CN108640934A - 一种金属镉有机骨架材料及其制备方法和应用 - Google Patents
一种金属镉有机骨架材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种金属镉有机骨架材料(MOF)及其制备方法，MOF结构简式为：[Cd2(TCPB)(1,4‑BIB)(OH)(H2O)2]n，其中H3TCPB为1,3,5‑三(4‑羧基苯氧基)苯；1,4‑BIB为1,4‑双咪唑苯。该MOF通过溶剂热法制得，即将Cd(NO3)2·4H2O，H3TCPB与1,4‑BIB以2:1:1的物质的量之比溶于H2O/DMF混合溶液中(体积比为5:3)，DMF为N,N‑二甲基甲酰胺，在水热反应釜中以160℃反应84小时；冷却至室温后收集无色条状晶体，用蒸馏水洗涤后，真空干燥即可。用波长为290nm的光激发该固态配合物，样品可发射较强荧光。该MOF在水溶液中具有吸附碘单质的能力，最大吸附量可达56.8mg g‑1，是一种潜在的碘吸附材料。
Description
技术领域
本发明涉及金属有机骨架材料(MOFs)，特别涉及一种金属镉有机骨架材料(MOF)，具体属于一种镉离子(II)与1,3,5-三(4-羧基苯氧基)苯和1,4-双咪唑苯构筑的金属镉有机骨架材料及其制备方法，以及该材料在水溶液中吸附碘单质的应用。
背景技术
碘是人体必需的微量元素之一，可用于治疗碘缺乏和甲状腺功能减退症，杀菌消毒，促进维生素的吸收，增强酶活性等。此外，核工厂和工业区释放的放射性碘也值得关注，因为它们的释放和扩散会影响人类的健康，造成严重的问题。因此，需要同时具有容量大，稳定性好和存储密度高的有效碘储存材料。目前已被使用的固体吸附剂包括活性炭，银交换丝光沸石(Ag-MOR)和金属有机框架材料(MOFs)等，但是，由于活性炭较低的着火温度和氮中毒效应，容易导致事故发生；另一方面，Ag-MOR作为捕捉碘化合物最有效的吸附剂之一，虽然其对温度、氧化和辐照条件具有良好的稳定性，但是Ag-MOR也存在以下缺点，如吸附能力低，银成本高，以及银对环境有严重影响等，这些缺点都鼓励科学家开发新的替代材料。在这种情况下，MOFs由于其高稳定性，低成本，高表面积和广泛的结构多样性而成为捕获碘的最有效候选物质之一。
发明内容
本发明的目的正是针对上述技术现状，提供一种金属镉有机骨架材料及其制备方法，并将该材料用于水溶液中碘单质的吸附。
本发明提供的一种金属镉有机骨架材料，结构简式为：[Cd2(TCPB)(1,4-BIB)(OH)(H2O)2]n，其中H3TCPB为1,3,5-三(4-羧基苯氧基)苯；1,4-BIB为1,4-双咪唑苯；结构式为：
该MOF的晶体属于单斜晶系，C2/c空间群，晶胞参数为： α＝90°，β＝107.27(3)°，γ＝90°。其不对称结构单元包含两个Cd2+，一个完全去质子化的TCPB3-，一个1,4-双咪唑苯，一个配位羟基以及两个配位水分子。Cd12+离子分别与TCPB3-配体上的三个氧原子(O9,O6i,O5ii)以及一个配位水分子上的一个氧原子(O10)还有1,4-双咪唑苯上的两个氮原子(N1，N2)配位，Cd1-O和Cd1-N的键长范围分别为2.230(8)～2.373(6)和Cd1离子配位后形成六配位八面体构型；而Cd22 +离子分别与TCPB3-配体上的五个氧原子(O8,O9，O5ii，O4ii，O7i)以及一个水分子及一个羟基上的两个氧原子(O11，O12)配位[对称操作代码：(i)x+1/2,y+1/2,z；(ii)x,y+1,z]，Cd2-O的键长范围为Cd2配位后形成七配位五角双锥构型；该配合物是一个三维结构。首先，双核金属离子通过1,4-双咪唑苯沿b轴方向连接形成1D链状结构，再通过配体TCPB3-相互连接形成三维网络结构。
X射线粉末衍射证实晶体样品均一稳定。室温条件下荧光发射光谱显示，当激发波长为290nm时，配合物的固体在389nm处可发射较强荧光，荧光强度为配体的1.5倍，量子产率为37.94％。此外，该MOF在水溶液中具有吸附碘单质的能力，最大吸附量可达56.8mg g-1，是一种潜在的碘吸附材料。
该MOF具有三维结构，用波长为290nm的光激发该固态配合物，样品可发较强荧光，可用作为发光材料。
本发明提供的一种金属镉有机骨架材料的制备方法，包括如下步骤：
(1)将摩尔比为2:1:1的Cd(NO3)2·4H2O，H3TCPB与1,4-BIB，加入到含有体积比为5:3的H2O和DMF混合溶剂的聚四氟乙烯管中；
(2)将此聚四氟乙烯管置于不锈钢反应釜中密封，在160℃下反应84小时，自然冷却至室温，得到无色条状晶体，用蒸馏水洗涤后真空干燥即可。
本发明的优点和效果：
本发明的金属镉MOF是在溶剂热合成条件下得到，制取工艺简单，产率及纯度较高。
本发明提供的金属镉MOF是基于1,3,5-三(4-羧基苯氧基)苯和1,4-双咪唑苯配体构筑的，该MOF具有三维结构，用波长为290nm的光激发该固态配合物，样品可发较强荧光。此外，该MOF在水溶液中具有吸附碘单质的能力，最大吸附量可达56.8mg g-1，是一种潜在的碘吸附材料。
附图说明
图1本发明金属镉MOF的晶体结构图。图中对称操作代码：(i)x+1/2,y+1/2,z；(ii)x,y+1,z
图2本发明金属镉MOF在298K的X射线粉末衍射图(实验及模拟图)
图3本发明金属镉MOF在298K的固体荧光光谱图
图4本发明金属镉MOF及其活化后和吸附碘后在298K的X射线粉末衍射图
图5本发明金属镉MOF在甲醇溶液中随时间变化脱附碘的紫外可见光谱
图6本发明金属镉MOF活化后与脱附碘后的红外光谱对比图
具体实施方式
实施例1.
按物质的量之比为2:1:1分别称取Cd(NO3)2·4H2O(582mg,0.2mmol)，H3TCPB(48.6mg,0.1mmol)和1,4-双咪唑苯(21.1mg,0.1mmol)置于23mL聚四氟乙烯反应釜内衬中，并加入5mL蒸馏水和3mL DMF，室温搅拌30min后，将其封存于不锈钢反应釜中，在160℃的可控温烘箱中恒温反应84h后，自然冷却至室温，得到满足X-Ray测试要求的无色条状晶体，用蒸馏水不断净洗并干燥后产率约36％。
金属镉MOF的结构测定：
将晶体样品固定在Bruker SMART 1000 CCD面探衍射仪上，以石墨单色器MoKα为辐射光源，收集样品对波长为的X-Ray衍射数据。以ω扫描方式，衍射数据经LP因子和经验吸收校正。全部X-Ray衍射图还原为衍射指标后，用SHELXTL-NT 5.10版程序包，直接法确定X-Ray衍射强度的位相，初始结构经全矩阵最小二乘法做数轮修正，找出全部非氢原子坐标，确认残余峰不再有非氢原子后，做各向异性温度因子处理。C原子采用理论加氢，水分子或羟基中O原子上的氢由差值Fourier合成给出， 并固定在母原子上。详细的晶体测定数据见表1。结构见图1。
表1金属镉MOF的晶体学数据
粉末衍射：
X-射线粉末衍射结果表明，晶体样品物相均一，实验衍射图谱与依据晶体结构模拟的粉末衍射图谱一致，见图2。
金属镉MOF的发光性质：
室温下测定了配体H3TCPB和配合物的固体荧光发射光谱(图3)。从图中可看出，在波长为290nm的光激发下，H3TCPB和配合物在383nm处有较强的发射峰，且配合物的发射峰强度明显强于配体。
金属镉MOF在水溶液中吸附碘单质的性质：
首先，将镉MOF的晶体粉末用甲醇溶剂浸泡3天，过滤收集，在70℃下加热3h，然后得到活化后的镉MOF粉末。其次，将80.0mg活化后的镉MOF粉末浸泡在一个盛有15.0mL含饱和碘的甲醇溶液密封玻璃小瓶中，室温放置96h后，粉末的颜色从白色变为浅棕色，此时的镉MOF材料中已吸附碘分子。X射线粉末衍射图证明此时的镉MOF仍保留其框架结构(图4)。为了测试MOF材料对碘分子的吸附量，将5.0mg吸附碘分子后的镉MOF材料浸泡到10.0mL甲醇溶液中，即将碘分子脱附到甲醇溶液中，此时监测溶液的紫外/可见光谱(图5)。结果显示，随着时间的增长，222nm处吸收带的强度增强，归因于MOF材料中释放到甲醇溶液中的I2浓度增大，此外255和355nm处的吸收带强度随着时间增长也不断增强，是由于多碘化物I3 -浓度增大。总而言之，浸泡在10.0mL甲醇中的5.0mg吸附碘分子后的镉MOF材料在7天内脱附了0.284mg碘；而碘的完全脱附需要10天，并且需要不断更换甲醇。通过紫外/可见光谱计算出活化后的镉MOF最大吸附碘量为56.8mg g-1。最终，镉MOF粉末的颜色从棕色变为白色。镉MOF活化后及脱附碘后的红外光谱峰位基本一致，证明镉MOF脱附碘后仍保持其主体骨架结构(图6)，证明该镉MOF材料对碘的吸收是可逆的，并且材料在脱附后可以再生使用。
Claims (4)
1.一种金属镉有机骨架材料，其特征在于，结构式为：
该材料的晶体属于单斜晶系，C2/c空间群，晶胞参数为： α＝90°，β＝107.27(3)°，γ＝90°。
2.如权利要求1所述的一种金属镉有机骨架材料的制备方法，其特征在于，包括如下步骤：
(1)将摩尔比为2:1:1的Cd(NO3)2·4H2O，H3TCPB与1,4-BIB，加入到含有体积比为5:3的H2O和DMF混合溶剂的聚四氟乙烯管中；
(2)将此聚四氟乙烯管置于不锈钢反应釜中密封，在160℃下反应84小时，自然冷却至室温，得到无色条状晶体，用蒸馏水洗涤后真空干燥即可。
3.如权利要求1所述的一种金属镉有机骨架材料作为发光材料的应用。
4.如权利要求1所述的一种金属镉有机骨架材料作为碘吸附材料的应用。
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