CN116589696B - 一种二维镉配位聚合物及其制备方法与应用 - Google Patents
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- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 33
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000013256 coordination polymer Substances 0.000 title claims abstract description 29
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 29
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- 239000011540 sensing material Substances 0.000 claims abstract description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
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- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- WHQSYGRFZMUQGQ-UHFFFAOYSA-N n,n-dimethylformamide;hydrate Chemical compound O.CN(C)C=O WHQSYGRFZMUQGQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000003446 ligand Substances 0.000 description 6
- 239000000725 suspension Substances 0.000 description 5
- 239000007900 aqueous suspension Substances 0.000 description 4
- 229910052747 lanthanoid Inorganic materials 0.000 description 4
- 150000002602 lanthanoids Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 3
- 230000009977 dual effect Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
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- 150000002910 rare earth metals Chemical class 0.000 description 1
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- 229930003231 vitamin Natural products 0.000 description 1
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Abstract
本发明公开了一种二维镉配位聚合物及其制备方法与应用,属于镉配位聚合物技术领域。本发明二维镉配位聚合物的分子简式为[Cd4(L)2(phen)2(H2O)8·7H2O]n,其中H4L为3,5‑二(3,4‑二羧基苯基)吡啶,phen为邻菲罗啉,n表示聚合。该配位聚合物通过溶剂热方法制得:将Cd(NO3)2·4H2O、H4L和混合于25mL聚四氟乙烯管中,再加入水和N,N‑二甲基甲酰胺作为溶剂,放入不锈钢反应釜中。120℃恒温保持72小时,冷却至室温后,得到无色条状晶体,用蒸馏水冲洗,并在室温下干燥即得到目标物。本发明二维镉配位聚合物可以作为天线对水溶液中的铽离子(Tb3+)进行有效敏化,是检测铽离子的良好荧光传感材料,检出限低至10.93nM。
Description
技术领域
本发明属于镉配位聚合物技术领域,具体涉及一种二维镉配位聚合物及其制备方法与应用。
背景技术
稀土元素被誉为“工业维生素”。铽是稀土家族的重要成员,在信息产业、玻璃工业、生化传感器和太阳能电池等领域具有广泛的应用前景。由于铽的广泛开发利用,它不可避免地渗透到环境、食物链和生物体中。因此,铽离子(Tb3+)含量的测定对人体和环境都至关重要。因为镧系元素的化学性质具有很大的相似性,这给镧系元素的定量分析带来困难。目前已经开发出多种检测铽离子的方法,如电感耦合等离子体质谱法、电化学方法和拉曼光谱法。荧光光谱法因其合成简单、识别速度快、检测准确、成本低等优点而备受关注。所以设计与合成可用于铽离子快速检测的荧光传感材料具有十分重要的意义。
发明内容
本发明的目的在于提供一种可以作为铽离子传感材料的二维镉配位聚合物及其制备方法。
本发明提供了一种二维镉配位聚合物,所述二维镉配位聚合物的分子简式为:[Cd4(L)2(phen)2(H2O)8·7H2O]n,其中L为H4L的去四质子形式,H4L为3,5-二(3,4-二羧基苯基)吡啶,phen为邻菲罗啉;结构式为:
所述二维镉配位聚合物的晶体学参数:单斜晶系,C2/c空间群, α=90°,β=90.1647°,γ=90°,/> Z=4。
配合物中镉离子均采用六配位模式,Cd1分别与来自两个L4-配体的三个羧基氧原子,来自一个L4-配体的氮原子,以及来自两个水分子的两个氧原子配位。Cd2与两个L4-配体上的两个氧原子,两个水分子,以及一个phen配体上的两个氮原子配位。Cd–N键长范围为Cd–O键长范围为/> 相邻的金属离子通过L4-配体连接形成一维波浪链,异面一维链通过Cd-N键交错编织形成二维网状结构。X射线粉末衍射证实晶体样品均一稳定。室温条件下配合物水悬浮液的荧光发射光谱显示,在268nm激发下,配合物显示出宽的发射带,在364nm和382nm处有双发射峰。当加入铽离子后配合物的发射光谱在488、543、585和620nm处显示出强的铽离子特征发射,在紫外灯(λ=254nm)照射下显示出明显的绿光,并可以通过肉眼观察到。本发明的镉配合物可以作为检测铽离子的荧光传感材料。
本发明提供了上述二维镉配位聚合物的制备方法,包括以下步骤:
步骤1,将摩尔比为2:1:2的Cd(NO3)2·4H2O、3,5-二(3,4-二羧基苯基)吡啶、邻菲罗啉混合置于聚四氟乙烯管中,加入水和N,N-二甲基甲酰胺作为溶剂;
步骤2,将此聚四氟乙烯管置于不锈钢反应釜中密封,在120℃下反应72小时,自然冷却到室温后,得到无色条状晶体,用蒸馏水冲洗,并在室温下干燥,收集产品得到二维镉配位聚合物。
二维镉配位聚合物作为荧光传感材料在检测水中铽离子的应用。
与现有技术相比本发明具有以下优点:
本发明的镉配合物是通过溶剂热合成得到的,制备方法简单,产率及纯度较高。本发明提供的镉配合物对铽离子的检测简单快速,肉眼可见。
附图说明
图1[Cd4(L)2(phen)2(H2O)8·7H2O]n的晶体结构图。图中对称操作代码:A=-x+3/2,y-1/2,-z+3/2;B=-x+1,y,-z+3/2;C=x+1/2,y+1/2,z。
图2二维镉配位聚合物在298K的X射线粉末衍射图(实验及模拟图)。
图3二维镉配位聚合物水悬浮液的荧光光谱图。
图4二维镉配位聚合物对不同镧系金属离子的荧光响应图。
图5二维镉配位聚合物对不同浓度的铽离子的荧光响应光谱。
图6二维镉配位聚合物的水悬浮液加入不同浓度的铽离子后在254nm紫外光下的视觉发光照片。
图7二维镉配位聚合物543nm处的荧光响应信号与铽离子浓度的线性关系。
具体实施方式
实施例1
将Cd(NO3)2·4H2O(30.85mg,0.10mmol)、H4L(20.35mg,0.05mmol)和phen(18.02mg,0.10mmol)混合于25mL聚四氟乙烯管中,再加入H2O(8mL)和DMF(2mL)作为溶剂,放入不锈钢反应釜中。120℃恒温保持72小时,冷却至室温后,获得无色条状晶体,用蒸馏水冲洗,并在室温下干燥,产率约为40%。
二维镉配位聚合物的结构测定:
晶体结构采用理学牛津衍射仪进行测定,Cu-Kα射线为辐射光源,收集数据的温度为150K。晶体结构由SHELXL-2014直接法解得。用全矩阵最小二乘法F2对所有非氢原子进行各向异性精修。最后使用理论加氢给配体上的C原子加氢。水分子上的氢原子通过差值Fourier合成给出。详细的晶体数据见表1。晶体结构见图1。
表1配合物的晶体学数据
粉末衍射:
X-射线粉末衍射数据用BrukerD8 Advance X-射线衍射仪采集(Cu-Kα, ),测试速度为5°/min,2θ范围为5-50°。结果表明实验衍射图谱与单晶模拟图谱一致,表明晶体样品物相均一,见图2。
镉配位聚合物作为荧光传感材料在水中对铽离子的识别:
将镉配合物研磨成粉末,将5mg粉末样品分散在50mL水中,超声处理30分钟后静置3天,取上层悬浮液作为研究使用。采用爱丁堡FS5荧光光谱仪记录室温下悬浮液的光致发光光谱。如图3所示,在268nm激发下,配合物的水悬浮液在364nm和382nm处显示双发射峰。通过向悬浮液中添加不同的镧系金属离子进行荧光传感实验,并记录相应的光致发光光谱。当加入铽离子时,配合物的发射光谱在488、543、585和620nm处显示出强的铽离子特征发射(图4),分别对应于铽离子5D4→7F6、5D4→7F5、5D4→7F4和5D4→7F3的发射跃迁,其中5D4→7F5跃迁最强。
镉配位聚合物在水中识别铽离子的灵敏度:
将铽离子逐渐加入到镉配合物的悬浮液中,从图5的滴定曲线可以看出,随着铽离子的增加,铽离子的特征峰强度逐渐增强。在紫外灯(λ=254nm)照射下显示出明显的绿光,并可以通过肉眼观察到(图6)。此外,543nm处的荧光强度与铽离子浓度相关,可以通过拟合((I-I0)/I0)与铽离子浓度之间的关系进行量化,其中I0和I分别为添加铽离子前后配合物水悬浮液在543nm处的荧光强度。如图7所示,在低浓度范围内,((I-I0)/I0)和Tb3+浓度之间存在良好的线性关系,检出限计算为10.93nM。表明该配位聚合物在水中对铽离子检测具有较高的灵敏度,因此具有良好的应用前景。
本发明说明书中未作详细描述的内容属于本领域专业技术人员公知的现有技术。尽管上面对本发明说明性的具体实施方式进行了描述,以便于本技术领域的技术人员理解本发明,但应该清楚,本发明不限于具体实施方式的范围,对本技术领域的普通技术人员来讲,只要各种变化在所附的权利要求限定和确定的本发明的精神和范围内,这些变化是显而易见的,一切利用本发明构思的发明创造均在保护之列。
Claims (3)
1.一种二维镉配位聚合物,其特征在于:所述二维镉配位聚合物的分子简式为:[Cd4(L)2(phen)2(H2O)8·7H2O]n,其中L为H4L的去四质子形式,H4L为3,5-二(3,4-二羧基苯基)吡啶,phen为邻菲罗啉;结构式为:
所述二维镉配位聚合物的晶体学参数:单斜晶系,C2/c空间群, α=90°,β=90.1647°,γ=90°,/> Z=4。
2.根据权利要求1所述的二维镉配位聚合物的制备方法,其特征在于,包括以下步骤:
步骤1,将摩尔比为2:1:2的Cd(NO3)2·4H2O、3,5-二(3,4-二羧基苯基)吡啶、邻菲罗啉混合置于聚四氟乙烯管中,加入水和N,N-二甲基甲酰胺作为溶剂;
步骤2,将此聚四氟乙烯管置于不锈钢反应釜中密封,在120℃下反应72小时,自然冷却到室温后,得到无色条状晶体,用蒸馏水冲洗,并在室温下干燥,收集产品。
3.如权利要求1所述的二维镉配位聚合物作为荧光传感材料在检测水中铽离子的应用。
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