CN110483558A - 一种具有阴离子骨架的微孔镉化合物的合成方法及其应用 - Google Patents
一种具有阴离子骨架的微孔镉化合物的合成方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种具有阴离子骨架的微孔镉化合物的合成方法及其应用，涉及配位化合物技术领域，以乙酸镉、配体1,2,4‑苯三酸、配体1,2‑二(4‑吡啶)‑乙烷为原料，在反应溶剂存在下，采用水热合成法制得；本发明成功合成了具有阴离子骨架的微孔镉化合物，该化合物的孔道中含有二甲基铵阳离子，这使得化合物在传感、吸附等方面将具有优越的性能，并且该化合物能够高选择性、高灵敏性的荧光传感抗生素呋喃西林。
Description
技术领域：
本发明涉及配位化合物技术领域，具体涉及一种具有阴离子骨架的微孔镉化合物的合成方法及其应用。
背景技术：
抗生素污染已成为当今世界重要的环境问题。由于抗生素废水具有生物毒性大、含有抑菌物质等特点,传统的物理吸附法、生物处理法在处理这类难降解有毒有机废水,尤其是含残留微量抗生素的废水时效果较差。如呋喃西林抗生素因有非常好的抗菌作用和药动力学的特性，被广泛应用。然而，呋喃西林和代谢物均可以使动物发生癌变和基因突变。不幸的是，在废水中往往呋喃西林的含量远远超标，由于呋喃西林浓度过高就会产生毒性效应，这使的人们急需发展一种高灵敏度、高选择性的方法来检测环境中呋喃西林的含量，为了使呋喃西林的检测限在ppb水平，各种有效的方法已经被人们所发展。然而，目前大多数的方法要么需要昂贵的设备，复杂的技术，要么就涉及多样本操作及时间的消耗。
具有活性位点的荧光金属-有机骨架(LMOFs)化合物，如化合物的结构上具有活性官能团或在孔道中有独立的离子等特点，这些化合物由于可以进行后修饰，因此，该类化合物在新型材料方面得到了快速的发展，特别是在化学传感器方面扮演着重要的角色。因为LMOFs化学传感器具有反应快、应用方便、成本低等特点，因此发展基于LMOFs化学传感器探针环境中的抗生素是十分必要的。
发明内容：
本发明所要解决的技术问题在于提供一种具有阴离子骨架的微孔镉化合物的合成方法，采用原位配体水热合成方法，易操作，原料来源充足，生产成本低廉，重复性好，所制微孔镉化合物适用于荧光传感抗生素呋喃西林。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种具有阴离子骨架的微孔镉化合物的合成方法，以乙酸镉、配体1,2,4-苯三酸、配体1,2-二(4-吡啶)-乙烷为原料，在反应溶剂存在下，采用水热合成法制得。
所述反应溶剂由N,N'-二甲基甲酰胺，丙酮和乙腈组成，三者体积比为3:1:2。
所述乙酸镉、配体1,2,4-苯三酸、配体1,2-二(4-吡啶)-乙烷的摩尔比为1:1:1。
上述微孔镉化合物在荧光传感抗生素中的应用。
所述抗生素包括磺胺二甲基嘧啶、磺胺嘧啶、青霉素G钠、氯霉素甲硝唑、罗硝唑、奥硝唑、呋喃妥因、呋喃西林，优选呋喃西林。
本发明的有益效果是：
(1)成功合成了具有阴离子骨架的微孔镉化合物，化合物1的孔道中含有二甲基铵阳离子，这使得化合物在传感、吸附等方面将具有优越的性能。
(2)化合物1具有较好的热稳定性，且化合物1可在pH为3.0-12.0的水中稳定存在，具有很好的实际应用价值。
(3)化合物1能够高选择性、高灵敏性的荧光传感抗生素呋喃西林。
附图说明：
图1为化合物1中二个镉原子的配位模式；
图2为阳离子[H2N(CH3)2]+填充在微孔化合物1孔道中；
图3为化合物1的热重曲线；
图4为化合物1对各种抗生素的荧光探针；
图5为对抗生素呋喃西林的细化滴定。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例和图示，进一步阐述本发明。
配合物[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(化合物1)的合成
将0.1mmol(21.0mg)的1,2,4-苯三酸和0.1mmol(18.4mg)的1,2-二(4-吡啶)-乙烷溶解在3.0mL的N,N'-二甲基甲酰胺，1.0mL的丙酮和2.0mL的乙腈溶液中，然后加入5.0mL的含有0.1mmol的Cd(CH3COOH)2·2H2O水溶液，将混合溶液放入反应釜中，加热到125℃，持续加热4天，然后以5℃/h的速率降到室温，得到无色块状晶体，产率:60％。C34H36Cd2N4O14元素分析(％):计算值：C,43.01；H,3.82；N,5.90。实验值：C,44.26；H,3.48；N,5.63。
配合物[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(1)的结构测定
将晶体用DMF洗干净后，挑选质量和尺寸合适的晶体置于Bruker-AXS SMART CCDX-单晶仪上，两个晶体数据用单色纯化的Mo-Kα射线进行扫描(石墨单色器)，其中λ为ω为0.3°，收集两个晶体的衍射数据，SAINT软件进行衍射数据的还原，用SADABS路线进行吸收校正。晶体结构采用直接法通过SHELXTL软件进行解析，用(F2)最小二乘法对化合物1的非氢原子和氢原子坐标，各向同性温度因子和各向异性温度因子精修至收敛。化合物1的解析和精修用SHELXL-97程序包完成。化合物1的相关晶体学数据列于表1中。
表1化合物1的晶体数据
aR1＝Σ||Fo|–|Fc|)/Σ|Fo|；wR2＝[Σw(Fo 2–Fc 2)2/Σw(Fo 2)2]1/2
配合物[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(1)的结构描述
在水热合成条件下得到了一例具有阴离子骨架的微孔镉化合物
[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(1)。结构分析显示，化合物1中有两个参与配位的镉原子，如图1中所示。Cd1和Cd2原子都是七配位的模式，空间几何构型为扭曲的五角双锥，其中参与配位的六个氧原子来自三个不同的1,2,4-苯三酸配体，一个氮原子来自1,2-二(4-吡啶)-乙烷配体，Cd1-O和Cd2-O的平均键长为和Cd1-N和Cd2-N的键长分别为和在化合物1中，完全质子化的1,2,4-苯三酸配体上的羧基采取双齿螯合的模式与镉原子配位，而1,2-二(4-吡啶)-乙烷配体连接着两个镉原子形成3D的孔道结构，如图2所示。
值得注意的是，化合物1是一个具有阴离子骨架的结构，在反应体系中，溶剂分子N,N'-二甲基甲酰胺发生了分解，生成了阳离子[H2N(CH3)2]+去平衡微孔化合物1的电荷。这些阳离子[H2N(CH3)2]+填充在阴离子的微孔化合物1孔道中。
配合物[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(1)的稳定性
我们将合成的晶体清洗，直到晶体纯净，然后在室温下烘干以备用。为了研究孔道化合物[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(1)框架的稳定性，我们对化合物1进行了热重分析，如图3。热重曲线分析发现化合物1的框架能稳定到250℃。此外，我们也研究了化合物1在水中不同pH值下的稳定性，研究发现化合物1可在pH为3.0-12.0的水中稳定存在。
配合物[H2N(CH3)2]2[Cd2(L)2(bpa)]n·2H2O(1)荧光探针抗生素
具有阴离子骨架的微孔镉化合物1由于具有高的热稳定性、大的孔面积以及活性位点，且镉化合物具有较强的荧光性质，因此，我们研究了化合物1对抗生素的荧光探针。
我们将3mg化合物1研磨，分散在3mL 0.1mol/L的各种抗生素中[磺胺二甲基嘧啶(SMZ)，磺胺嘧啶(SDZ)，青霉素G钠(PCL)，氯霉素甲硝唑(CAP)，罗硝唑(RDZ)，奥硝唑(ODZ)，呋喃妥因(NFT)，呋喃西林(NZF)]，研究其对抗生素的荧光传感作用。
由图4可以看出，化合物1对呋喃西林有很好的荧光淬灭作用。这一结果证明了化合物1能够高选择性、高灵敏性的荧光传感抗生素呋喃西林。
为了进一步细化对呋喃西林的荧光传感过程，我们做了滴定实验。将0.1M的呋喃西林溶液逐滴滴入含有化合物1的溶液中，然后观察荧光强度的变化。如图5所示，当呋喃西林的浓度为45ppm时，荧光基本淬灭完全。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种具有阴离子骨架的微孔镉化合物的合成方法，其特征在于：以乙酸镉、配体1,2,4-苯三酸、配体1,2-二(4-吡啶)-乙烷为原料，在反应溶剂存在下，采用水热合成法制得。
2.根据权利要求1所述的合成方法，其特征在于：所述反应溶剂由N,N'-二甲基甲酰胺，丙酮和乙腈组成，三者体积比为3:1:2。
3.根据权利要求1所述的合成方法，其特征在于：所述乙酸镉、配体1,2,4-苯三酸、配体1,2-二(4-吡啶)-乙烷的摩尔比为1:1:1。
4.权利要求1所述的具有阴离子骨架的微孔镉化合物在荧光传感抗生素中的应用。
5.根据权利要求4所述的应用，其特征在于：所述抗生素包括磺胺二甲基嘧啶、磺胺嘧啶、青霉素G钠、氯霉素甲硝唑、罗硝唑、奥硝唑、呋喃妥因、呋喃西林。
6.根据权利要求5所述的应用，其特征在于：所述抗生素优选呋喃西林。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121842A (zh) * | 2021-04-30 | 2021-07-16 | 华北电力大学 | 一种基于锆基金属有机框架材料、制备及其在硝基呋喃类抗生素处理中的应用 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584866A (zh) * | 2012-01-18 | 2012-07-18 | 郑州轻工业学院 | 1,2-萘二酸镉配合物及其制备方法 |
| CN107602598A (zh) * | 2017-08-04 | 2018-01-19 | 三峡大学 | 一种Zn、Tb异金属基有机晶态材料、制备方法及其传感识别抗生素上的应用 |
| CN109336914A (zh) * | 2018-11-03 | 2019-02-15 | 桂林理工大学 | 偏苯三甲酸镉配合物及制备方法 |
| KR20190061326A (ko) * | 2017-11-27 | 2019-06-05 | 연세대학교 산학협력단 | 올레핀에 대한 선택적 흡착능을 갖는 분리 흡착제 및 이의 제조방법 |
-
2019
- 2019-08-26 CN CN201910790671.5A patent/CN110483558B/zh active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584866A (zh) * | 2012-01-18 | 2012-07-18 | 郑州轻工业学院 | 1,2-萘二酸镉配合物及其制备方法 |
| CN107602598A (zh) * | 2017-08-04 | 2018-01-19 | 三峡大学 | 一种Zn、Tb异金属基有机晶态材料、制备方法及其传感识别抗生素上的应用 |
| KR20190061326A (ko) * | 2017-11-27 | 2019-06-05 | 연세대학교 산학협력단 | 올레핀에 대한 선택적 흡착능을 갖는 분리 흡착제 및 이의 제조방법 |
| CN109336914A (zh) * | 2018-11-03 | 2019-02-15 | 桂林理工大学 | 偏苯三甲酸镉配合物及制备方法 |
Non-Patent Citations (3)
| Title |
|---|
| MANISHKUMAR R. SHIMPI ET AL: "Synthesis and st ructural evaluation of fi ve coordination complexes of benzenepen tacarboxylic acid with aza-donor ligands", 《JOURNAL OF MOLE CULAR STRUCTURE》 * |
| REN, Y. ET AL: "Two 3D zinc-bpe frameworks constructed from 2-carboxyl/sulfo-terephthalate: Crystal structures and luminescent properties", 《RUSSIAN JOURNAL OF COORDINATION CHEMISTRY》 * |
| WANG, YAN-NING ET AL: "4-(4-Carboxyphenoxy)phthalate-based coordination polymers and their application in sensing nitrobenzene", 《DALTON TRANSACTIONS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121842A (zh) * | 2021-04-30 | 2021-07-16 | 华北电力大学 | 一种基于锆基金属有机框架材料、制备及其在硝基呋喃类抗生素处理中的应用 |
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