快速检测金属离子污染物的方法为,以Fe3+和Cu2+的检测为例:
制作荧光强度和物质的量的响应曲线:首先测定Fe3+不存在时传感材料的荧光强度F0,然后加入梯度物质的量的Fe3+,测定Fe3+存在时传感材料的荧光强度F,当Fe3+物质的量增大到0.10μmol时,配合物的荧光强度淬灭了88.11%。目前尚未见有文献或者专利利用此配合物检测环境中Fe3+。
制作荧光强度和物质的量的响应曲线:首先测定Cu2+不存在时传感材料的荧光强度F0,然后加入梯度物质的量的Cu2+,测定Cu2+存在时传感材料的荧光强度F,当Cu2+的量增大至0.10μmol时,配合物的荧光强度淬灭了50.51%。目前尚未见有文献或者专利利用此配合物检测环境中Cu2+。
同理对Ag+,Na+,Ni2+,Co2+,pb2+,Zn2+,Ba2+,Ca2+,Mg2+和Al3+的检测效果见附图。
这充分说明了本发明所提供的荧光传感材料可用于金属离子污染物检测。
本发明所提供的发光金属有机框架应用具有如下特点:
1.合成的发光金属有机框架通过对Ag+,Na+,Ni2+,Co2+,Pb2+,Zn2+,Ba2+,Ca2+,Mg2+,Al3+,Cu2+和Fe3+的传感性能,可用作传感器中敏感材料的研制开发或者用于环境中金属离子污染物的检测。
2.合成的发光金属有机框架材料在金属离子检测方面具有快速、简便、灵敏等优点。
综上所述,本发明提供了一种通过发光金属有机框架的发光性质检测被分析物的一种方法,所述的被检测物包括各种金属离子污染物。因此,在环境检测等方面有广泛的应用前景。
附图说明
图1为所合成的发光金属有机框架对不同物质的量的Ba2+的荧光响应曲线;
图2为所合成的发光金属有机框架对不同物质的量的Fe3+的荧光响应曲线;
图3为所合成的发光金属有机框架对不同物质的量的Cu2+的荧光响应曲线;
图4为所合成的发光金属有机框架对不同物质的量的Al3+的荧光响应曲线;
图5为所合成的发光金属有机框架对不同物质的量的Co2+的荧光响应曲线;
具体实施方式
实施例1配合物的合成:
将H4L(24.6mg,0.05mmol)、MnSO4(15.0mg,0.1mmol)、邻菲罗啉(18.0mg,0.1mmol),4mLDMF(N,N-二甲基甲酰胺)、2mLH0O和0.1mL浓硝酸的混合物置于聚四氟乙烯内胆中,在85℃下恒温反应3天,然后自然冷却至室温,过滤,所得产物用DMF洗涤,室温干燥,得到块状晶体。
实施例2(Ba2+传感),过程如下:
首先测定Ba2+不存在时传感材料的荧光强度F0,然后加入梯度物质量的Ba2+(0μmol、0.005μmol、0.01μmol、0.02μmol、0.03μmol、0.04μmol、0.06μmol、0.08μmol、0.10μmol),测定不同物质的量Ba2+存在时传感材料的荧光强度F,绘制出荧光强度F随Ba2+物质的量变化的曲线,见图1,测试结果表明,其荧光强度随着Ba2+物质的量不断增加而逐渐淬灭;在加入Ba2+物质的量达到0.10μmol时,配合物的荧光强度淬灭了23.59%。
实施例3(Fe3+传感),过程如下:
首先测定Fe3+不存在时传感材料的荧光强度F0,然后加入梯度物质量的Fe3+(0μmol、0.005μmol、0.01μmol、0.02μmol、0.03μmol、0.04μmol、0.06μmol、0.08μmol、0.10μmol),测定不同物质的量Fe3+存在时传感材料的荧光强度F,绘制出荧光强度F随Fe3+物质的量变化的曲线,见图2,测试结果表明,其荧光强度随着Fe3+物质的量不断增加而逐渐淬灭;在加入Fe3+物质的量达到0.10μmol时,配合物的荧光淬灭程度达到了88.11%。
实施例4(Cu2+传感),过程如下:
首先测定Cu2+不存在时传感材料的荧光强度F0,然后加入梯度物质量的Cu2+(0μmol、0.005μmol、0.01μmol、0.02μmol、0.03μmol、0.04μmol、0.06μmol、0.08μmol、0.10μmol),测定不同物质的量Cu2+存在时传感材料的荧光强度F,绘制出荧光强度F随Cu2+物质的量变化的曲线,见图3,测试结果表明,其荧光强度随着Cu2+物质的量不断增加而逐渐淬灭;在加入Cu2+物质的量达到0.10μmol时,配合物的荧光淬灭程度达到了50.51%。
实施例5(Al3+传感),过程如下:
首先测定Al3+不存在时传感材料的荧光强度F0,然后加入梯度物质量的Al3+(0μmol、0.005μmol、0.01μmol、0.02μmol、0.03μmol、0.04μmol、0.06μmol、0.08μmol、0.10μmol),测定不同物质的量Al3+存在时传感材料的荧光强度F,绘制出荧光强度F随Al3+物质的量变化的曲线,见图4,测试结果表明,其荧光强度随着pb2+物质的量不断增加而逐渐增强;在加入Al3+物质的量达到0.10μmol时,配合物的荧光增强程度达到了210.28%。
实施例6(Co2+传感),过程如下:
首先测定Co2+不存在时传感材料的荧光强度F0,然后加入梯度物质量的Co2+(0μmol、0.005μmol、0.01μmol、0.02μmol、0.03μmol、0.04μmol、0.06μmol、0.08μmol、0.10μmol),测定不同物质的量Co2+存在时传感材料的荧光强度F,绘制出荧光强度F随Co2+物质的量变化的曲线,见图5,测试结果表明,其荧光强度随着Co2+物质的量不断增加而逐渐增加;在加入Co2+物质的量达到0.10μmol时,配合物的荧光淬灭程度达到了35.07%。
Claims (7)
1.一种可用于金属离子污染物检测的发光金属有机框架的制备方法,采用溶剂热法制备金属锰盐、二-(3,5-二羧基苯基)对苯二甲酰胺(H4L)配体和邻菲罗啉形成的发光金属有机框架,其具体制备过程为:H4L配体、MnSO4和邻菲罗啉按摩尔比1∶2∶2混合溶于溶剂置于聚四氟乙烯内胆中,在85℃下恒温反应3天,然后自然冷却至室温,过滤,所得产物用DMF洗涤,室温干燥,得到块状晶体。
2.权利要求1所述的发光金属有机框架在金属离子污染物检测中的应用。
3.如权利要求2所述的应用,所述金属离子Ag+,Na+,Ni2+,Co2+,Pb2+,Zn2+,Ba2+,Ca2+,Mg2+,Al3+,Cu2+和Fe3+等。
4.如权利要求2或3所述的应用,检测方法为:(1)制作荧光强度和物质的量的响应曲线:首先测定金属离子不存在时传感材料的荧光强度F0,然后加入梯度物质的量的金属离子,测定金属离子存在时传感材料的荧光强度F,绘制出发光金属有机框架对不同金属离子荧光响应图。
5.按权利要求3所示,金属离子污染物与金属有机框架可以产生相互作用,从而导致配合物的荧光增强或者淬灭。
6.按权利要求4所述的方法,其特征在于所述溶剂为DMA,发光金属有机框架和溶剂的配比为3mg∶3mL。
7.按权利要求4所述的方法,加入梯度物质量的Fe3+(0μmol、0.005μmol、0.01μmol、0.02μmol、0.03μmol、0.04μmol、0.06μmol、0.08μmol、0.10μmol);Al3+,Cu2+,Mg2+,Ca2+,Ba2+,Ag+,Na+,Ni2+,Co2+,Pb2+和Zn2+的加入量如上所述。
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CN107235838A (zh) * | 2017-05-05 | 2017-10-10 | 浙江大学 | 用于重金属铅离子探测的金属‑有机框架材料及其制备方法 |
CN107936954A (zh) * | 2017-11-26 | 2018-04-20 | 山西大学 | 一种二维镉有机骨架配合物及其制备方法与应用 |
CN110628037A (zh) * | 2019-09-12 | 2019-12-31 | 重庆师范大学 | 黄色荧光的混配体锰超分子聚合物及其制备方法与应用 |
CN113185969A (zh) * | 2021-04-29 | 2021-07-30 | 浙江大学 | 一种用于水体中金属离子实时检测的荧光薄膜及其制备方法 |
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CN107235838A (zh) * | 2017-05-05 | 2017-10-10 | 浙江大学 | 用于重金属铅离子探测的金属‑有机框架材料及其制备方法 |
CN107235838B (zh) * | 2017-05-05 | 2019-09-06 | 浙江大学 | 用于重金属铅离子探测的金属-有机框架材料及其制备方法 |
CN107936954A (zh) * | 2017-11-26 | 2018-04-20 | 山西大学 | 一种二维镉有机骨架配合物及其制备方法与应用 |
CN107936954B (zh) * | 2017-11-26 | 2019-11-19 | 山西大学 | 一种二维镉有机骨架配合物及其制备方法与应用 |
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