CN109251214B - 一种锌配合物及其制备方法和用途 - Google Patents
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- 239000011701 zinc Substances 0.000 title claims abstract description 23
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000010668 complexation reaction Methods 0.000 title description 2
- 239000013078 crystal Substances 0.000 claims abstract description 14
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- FEBRHATXLQPYLJ-UHFFFAOYSA-N 4-(1h-pyrazol-5-yl)pyridine Chemical compound N1N=CC=C1C1=CC=NC=C1 FEBRHATXLQPYLJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 239000007850 fluorescent dye Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000005284 excitation Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 150000003504 terephthalic acids Chemical class 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 150000003751 zinc Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- C07F3/06—Zinc compounds
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Abstract
本发明公开了一种锌配合物及其制备方法和用途，锌配合物的分子式为：C16H13N3O5Zn分子量为392.66。其制备方法是将4‑(1H‑吡唑‑3‑基)吡啶、对苯二甲酸和硝酸锌放入高压反应釜中，然后加入水中，在120°C的条件下反应得到块状晶体。该材料在370nm的入射光照射下产生很强的蓝色荧光，并且通过荧光的强度变化可以选择性识别水中的三价铁离子。本发明工艺简单、化学组分易于控制、重复性好且产量高。
Description
技术领域
本发明涉及一种锌配合物的制备与应用，包括对金属离子的识别。
背景技术
荧光探针因其在环境及生物化学领域的广泛应用而倍受关注，特别是快速、灵敏度地检测有毒的小分子或与生命活动相关的金属阳离子更是科研人员面临的重要的研究课题之一，比如铁离子的快速灵敏识别具有很重要的意义。与传统的环境检测分析方法相比，荧光法由于具有选择性好、灵敏度好、仪器简单、操作简便等优点而倍受分析工作者的关注，已成为一种快速、敏灵、高效的分析检测技术。如何制备高灵敏度和高选择性的识别小分子仍有待进一步研究。
发明内容
本发明的目的是设计合成新型锌配合物{[Zn(C8H7N3)(C8H4O4)]•H2O}n，并同时提供其制备方法和用途。
本发明一方面提供了一种锌配合物，其分子式为：C16H13N3O5Zn，分子量为392.66，结构式为{[Zn(C8H7N3)(C8H4O4)]•H2O}n，其中C8H7N3为4-(1H-吡唑-3-基)吡啶，C8H4O4为去质子的对苯二甲酸；其在370nm波长的激发下，可以发射出蓝色荧光, 通过单晶衍射仪测定其结构，晶体学参数如下：
本发明另一方面提供了一种锌配合物的制备方法，具体步骤为：将0.016-0.16 g对苯二甲酸、0.016-0.16g4-(1H-吡唑-3-基)吡啶和0.030-0.3 g硝酸锌混合，然后加入10-100ml水中，搅拌10分钟，然后放在120℃的烘箱中静止72h后，冷却得到无色的块状晶体即{[Zn(C8H7N3)(C8H4O4)]•H2O}n。
本发明最后一方面提供了一种上述锌配合物的用途，其可以在多种常见金属离子的水溶液中，应用于对Fe3+的识别，应用于荧光探针。
本发明具有工艺简单、化学组分易于控制、重复性好并产量高等优点。
附图说明
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其它的附图。
图1 {[Zn(C8H7N3)(C8H4O4)]•H2O}n的晶体学不对称单元图。
图2 分散于不同金属离子水溶液中的锌配合物的荧光发射谱图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面结合具体实施例对发明进行清楚、完整的描述。
实施例1
将0.016 g对苯二甲酸、0.016g 4-(1H-吡唑-3-基)吡啶和0.030g硝酸锌混合，然后加入10ml水中，搅拌10分钟，然后放在120℃的烘箱中静止72h后，冷却得到无色的块状晶体。
使用如下仪器及方法对产物进行表征：1、挑选尺寸为0.25×0.25×0.24 mm3的晶体用于单晶结构分析，单晶衍射数据在Bruker-AXS SMART APEX2 CCD衍射仪上收集，用石墨单色器单色化的Mokα射线（λ＝0.71073 Å），3.06°≤θ≤27.72°。所得化合物属于三斜晶系，空间群皆为P-1，晶胞参数大约为a = 8.4055 Å，b = 9.5590 Å，c = 11.305 Å，α=68.11°，β= 87.42°，γ= 69.37°。晶体结构见图1，（使用Diamond软件绘制），晶体参数如表1：
实施例2
将0.16 g对苯二甲酸、0.16g 4-(1H-吡唑-3-基)吡啶和0.3 g硝酸锌混合，然后加入100ml水中，搅拌10分钟，然后放在120℃的烘箱中静止72h后，冷却得到无色的块状晶体。
实施例3
使用了八种金属离子水溶液作为待测物，分别为：Zn2+, Cd2+, Co2+, Ni2+, Mg2+,Mn2+, Cu2+, 和Fe3+。研究了锌配合物在各种离子水溶液中的荧光特性。称量3 mg 锌配合物于3ml以上溶剂中，超声3-4分钟，使锌配合物良好分散于液体中 (λex=370nm，狭缝宽度为1.5nm)，测试锌配合物在液体介质中的发光特性。结果表明只有Fe3+中锌配合物的荧光淬灭明显，这也表明了该材料有潜力作为特异性识别Fe3+的荧光探针，结果如图2所示。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明实施例技术方案的精神和范围。
Claims (2)
1.一种锌配合物的制备方法，特征在于，所述锌配合物的分子式为：C16H13N3O5Zn，分子量为392.66，结构式为{[Zn(C8H7N3)(C8H4O4)]•H2O}n，其中C8H7N3为4-(1H-吡唑-3-基)吡啶，C8H4O4为去质子的对苯二甲酸；其在370nm波长的激发下，可以发射出蓝色荧光, 通过单晶衍射仪测定其结构，晶体学参数如下：
具体步骤为：将0.016-0.16 g对苯二甲酸、0.016-0.16g4-(1H-吡唑-3-基)吡啶和0.030-0.3 g硝酸锌混合，然后加入10-100ml水中，搅拌10分钟，然后放在120℃的烘箱中静止72h后，冷却得到无色的块状晶体即{[Zn(C8H7N3)(C8H4O4)]•H2O}n。
2.一种如权利要求1所述的锌配合物的用途，其可以在多种常见金属离子的水溶液中，应用于对Fe3+的识别，应用于荧光探针。
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