CN113185698B - 一种四核镉簇有机框架的制备方法及其应用 - Google Patents
一种四核镉簇有机框架的制备方法及其应用 Download PDFInfo
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Abstract
本发明提供了一种四核镉簇有机框架的制备方法及其应用,以3,3′5,5′‑偶氮苯四羧酸(C16H6N2O8)(H4abtc)和Cd2+为原料,构建了微孔三维有机骨架{[Cd4(abtc)2·3H2O]}n。本发明可作为荧光传感器灵敏的识别抗生素,根据Stern‑Volmer公式,计算KSV值分别为25700M‑1(TC)、61000M‑1(THI)、54000M‑1(NFT)、48000M‑1(NFZ)、47000M‑1(CHL)和24000M‑1(SDI);根据LOD=3Sb/KSV公式,计算出抗生素检出限(LOD)为1.11ppm(TC)、3.25ppm(THI)、3.45ppm(NFT)、3.60ppm(NFZ)、3.84ppm(CHL)和7.39ppm(SDI)。
Description
技术领域
本发明属于合成金属有机框架技术领域,具体涉及到一种四核镉簇有机框架的制备方法及其应用。
背景技术
近年来,抗生素已被成功开发用于改善人类健康,也用于预防和治疗动物和植物感染、以及促进畜牧业的生长。但是,抗生素在治疗的同时不能被完全的利用,部分代谢的抗生素沿着排泄物排出,将人或家畜排泄物排入河流或用作农田肥料的做法导致环境中存在抗生素,不仅如此,它们还可以通过其他的途径排放,主要是由污水处理厂引入到河流、地下水和土壤环境中,进而造成一系列的环境问题。所以,抗生素越来越受到关注,因为其的滥用不仅对生态环境造成了污染,而且极大的威胁了人类的健康。环境中常见的抗生素污染物主要有四环素(TC)、甲砜霉素(THI)、呋喃妥因(NFT)、呋喃西林(NFZ)、氯霉素(CHL)和磺胺嘧啶(SDI)等。
但是这些抗生素分布较广,含量较低,对其的检测存在着挑战。目前已报道了气相色谱质谱法(GC-MS)、液相色谱质谱法(LC-MS)、胶束电动毛细管色谱法(EC)、拉曼光谱法等多种方法来测定抗生素的残留。虽然这些方法满足了灵敏度要求,但由于设备昂贵,操作也非常耗时。因此,开发特异性、敏感性、易用性和低成本效益的检测设备来监测抗生素的存在迫在眉睫。荧光MOFs属于MOFs功能材料中的重要一类。荧光MOFs在传感领域有着显著的优点,如操作方便、成本低、灵敏度高和高选择性等。MOFs的FL性质通常来源于有机配体,它们被作为分析物特异性检测的识别位点。特别是荧光团,它根据介质的微环境而显示出荧光颜色和强度的变化,它们可作为各种荧光传感器和探针的信号部分。基于这些原因,荧光MOFs不仅吸引了广泛的兴趣,而且在新型的荧光传感材料领域成为了研究的热点。
发明内容
本发明的目的是为了克服现有技术中的问题,提供一种四核镉簇有机框架的制备方法及其应用。
为实现上述目的,本发明是通过以下技术方案来实现:
一种四核镉簇有机框架,分子式为C32H18Cd4N4O19,结构式为{[Cd4(abtc)2·3H2O]}n,其为单斜晶系,晶胞参数为 α=90°,β=133.4710(10)°,γ=90°, 空间群为C2/c,对称操作码为(a)x,1-y,-0.5+z;(b)x,-y,-0.5+z;(c)-0.5+x,-0.5+y,-1+z;(d)x,1-y,0.5+z;(e)x,-y,0.5+z;(f)0.5-x,0.5-y,1-z;(g)0.5+x,0.5+y,1+z;(h)1-x,y,1.5-z。
一种四核镉簇有机框架的制备方法,包括以下步骤:将四水硝酸镉[Cd(NO3)2·4H2O]和H4abtc混合后,超声处理,恒温静置反应,冷却至室温,过滤,洗涤,干燥,即得所述四核镉簇有机框架{[Cd4(abtc)2·3H2O]}n。
进一步,所述四水硝酸镉[Cd(NO3)2·4H2O]和H4abtc的摩尔比为1:2~1:2.5。
进一步,所述恒温静置反应温度为100℃~120℃,反应时间为2~3天。
本发明还提供了上述四核镉簇有机框架应用于荧光传感器灵敏识别四环素(TC)、甲砜霉素(THI)、呋喃妥因(NFT)、呋喃西林(NFZ)、氯霉素(CHL)和磺胺嘧啶(SDI)。
与现有技术相比,本发明的有益效果如下:
(1)本发明四核镉簇有机框架是由d10过渡金属镉离子和H4abtc经溶剂热反应形成的配合物{[Cd4(abtc)2·3H2O]}n,该配合物对水溶液中抗生素具备荧光传感能力,可传感四环素(TC)、甲砜霉素(THI)、呋喃妥因(NFT)、呋喃西林(NFZ)、氯霉素(CHL)和磺胺嘧啶(SDI)六种抗生素。通过荧光光谱图研究其荧光性能,并计算KSV值和检出限(LOD),从数据得知配合物{[Cd4(abtc)2·3H2O]}n对四环素的猝灭效果最明显,可以有效的猝灭四环素。
(2)当抗生素TC与THI、NFT、NFZ、CHL或SDI共存时,可忽略THI、NFT、NFZ、CHL或SDI的干扰,{[Cd4(abtc)2·3H2O]}n对TC具有较高的猝灭选择性。
附图说明
图1是实施例{[Cd4(abtc)2·3H2O]}n的非基本结构单元图;
图2是实施例{[Cd4(abtc)2·3H2O]}n配体周围的环境图;
图3是实施例{[Cd4(abtc)2·3H2O]}n的二维链图;
图4是实施例{[Cd4(abtc)2·3H2O]}n的拓扑图;
图5是实施例{[Cd4(abtc)2·3H2O]}n传感TC的荧光图;
图6是实施例{[Cd4(abtc)2·3H2O]}n传感NFT的荧光图;
图7是实施例{[Cd4(abtc)2·3H2O]}n传感NFZ的荧光图;
图8是实施例{[Cd4(abtc)2·3H2O]}n传感SDI的荧光图;
图9是实施例{[Cd4(abtc)2·3H2O]}n传感THI的荧光图;
图10是实施例{[Cd4(abtc)2·3H2O]}n传感CHL的荧光图;
图11是实施例{[Cd4(abtc)2·3H2O]}n传感TC的Stern-Volmer图;
图12是实施例{[Cd4(abtc)2·3H2O]}n传感NFT的Stern-Volmer图;
图13是实施例{[Cd4(abtc)2·3H2O]}n传感NFZ的Stern-Volmer图;
图14是实施例{[Cd4(abtc)2·3H2O]}n传感SDI的Stern-Volmer图;
图15是实施例{[Cd4(abtc)2·3H2O]}n传感THI的Stern-Volmer图;
图16是实施例{[Cd4(abtc)2·3H2O]}n传感CHL的Stern-Volmer图;
图17是实施例{[Cd4(abtc)2·3H2O]}n选择性图。
具体实施方式
以下所述实例以本发明技术方案为前提进行实施,给出了详细的实施方式和具体的操作过程,但并不限制本发明专利的保护范围,凡采用等同替换或等效变换的形式所获得的技术方案,均应落在本发明的保护范围之内。
实施例1
一种四核镉簇有机框架的制备方法,包括以下步骤:将四水硝酸镉[Cd(NO3)2·4H2O]和H4abtc按摩尔比为1:2置于25mL玻璃瓶中,超声20min,在100℃恒温静置反应2~3天,冷却至室温,过滤,洗涤,干燥,制备成Cd2+与偶氮四羧酸的配合物{[Cd4(abtc)2·3H2O]}n。
(1)晶体结构分析
如图1所示,不对称细胞单元由两个独立的Cd2+离子、一个abtc4-配体和一个水分子组成。Cd1原子与4个不同abtc4-配体的7个氧原子进行七配位,形成了扭曲的五-双金字塔配位结构。而Cd2原子与来自4种不同abtc4-配体的5个羧酸氧原子和一个来自水分子的氧原子进行六配位,形成八面体配位几何结构。Cd-O键距为O-Cd-O键角为53.18(10)~180.000(1),这与之前的其他Cd(II)羧酸类化合物的研究结果一致。从图2中可知,晶体结构中所有配体的羧基都发生了脱质子化。有趣的是,abtc4-配体采用桥接9个Cd2+离子,abtc4-配体上的羧基采取三种配位方式:一种采用μ2-η1:η1的配位方式,两种采用μ2-η2:η1的配位方式,一种采用μ3-η1:η2:η1的配位方式。根据图3,在配合物{[Cd4(abtc)2·3H2O]}n的结构,每个Cd1离子通过abtc4-配体连接形成一个二维层,这些层进一步与Cd2离子生成3d孔道框架。如图4,从结构拓扑上看,双核镉簇连接了3个abtc4-配体,可以简化为一个3连接节点,abtc4-配体也可以看作是一个4连接节点。因此,将配合物{[Cd4(abtc)2·3H2O]}n的整个结构定义为一个(3,8)连接的三维网络。
(2){[Cd4(abtc)2·3H2O]}n传感抗生素(TC、THI、NFT、NFZ、CHL和SDI)的应用
采用{[Cd4(abtc)2·3H2O]}n来传感6种抗生素TC、THI、NFT、NFZ、CHL和SDI,具体步骤如下:将0.5mg研磨过后的{[Cd4(abtc)2·3H2O]}n置于1mL水溶液中,超声20min制成悬浮液。取1mL的悬浮液于比色皿中,然后分别逐渐滴加100μL的抗生素(TC、THI、NFT、NFZ、CHL和SDI)溶液,通过荧光光谱图研究其荧光性能,如图5~10所示。根据荧光光谱图可以看出,{[Cd4(abtc)2·3H2O]}n的荧光强度随着六种抗生素浓度的增加而猝灭(通过添加逐渐滴加100μL的抗生素溶液),其中,对四环素的猝灭尤为明显。根据Stern-Volmer方程(I0/I=KSV[M]+1)计算KSV值,如图11~16所示,KSV值分别为25700M-1(TC)、61000M-1(THI)、54000M-1(NFT)、48000M-1(NFZ)、47000M-1(CHL)和24000M-1(SDI);根据LOD=3Sb/KSV公式,计算出抗生素检出限为1.11ppm(TC)、3.25ppm(THI)、3.45ppm(NFT)、3.60ppm(NFZ)、3.84ppm(CHL)和7.39ppm(SDI)。同时,从KSV和LOD值可以看出{[Cd4(abtc)2·3H2O]}n是一种高效的识别四环素的荧光传感器。
(3){[Cd4(abtc)2·3H2O]}n传感的选择性实验
在实际的传感应用中,选择性是影响传感器材料性能的重要因素。在选择性实验中,初步记录{[Cd4(abtc)2·3H2O]}n分散溶剂的荧光光谱,在这些体系中,首先记录悬浮液的初始光谱,接着分别加入100μL的(THI、NFT、NFZ、CHL和SDI)的溶液并记录荧光光谱。在THI、NFT、NFZ、CHL和SDI存在的情况下,{[Cd4(abtc)2·3H2O]}n的发射强度略有变化。在{[Cd4(abtc)2·3H2O]}n和干扰物的混合物中引入TC后,体系的荧光淬灭效果更佳明显,如图17所示,结果表明,THI、NFT、NFZ、CHL和SDI的干扰可以忽略,{[Cd4(abtc)2·3H2O]}n的发射强度在干扰混合物的存在下发生淬灭,这证明了当溶液中加入其他抗生素时,{[Cd4(abtc)2·3H2O]}n对TC具有较高的猝灭选择性。
实施例2
一种四核镉簇有机框架的制备方法,包括以下步骤:将四水硝酸镉[Cd(NO3)2·4H2O]和H4abtc按摩尔比为1:2.5置于25mL玻璃瓶中,超声20min,在110℃恒温静置反应2~3天,冷却至室温,过滤,洗涤,干燥,制备成Cd2+与偶氮四羧酸的配合物{[Cd4(abtc)2·3H2O]}n。
实施例3
一种四核镉簇有机框架的制备方法,包括以下步骤:将四水硝酸镉[Cd(NO3)2·4H2O]和H4abtc按摩尔比为1:2置于25mL玻璃瓶中,超声20min,在120℃恒温静置反应2~3天,冷却至室温,过滤,洗涤,干燥,制备成Cd2+与偶氮四羧酸的配合物{[Cd4(abtc)2·3H2O]}n。
Claims (5)
1.一种四核镉簇有机框架,其特征在于,分子式为C32H18Cd4N4O19,结构式为{[Cd4(abtc)2·3H2O]} n ,其中abtc4-为偶氮苯四羧酸去掉四个质子的形式,其为单斜晶系,晶胞参数为a=25.4539(15)Å,b=13.0476(8)Å,c=18.0985(10)Å,α=90°,β= 133.4710(10)°,γ=90°,V=4362.1(4)Å3,空间群为C2/c,对称操作码为(a) x, 1-y, -0.5+z; (b) x, -y, -0.5+z; (c) -0.5+x, -0.5+y, -1+z; (d) x, 1-y, 0.5+z; (e) x, -y, 0.5+z; (f)0.5-x, 0.5-y, 1-z; (g) 0.5+x, 0.5+y, 1+z; (h) 1-x, y, 1.5-z。
2.一种四核镉簇有机框架的制备方法,其特征在于,包括以下步骤:将四水硝酸镉[Cd(NO3)2·4H2O]和偶氮苯四羧酸H4abtc混合后,超声处理,恒温静置反应,冷却至室温,过滤,洗涤,干燥,即得所述四核镉簇有机框架{[Cd4(abtc)2·3H2O]} n 。
3.根据权利要求2所述的一种四核镉簇有机框架的制备方法,其特征在于,所述四水硝酸镉[Cd(NO3)2·4H2O]和H4abtc的摩尔比为1:2~1:2.5。
4.根据权利要求2所述的一种四核镉簇有机框架的制备方法,其特征在于,所述恒温静置反应温度为100℃~120℃,反应时间为2~3天。
5.一种四核镉簇有机框架的应用,其特征在于,所述四核镉簇有机框架应用于荧光传感器灵敏识别四环素TC、甲砜霉素THI、呋喃妥因NFT、呋喃西林NFZ、氯霉素CHL和磺胺嘧啶SDI。
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