CN107417712B - 一种镉有机骨架配合物及其制备方法 - Google Patents
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- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 20
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000010668 complexation reaction Methods 0.000 title description 3
- 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 24
- 239000013078 crystal Substances 0.000 claims abstract description 11
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- 239000010432 diamond Substances 0.000 claims abstract description 4
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Chemical compound [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- HISPXWSTPJFDDI-UHFFFAOYSA-N 2-(1,2,4-triazol-1-yl)terephthalic acid Chemical compound N1(N=CN=C1)C1=C(C(=O)O)C=CC(=C1)C(=O)O HISPXWSTPJFDDI-UHFFFAOYSA-N 0.000 claims description 3
- 239000012046 mixed 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
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- 238000001291 vacuum drying Methods 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims 1
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- 239000000463 material Substances 0.000 abstract description 9
- 230000003287 optical effect Effects 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- RWLIKKYPSHXLNR-UHFFFAOYSA-N 2,5-bis(1,2,4-triazol-1-yl)terephthalic acid Chemical compound N1(N=CN=C1)C1=C(C(=O)O)C=C(C(=C1)C(=O)O)N1N=CN=C1 RWLIKKYPSHXLNR-UHFFFAOYSA-N 0.000 abstract description 3
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003446 ligand Substances 0.000 description 10
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- 238000002447 crystallographic data Methods 0.000 description 3
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- -1 1H-1, 2,4- triazolyl Chemical group 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 229910052723 transition metal Inorganic materials 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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Abstract
本发明公开了一种镉有机骨架配合物及其制备方法。所述配合物化学式为[Cd(L)(H2O)2]n,其中H2L为2,5‑二(1H‑1,2,4‑三唑基)对苯二甲酸。所述制备方法,是将摩尔比为1:2的H2L与硝酸镉加入体积比为4:1的H2O和DMF中,室温搅拌30分钟后,在密闭反应釜中于120℃反应72小时,即得到无色菱形状晶体,产率为76%。本发明的配合物具有三维骨架结构,其中镉离子采用六配位八面体配位模式。当用320nm波长的光激发该固态配合物时,配合物在414nm处出现发射峰,CIE色坐标为(0.15,0.0439),位于蓝光区,该配合物可作为光学材料应用。
Description
技术领域
本发明涉及过渡金属配合物,具体属于一种镉有机骨架配合物,特别是一种基于镉(II)离子和2,5-二(1H-1,2,4-三唑基)对苯二甲酸构筑的具有发光性质的镉配合物及其制备方法。
背景技术
过渡金属配合物由于具有光、电、磁等多种特性,在磁性、发光、吸附等领域表现出广阔的应用前景,其中含有d10电子的过渡金属有机配合物作为光致发光材料同传统无机发光材料相比,一方面因其特殊的分子刚性结构,使得分子辐射跃迁概率大大增强,即具有高荧光量子效率;另一方面又兼具无机物的高稳定性,即为其作为功能材料应用提供了保证,是一类良好的发光材料。
2,5-二(1H-1,2,4-三唑基)对苯二甲酸,由于同时含有N和O配位原子且结构对称,具有良好的光热稳定性和发光性,特别是当其与具有d10电子结构的金属离子配位形成配合物后,在发光、光记录与存储等领域具有应用价值。到目前为止,过渡金属与2,5-二(1H-1,2,4-三唑基)对苯二甲酸构筑的配合物还未见报导。
发明内容
本发明基于上述情况,提供一种可以作为光学材料的镉配合物及其制备方法。
本发明提供的一种镉有机骨架配合物,其化学式为:[Cd(L)(H2O)2]n,其中H2L为2,5-二(1H-1,2,4-三唑基)对苯二甲酸;结构式为:
该配合物的晶体属于单斜晶系,空间群为C2/c,晶胞参数: α=γ=90°,β=96.857(1)°。该配合物中镉离子为六配位,每个Cd(II)离子与四个氧原子和两个氮原子配位,其中两个氧(O1,O1C)和两个氮(N3A,N3B)来自四个对称性相关的L2-配体,另外两个氧(O2,O2C)来自两个配位的H2O分子,即该配合物通过配位键将相邻的去质子化的配体阴离子连接起来,最终构筑成三维网状结构。Cd-O键的键长范围为X射线粉末衍射证实晶体样品为均相。在室温下,用320nm波长的光激发该配合物的固体粉末,结果显示,配合物在414nm处出现发射峰,相比配体,其荧光强度增强六倍以上,并且发生了红移。因此,本发明的镉配合物可以作为光学材料。
本发明提供一种镉有机骨架配合物的制备方法,包括如下步骤:
(1)将摩尔比为1:2的2,5-二(1H-1,2,4-三唑基)对苯二甲酸与Cd(NO3)2·4H2O加入到体积比为4:1的H2O和DMF混合溶剂中,置于聚四氟乙烯管中室温搅拌30分钟。
(2)将步骤(1)中的聚四氟乙烯管置于不锈钢反应釜中密封,温度控制在120℃,反应72小时,自然降温至室温,得到无色菱形状晶体,蒸馏水洗涤三次,真空干燥即可。
本发明的优点和效果:
本发明的过渡金属镉有机骨架配合物通过混合溶剂热法合成得到,制备方法简单,成本低,产量高,晶相均一。
本发明提供的镉有机骨架配合物基于一种刚性配体2,5-二(1H-1,2,4-三唑基)对苯二甲酸构筑,室温条件下该配合物的固体荧光发射光谱显示,当激发波长为320nm时,配合物显示出较强的蓝光特征,色坐标为(0.15,0.0439)。
本发明的镉有机骨架配合物可以用作光学材料。
附图说明
图1镉有机骨架配合物的结构图。其中对称操作代码为A=-x,-y+1,-z,B=x,-y+1,z+1/2,C=-x,y,-z+1/2。
图2镉有机骨架配合物的红外光谱图。
图3镉有机骨架配合物在298K的X射线粉末衍射图(实验及模拟图)。
图4镉有机骨架配合物的热分析图。
图5镉有机骨架配合物及2,5-二(1H-1,2,4-三唑基)对苯二甲酸在298K的荧光光谱图。
具体实施方式
实施例1.本发明配合物[Cd(L)(H2O)2]n的制备方法
称取0.05mmol H2L与0.1mmolCd(NO3)2·4H2O放入15ml的聚四氟乙烯管中,并加入8ml H2O和2ml DMF,室温搅拌30分钟。然后将聚四氟乙烯管密封于不锈钢反应釜中,温度控制在120℃加热72小时,自然降至室温,得到无色菱形状晶体,用蒸馏水洗涤三次,真空干燥,所得镉配合物的产率为76%。红外光谱(波数,cm-1):3446(m),3134(m),2309(w),1837(w),1764(w),1588(s),1534(s),1442(m),1410(m),1362(s),1335(s),1282(s),1233(m),1216(m),1142(s),1075(m),1000(w),980(s),914(m),886(m),814(s),671(m),653(m),567(w)。
实施例2.本发明配合物[Cd(L)(H2O)2]n的晶体结构
在显微镜下选取合适大小的单晶,采用X射线衍射,以Bruker Smart Apex II探测器通过石墨单色器单色化的Mo-Kα射线,扫描方式ω,室温收集衍射数据。所有衍射数据经SAINT还原后,使用SADABS程序进行半经验吸收校正。晶体结构由SHELXL-97直接法解得。详细的晶体测定数据见表1;晶体结构如图1所示,每个Cd(II)均采用六配位模式,L2-提供四个配位原子分别与四个中心离子Cd(II)进行配位,由此形成三维网状结构。
表1配合物的晶体学数据
实施例3.本发明配合物[Cd(L)(H2O)2]n的红外光谱
取微量[Cd(L)(H2O)2]n固体粉末,与KBr压片,在红外光谱仪记录4000-400cm-1吸收,见图2。配合物特征吸收峰(cm-1)与相应的振动模式为:配合物在3134cm-1的宽带吸收对应于水分子的O-H伸缩振动。配合物在1700cm-1处特征带和配体相比很弱,表明羧基与Cd(II)离子反应完全去质子化。
实施例4.本发明配合物[Cd(L)(H2O)2]n的物相分析
X射线粉末衍射如图3所示,实验衍射图谱与依据晶体结构模拟的粉末衍射图谱一致,表明晶体样品均一。
实施例5.本发明配合物[Cd(L)(H2O)2]n的热稳定性
热稳定性如图4所示,配合物在90℃左右开始失重,在90~130℃之间首先失去两分子的配位水分子(实验值8.21%,理论值8.16%),在350℃左右配合物骨架开始逐渐坍塌。说明该配合物在室温下可以稳定存在。
实施例6.本发明配合物[Cd(L)(H2O)2]n的发光性质
在室温下测定了配体和配合物的固体荧光发射光谱(图5)。从图中可看出,在320nm波长激发下,配合物在414nm处有较强的蓝光发射峰,可以归因于电子在配体间的跃迁。与配体相比,配合物的荧光显著增强且发生了红移,原因是配体与金属离子配位后有效地增强了配体的刚性,降低了非辐射能量损失。
Claims (1)
1.一种镉有机骨架配合物的制备方法,所述镉有机骨架配合物,化学式为:[Cd(L)(H2O)2]n,其中H2L为2,5-二(1H-1,2,4-三唑基)对苯二甲酸;结构式为:
其特征在于,制备方法包括如下步骤:
(1)将摩尔比为1:2的2,5-二(1H-1,2,4-三唑基)对苯二甲酸与硝酸镉加入到含有体积比为4:1的H2O和DMF混合溶剂的聚四氟乙烯管中,室温搅拌30分钟;
(2)将此聚四氟乙烯管置于不锈钢反应釜中密封,升温至120℃反应72小时,自然降至室温,得到无色菱形状晶体,用蒸馏水洗涤三次,真空干燥即可。
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含N杂环配位聚合物的结构及性质研究;马琦;《中国博士学位论文全文数据库 工程科技I辑》;20101115(第11期);第B014-38页 * |
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