CN106977748A - 均苯三甲酸锌聚合物的制备、结构及其荧光性质 - Google Patents
均苯三甲酸锌聚合物的制备、结构及其荧光性质 Download PDFInfo
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Abstract
本发明公开了一种锌聚合物的制备、结构及其荧光性质。该锌聚合物属于三斜晶系,空间群为
Description
技术领域
本发明属于配合物制备技术领域,特别涉及一种锌配位聚合物的制备、结构及其荧光性质。
背景技术
有机配体桥连金属离子或原子簇形成一维至三维无限伸展的结构。结构多样的有机配体能够和许多金属离子反应形成结构各异且具有特殊性质的配位聚合物。由于羧基含有两个能与金属离子配位的氧原子,配位方式多种多样,所以多羧酸类有机配体成为人们常用的一种配体。氮杂环类的配体,也能发生配位,对称性的杂环类配体(如吡嗪)也能起到桥连金属离子的作用,从而得到有微孔结构的金属配合物。
发明内容
本发明的目的是提供一种锌聚合物的制备、结构及其荧光性质。
本发明的思路:利用均苯三甲酸、吡嗪为配体与硝酸锌通过水热法获得锌配位聚合物。
均苯三甲酸锌聚合物的结构见附图1。该配合物属于三斜晶系,空间群为Pī,基本结构单元中包含两个锌离子,三分之四个均苯三甲酸阴离子,二分之一个吡嗪分子,六个配位水和两个游离的水分子。Zn(II)离子都是六配位的。Zn1分别与来自两个不同的均苯三甲酸阴离子中的羧基氧原子(O3、O5A、O6A),一个吡嗪分子的氮原子(N1),两个水分子的氧原子(O9、O10)配位。Zn2分别与来自两个不同的均苯三甲酸阴离子中的羧基氧原子(O1、O1B),四个水分子的氧原子(O7、O8、O7A、O8A)配位。Zn-O键长在之间,Zn-N键长是
该锌配位聚合物的制备方法为:
(1)称量0.1~0.5毫摩尔均苯三甲酸溶解于5~10毫升蒸馏水中,将溶液移入容积为25毫升的密封反应釜中;
(2)称量0.3~1.5毫摩尔氢氧化钾,并加入步骤(1)中;
(3)称量0.1~0.5毫摩尔的吡嗪溶解于2~5毫升蒸馏水中,并加入步骤(1)中;
(4)称量0.2~1毫摩尔硝酸锌溶于5~10毫升的蒸馏水中,将溶液加入到步骤(1)中;
(5)将反应釜密封,在120℃下恒温2天,然后缓慢冷却至室温,过滤,得到白色块状晶体,即为锌配位聚合物。
本发明具有工艺简单、成本低廉、重复性好等优点,成功的合成了锌配位聚合物,为合成过渡金属的配合物提供了一定的依据。
在室温下测试了配体和配合物的固体荧光发射光谱,如附图2所示。结果表明,配体和配合物都具有荧光性,配合物最大发射波长为469nm(激发波长为270nm),相比于配体Py-3-CA的323nm(激发波长为290nm)发生了146nm的红移。说明配合物具有良好的荧光性能。
附图说明
图1是本发明的锌配合物的分子结构图。
图2是配合物与配体的荧光图。
具体实施方式
实施例:
(1)称量0.2毫摩尔均苯三甲酸(0.0414g)溶解于5毫升蒸馏水中,将溶液移入容积为25毫升的密封反应釜中;
(2)称量0.6毫摩尔氢氧化钾(0.0336g),并加入步骤(1)中;
(3)称量0.3毫摩尔的吡嗪(0.0240g)溶解于2毫升蒸馏水中,并加入步骤(1)中;
(4)称量0.2毫摩尔硝酸锌(0.0594g)溶于5毫升的蒸馏水中,将溶液加入到步骤(1)中;
(5)将反应釜密封,在120℃下恒温2天,然后缓慢冷却至室温,过滤,得到灰色块状晶体,即为锌配位聚合物。
所述锌配合物属于三斜晶系,空间群为Pī,基本结构单元中包含两个锌离子,三分之四个均苯三甲酸阴离子,二分之一个吡嗪分子,六个配位水和两个游离的水分子。Zn(II)离子都是六配位的。Zn1分别与来自两个不同的均苯三甲酸阴离子中的羧基氧原子(O3、O5A、O6A),一个吡嗪分子的氮原子(N1),两个水分子的氧原子(O9、O10)配位。Zn2分别与来自两个不同的均苯三甲酸阴离子中的羧基氧原子(O1、O1B),四个水分子的氧原子(O7、O8、O7A、O8A)配位。Zn-O键长在之间,Zn-N键长是
Claims (3)
1.一种锌配位聚合物的结构。该配合物属于三斜晶系,空间群为Pī,基本结构单元中包含两个锌离子,三分之四个均苯三甲酸阴离子,二分之一个吡嗪分子,六个配位水和两个游离的水分子。Zn(II)离子都是六配位的。Zn1分别与来自两个不同的均苯三甲酸阴离子中的羧基氧原子(O3、O5A、O6A),一个吡嗪分子的氮原子(N1),两个水分子的氧原子(O9、O10)配位。Zn2分别与来自两个不同的均苯三甲酸阴离子中的羧基氧原子(O1、O1B),四个水分子的氧原子(O7、O8、O7A、O8A)配位。Zn-O键长在之间,Zn-N键长是
2.根据权利要求1所述的锌配位聚合物的制备方法,其特征在于具体步骤为:
(1)称量0.2毫摩尔均苯三甲酸溶解于5毫升蒸馏水中,将溶液移入容积为25毫升的密封反应釜中;
(2)称量0.6毫摩尔氢氧化钾,并加入步骤(1)中;
(3)称量0.3毫摩尔的吡嗪溶解于2毫升蒸馏水中,并加入步骤(1)中;
(4)称量0.5毫摩尔硝酸锌溶于5毫升的蒸馏水中,将溶液加入到步骤(1)中;
(5)将反应釜密封,在120℃下恒温2天,然后缓慢冷却至室温,过滤,得到白色块状晶体,即为锌配位聚合物。
3.配合物的荧光性质
在室温下测试了配体和配合物的固体荧光的发射光谱。结果表明,配体和配合物都具有荧光性,配合物最大发射波长为469nm(激发波长为270nm),相比于配体的323nm(激发波长为290nm)发生了146nm的红移。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108586768A (zh) * | 2018-06-11 | 2018-09-28 | 上海大学 | 二维锌配位聚合物及其制备方法 |
CN111825851A (zh) * | 2020-08-11 | 2020-10-27 | 盐城工学院 | 一种基于pbp和多羧酸配体的发光金属-有机框架材料及其制备方法和应用 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108586768A (zh) * | 2018-06-11 | 2018-09-28 | 上海大学 | 二维锌配位聚合物及其制备方法 |
CN111825851A (zh) * | 2020-08-11 | 2020-10-27 | 盐城工学院 | 一种基于pbp和多羧酸配体的发光金属-有机框架材料及其制备方法和应用 |
CN111825851B (zh) * | 2020-08-11 | 2022-04-05 | 盐城工学院 | 一种基于pbp和多羧酸配体的发光金属-有机框架材料及其制备方法和应用 |
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