CN106699781B - 基于衣康酸-吡嗪混合配体的锌(ii)荧光材料及制备方法 - Google Patents
基于衣康酸-吡嗪混合配体的锌(ii)荧光材料及制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 51
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000003446 ligand Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- ZINNZPSOCZHJCR-UHFFFAOYSA-N N1=CC=NC=C1.C(C(=C)CC(=O)O)(=O)O Chemical compound N1=CC=NC=C1.C(C(=C)CC(=O)O)(=O)O ZINNZPSOCZHJCR-UHFFFAOYSA-N 0.000 title claims abstract description 7
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 claims abstract description 34
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims abstract description 20
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims abstract description 20
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001868 water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010276 construction Methods 0.000 claims abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 14
- 239000011701 zinc Substances 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 5
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000000523 sample Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
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- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 16
- 238000001035 drying Methods 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 8
- 238000001914 filtration Methods 0.000 description 5
- 239000012621 metal-organic framework Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004467 single crystal X-ray diffraction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
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- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
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Abstract
本发明公开了一种基于衣康酸‑吡嗪混合配体的晶态锌(II)荧光材料及其制备方法,该荧光材料的分子式为[Zn2(YKS)2(BQ)(H2O)4]n(其中,YKS=衣康酸配体,BQ=吡嗪),单晶结构具有二维层状结构,其不对称构筑单元包含一个二价锌离子、一个衣康酸配体、半个吡嗪配体和两个末端配位水分子。本发明的合成和提纯方法简单,成本低廉,荧光性能良好,作为荧光材料在发光分子器件和荧光探针等领域具良好的应用前景。
Description
技术领域
本发明属于光学材料应用技术领域,具体涉及一种基于衣康酸-吡嗪混合配体的晶态锌(II)荧光材料:[Zn2(YKS)2(BQ)(H2O)4]n(其中,YKS=衣康酸配体,BQ=吡嗪),及其制备方法以及其作为荧光材料在发光分子器件和荧光探针等领域的应用。
背景技术
随着无机多孔材料以及合成化学的迅猛发展,金属有机框架材料(Metal OrganicFrameworks,MOFs)作为一种新型的多孔材料近年来受到了广泛关注。金属有机框架材料不但具有与传统沸石分子筛材料类似的多孔晶体结构,而且其结构还具有可裁剪性和易功能化的特性,在催化、气体吸附、气体分离、光学材料等领域具有广阔的应用前景。[Chem.Soc.Rev.,2008,37:191-214;Chem.Soc.Rev.,2009,38:1257-1283;Nature,2003,423:705-714]
过渡金属离子,尤其是锌、镉等金属离职因其具有特殊的电子结构和成键特征,可以表现出独特的荧光性质,而通过与配体的作用,又可以增强其荧光强度,因此过渡金属配合物的研究为荧光材料的设计提供了广阔的前景。目前设计和合成含有Zn2+、Cd2+等离子的金属配合物,使之作为发光分子器件和荧光探针是配位化学研究领域的重要课题之一。[Angew.Chem.Int.Ed.,2011,50:8110—8113]
发明内容
本发明的目的旨在开发一种新型晶态锌(II)荧光材料,同时提供此材料的制备方法及其作为荧光材料在发光分子器件和荧光探针等领域的应用。
为实现上述目的,本发明采用以下技术方案:
一种晶态锌(II)荧光材料,所述晶态锌(II)荧光材料的分子式为[Zn2(YKS)2(BQ)(H2O)4]n(其中,YKS=衣康酸配体,BQ=吡嗪),且晶态锌(II)荧光材料的单晶结构具有二维层状结构,所述的二维层状结构的不对称构筑单元包含一个二价锌离子、一个衣康酸配体、半个吡嗪配体和两个末端配位水分子。
所述的晶态锌(II)荧光材料的制备方法,步骤如下:将硝酸锌、衣康酸和吡嗪的水溶液加入反应瓶中,然后加入DMF,在搅拌的条件下逐滴加入氢氧化钠水溶液将体系的pH调到4.6~5.2,搅拌5~10min后密封,在85~100℃的恒温条件下加热20~48h,冷却至室温,过滤、干燥,得到晶态锌(II)荧光材料。
衣康酸和吡嗪的摩尔比为2~4:1~2:2~3。
以0.2mmol衣康酸为基准,所述DMF的用量为1~5mL。
以0.2mmol衣康酸为基准,所述氢氧化钠水溶液的浓度为0.1~2.0mol/L。
所述氢氧化钠水溶液用于调控反应混合溶液的pH值;优选的,pH=4.8。
所述的晶态锌(II)荧光材料作为作为荧光材料在发光分子器件和荧光探针等领域的应用。
本发明的有益效果:本发明的晶态锌(II)荧光材料的合成和提纯方法简单,条件温和,成本低廉,荧光性能良好,可以满足工业发展的需求,作为荧光材料在发光分子器件和荧光探针等领域具有好的应用前景。
附图说明
图1为本发明晶态锌(II)荧光材料单晶结构中不对称锌离子的配位环境。
图2为本发明晶态锌(II)荧光材料单晶结构中衣康酸配体的配位方式。
图3为本发明晶态锌(II)荧光材料单晶结构的二维层状结构。
图4为实施例1制备得到的晶态锌(II)荧光材料的理论(下)和实测(上)PXRD图。
图5为实施例1制备得到的晶态锌(II)荧光材料的固体荧光发射光谱图。
具体实施方式
为进一步阐释本发明,下面给出一系列实施例。这些实施例完全是例证性的,它们仅用来对本发明进行具体描述,不应当理解为对本发明的限制。
实施例1
本实施例的晶态锌(II)荧光材料的制备方法如下:
将800微升1mol/L的Zn(NO3)3水溶液、200微升1mol/L的衣康酸水溶液和600微升1mol/L的吡嗪水溶液放在15mL的小瓶中,然后加入2mL DMF,在搅拌的情况下,逐滴加入1mol/L的氢氧化钠水溶液将pH调到4.8,搅拌10分钟后密封,然后放在恒温干燥箱中90℃恒温加热24h,冷却至室温,可得大量无色晶体,过滤,水洗三次,室温干燥得到晶态锌(II)荧光材料,产量为0.095g,产率为88.1%。
(1)通过Bruker D8ADVANCE粉末X射线衍射仪对所得晶体样品进行表征,所得实测和理论的PXRD图谱的峰值位置一致(见附图4),且无杂峰出现,证明了所得晶态锌(II)荧光材料纯度好,无杂质。
(2)本实施例的晶态锌(II)荧光材料的晶体数据
通过Bruker D8Quest CMOS单晶X射线衍射仪对其单晶进行检测,对所得数据解析和精修可得到:分子式为C14H20N2O12Zn2,分子量为539.06,单斜晶系P2(1)/n空间群,晶胞参数α=90°,β=92.008(3)°,γ=90°,晶胞体积V=959.53(16),密度为2.568g/cm3,Z=2。
(3)本实施例的晶态锌(II)荧光材料的固体荧光发射光谱
在室温下研究了所得晶态样品的固体荧光(见附图5)。激发波长为374nm,配合物在424nm处出现较强的荧光发射峰.这可能是由配体到金属的电子跃迁(LMCT)所致,即配合物被激发时,吡嗪配体的π电子跃迁到Zn的d*轨道上。
实施例2
本实施例的晶态锌(II)荧光材料的制备方法,步骤如下
将400微升1mol/L的Zn(NO3)3水溶液、200微升1mol/L的衣康酸水溶液和200微升1mol/L的吡嗪水溶液放在15mL的小瓶中,然后加入1mL DMF,在搅拌的情况下,逐滴加入0.1mol/L的氢氧化钠水溶液将pH调到5.2,搅拌5分钟后密封,然后放在恒温干燥箱中85℃恒温加热48h,冷却至室温,过滤、室温干燥得到所述锌(II)荧光材料。
实施例3
本实施例的晶态锌(II)荧光材料的制备方法,步骤如下
将800微升1mol/L的Zn(NO3)3水溶液、200微升1mol/L的衣康酸水溶液和400微升1mol/L的吡嗪水溶液放在15mL的小瓶中,然后加入5mL DMF,在搅拌的情况下,逐滴加入2mol/L的氢氧化钠水溶液将pH调到4.6,搅拌8分钟后密封,然后放在恒温干燥箱中100℃恒温加热30h,冷却至室温,过滤、室温干燥得到所述锌(II)荧光材料。
实施例4
本实施例的晶态锌(II)荧光材料的制备方法,步骤如下
将600微升1mol/L的Zn(NO3)3水溶液、400微升1mol/L的衣康酸水溶液和200微升1mol/L的吡嗪水溶液放在15mL的小瓶中,然后加入3mL DMF,在搅拌的情况下,逐滴加入1.5mol/L的氢氧化钠水溶液将pH调到5.0,搅拌6分钟后密封,然后放在恒温干燥箱中95℃恒温加热20h,冷却至室温,过滤、室温干燥得到所述锌(II)荧光材料。
实施例5
本实施例的晶态锌(II)荧光材料的制备方法,步骤如下
将600微升1mol/L的Zn(NO3)3水溶液、200微升1mol/L的衣康酸水溶液和600微升1mol/L的吡嗪水溶液放在15mL的小瓶中,然后加入2mL DMF,在搅拌的情况下,逐滴加入1mol/L的氢氧化钠水溶液将pH调到4.8,搅拌6分钟后密封,然后放在恒温干燥箱中95℃恒温加热30h,冷却至室温,过滤、室温干燥得到所述锌(II)荧光材料。
以上显示和描述了本发明的基本原理和主要特征以及本发明的优点。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 (4)
1.一种基于衣康酸-吡嗪混合配体的晶态锌(II)荧光材料,其特征在于:所述晶态锌(II)荧光材料的分子式为[Zn2(YKS)2(BQ)(H2O)4]n,其中,YKS= 衣康酸配体,BQ = 吡嗪,单晶结构具有二维层状结构,其不对称构筑单元包含一个二价锌离子、一个衣康酸配体、半个吡嗪配体和两个末端配位水分子,所述的晶态锌(II)荧光材料的制备方法,步骤如下:将硝酸锌、衣康酸和吡嗪的水溶液加入反应瓶中,然后加入DMF,在搅拌的条件下逐滴加入氢氧化钠水溶液,将体系的pH调到4.6~5.2,搅拌5~10min后密封,在85~100℃的恒温条件下加热20~48h,冷却至室温,过滤、干燥,得到晶态锌(II)荧光材料。
2.根据权利要求1所述的基于衣康酸-吡嗪混合配体的晶态锌(II)荧光材料,其特征在于:所述硝酸锌、衣康酸和吡嗪的物质的量之比为2~4:1~2:2~3。
3.根据权利要求1所述的基于衣康酸-吡嗪混合配体的晶态锌(II)荧光材料,其特征在于:以0.2mmol衣康酸为基准,所述DMF的用量为1~5mL。
4.根据权利要求1所述的晶态锌(II)荧光材料作为发光材料在发光分子器件和荧光探针领域中的应用。
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