CN107445982A - 一种具有绿色荧光发射特性的过渡金属配合物及制备方法 - Google Patents
一种具有绿色荧光发射特性的过渡金属配合物及制备方法 Download PDFInfo
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- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 12
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
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- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了一种具有绿色荧光发射特性的过渡金属配合物及制备方法。该过渡金属配合物的化学式为M2(HL)3(NO3),式中M为二价过渡金属,HL为1,1‑[7,7’‑二‑(8‑羟基负离子喹啉)]。同时还公开了一种具有绿色荧光发射特性的过渡金属配合物的制备方法。本发明公开了一种具有绿色荧光发射特性的二核过渡金属簇结构配合物,其制备方法简单,绿色环保,在荧光材料方面具有良好的潜在应用前景。
Description
技术领域
本发明涉及一种具有绿色荧光发射特性的过渡金属配合物及制备方法。
背景技术
自从1987年美国柯达公司Tang和Van Slyke报导了Alqs(q=8-羟基喹啉)作为发光层的双层绿色有机电致发光(EL)器件以来,8-羟基喹啉及其衍生物作为配体的金属有机配合物发光材料就引起了广泛关注。8-羟基喹啉是一种一元双齿螯合配体,可以与多种金属形成不同配位模式的金属有机配合物荧光材料。人们不断通过改变金属离子和配体结构,来发现性能更佳的金属有机配合物荧光材料。由于制备工艺简便,易于调控,在8-羟基喹啉的衍生物的开拓中,研究通过原位反应获得1,1-[7,7’-二-(8-羟基负离子喹啉)]配体并与过渡金属配位得到新型配合物的方法受到关注。但是目前这些方案都需加入NaN3等有毒物质,这就对实验环境有了约束,增加了应用成本,同时会对环境产生污染,大大限制了其在应用上的进一步推广。基于此原因,研究8-羟基喹啉类过渡金属有机配合物的荧光性能,探究对8-羟基喹啉类原位配体并配位形成金属有机配合物荧光材料的更加合理的制备具有重要意义。
发明内容
本发明的目的在于提供一种具有绿色荧光发射特性的过渡金属配合物及制备方法。
本发明所采取的技术方案是:
一种具有绿色荧光发射特性的过渡金属配合物,其化学式为M2(HL)3(NO3),式中M为二价过渡金属,HL为1,1-[7,7’-二-(8-羟基负离子喹啉)]。
优选的,M为Mn、Ni、Cu、Zn中的其中一种。
进一步优选的,M为Zn。
一种具有绿色荧光发射特性的过渡金属配合物的制备方法,是将二价过渡金属的硝酸盐与8-羟基喹啉在溶剂中进行水热反应,得到上述的具有绿色荧光发射特性的过渡金属配合物。
二价过渡金属的硝酸盐与8-羟基喹啉的摩尔比为1:1。
优选的,二价过渡金属的硝酸盐为硝酸锰、硝酸镍、硝酸铜、硝酸锌中的其中一种。
进一步优选的,二价过渡金属的硝酸盐为硝酸锌。
溶剂为C1~C4的低级醇与水混合液。
C1~C4的低级醇与水的体积比为1:2。
水热反应的温度为150~170℃,时间为70~80h。
本发明的有益效果是:
本发明公开了一种具有绿色荧光发射特性的二核过渡金属簇结构配合物,其制备方法简单,绿色环保,在荧光材料方面具有良好的潜在应用前景。
具体而言:
1)设计制备方法工艺简单,不需加入NaN3等有毒物质,通过控制醇-水比例,原位反应就可以发生并配位,反应更为绿色环保;
2)有效降低生产成本,改进了原位反应的既有模式,大大拓宽其应用范围;
3)结构新颖,一种具有绿色荧光发射特性的过渡金属配合物表现为二核金属簇结构;
4)本发明提供多一种具有绿色荧光发射特性的过渡金属配合物,在绿色荧光材料方面具有良好的潜在应用。
附图说明
图1为本发明原位反应生成配体HL-的反应示意图;
图2为本发明过渡金属配合物Zn2(HL)3(NO3)的平面结构示意图;
图3为本发明过渡金属配合物Zn2(HL)3(NO3)的空间结构示意图;
图4为本发明过渡金属配合物Zn2(HL)3(NO3)的XRD测试示意图;
图5为本发明过渡金属配合物Zn2(HL)3(NO3)的红外测试示意图;
图6为本发明过渡金属配合物Zn2(HL)3(NO3)在425nm激发光激发下的荧光发射光谱示意图;
图7为本发明过渡金属配合物Zn2(HL)3(NO3)的热重测试示意图。
具体实施方式
一种具有绿色荧光发射特性的过渡金属配合物,其化学式为M2(HL)3(NO3),式中M为二价过渡金属,HL为1,1-[7,7’-二-(8-羟基负离子喹啉)]。
优选的,M为Mn、Ni、Cu、Zn中的其中一种。
进一步优选的,M为Zn,即化学式为Zn2(HL)3(NO3)。
一种具有绿色荧光发射特性的过渡金属配合物的制备方法,是将二价过渡金属的硝酸盐与8-羟基喹啉在溶剂中进行水热反应,得到上述的具有绿色荧光发射特性的过渡金属配合物。
优选的,二价过渡金属的硝酸盐与8-羟基喹啉的摩尔比为1:1。
优选的,二价过渡金属的硝酸盐为硝酸锰、硝酸镍、硝酸铜、硝酸锌中的其中一种。
进一步优选的,二价过渡金属的硝酸盐为硝酸锌。
优选的,二价过渡金属的硝酸盐与溶剂的用量比为1mol:(20~30)L。
优选的,溶剂为C1~C4的低级醇与水混合液。
优选的,C1~C4的低级醇与水的体积比为1:2。
优选的,C1~C4的低级醇为乙醇。
优选的,水热反应的反应器为聚四氟乙烯反应釜。
优选的,水热反应的温度为150~170℃,时间为70~80h;进一步优选的,水热反应的温度为160℃,时间为72h。
以下通过具体的实施例对本发明的内容作进一步详细的说明。除非特别说明,本发明采用的试剂、设备和方法为本技术领域常规可市购的试剂、设备和常规使用的方法。
实施例:
一、制备具有绿色荧光发射特性的过渡金属配合物
具体合成方法为:将六水合硝酸锌(0.5毫摩尔),8-羟基喹啉(0.5毫摩尔),依次加入聚四氟乙烯反应釜中,加入乙醇-水混合溶剂(4:8毫升),封口密闭,升温至160度,恒温72小时后,在48小时降温至室温,产率约56%。
本发明原位反应生成配体HL-的反应示意图如附图1所示,附图2为本发明过渡金属配合物Zn2(HL)3(NO3)的平面结构示意图。
二、产物结构的确定
将上述实施例制备得到的产物经过单晶衍射、荧光和红外表征确定,其化学结构式为Zn2(HL)3(NO3),HL-=1,1-[7,7’-二-(8-羟基负离子喹啉)]。
单晶衍射的结果如下:
分子量为1135.79,三方晶系,R-3空间群, α=90°,β=90,γ=120°,T=150(2)K,Z=6,ρ=1.668mg·m-3,Rint=0.0172,R1=0.0492,wR2=0.1584。空间结构由SHELXT解出,Diamond绘制,其最终确定的空间结构示意图如附图3所示。其数据表明,基本结构单元中包括,两个中心原子Zn(α),三个原位配体HL,以及一个游离的NO3 -。中心原子Zn均采取六配位的模式,形成稍稍畸变的八面体构型。Zn1-O1,Zn2-O2的键长分别为和Zn1-N1,Zn2-N2的键长分别为和HL-原位配体的两个O原子间形成氢键 O2···H2O···O1=177.191(4477)°),增加了结构的稳定性。
过渡金属配合物Zn2(HL)3(NO3)的XRD测试结果如附图4所示。从图4可以判断,所得配合物的XRD衍射曲线与理论曲线十分吻合,说明所制备出来的配合物纯度很高。
过渡金属配合物Zn2(HL)3(NO3)的红外表征结果如附图5所示。从图5可以发现,乙基的红外特征峰2963cm-1,2934cm-1,2876cm-1,羟基的红外特征峰3431cm-1。
附图6为过渡金属配合物Zn2(HL)3(NO3)在425nm激发光激发下的荧光发射光谱示意图。其是使用日本日立F-4600荧光分光光度计在室温条件下进行测试。从图6可见,该配合物在425nm激发波长下,其固体荧光发射峰为551nm,具有非常好的绿色荧光发射性能。
附图7为本发明过渡金属配合物Zn2(HL)3(NO3)的热重测试示意图。其是使用热重分析仪在N2氛围下升温速率10℃/min对配合物进行测试,在室温~800℃范围内的热重曲线。从图7可以发现,加热到340℃左右才开始逐渐分解失去配体,这是由于喹啉共轭链及结构内氢键大大增强了结构的稳定性。当温度达到610℃左右配合物完全解体,分解率达到86%。可以得出,该配合物具有很好的热稳定性能。
Claims (10)
1.一种具有绿色荧光发射特性的过渡金属配合物,其化学式为M2(HL)3(NO3),式中M为二价过渡金属,HL为1,1-[7,7’-二-(8-羟基负离子喹啉)]。
2.根据权利要求1所述的一种具有绿色荧光发射特性的过渡金属配合物,其特征在于:M为Mn、Ni、Cu、Zn中的其中一种。
3.根据权利要求2所述的一种具有绿色荧光发射特性的过渡金属配合物,其特征在于:M为Zn。
4.一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:将二价过渡金属的硝酸盐与8-羟基喹啉在溶剂中进行水热反应,得到权利要求1所述的具有绿色荧光发射特性的过渡金属配合物。
5.根据权利要求4所述的一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:二价过渡金属的硝酸盐与8-羟基喹啉的摩尔比为1:1。
6.根据权利要求5所述的一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:二价过渡金属的硝酸盐为硝酸锰、硝酸镍、硝酸铜、硝酸锌中的其中一种。
7.根据权利要求6所述的一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:二价过渡金属的硝酸盐为硝酸锌。
8.根据权利要求4所述的一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:溶剂为C1~C4的低级醇与水混合液。
9.根据权利要求8所述的一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:C1~C4的低级醇与水的体积比为1:2。
10.根据权利要求4所述的一种具有绿色荧光发射特性的过渡金属配合物的制备方法,其特征在于:水热反应的温度为150~170℃,时间为70~80h。
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CN105503965A (zh) * | 2016-01-11 | 2016-04-20 | 天津师范大学 | 稀土(iii)-过渡(ii)混金属荧光配合物及其制备方法与应用 |
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CN101468966A (zh) * | 2007-12-28 | 2009-07-01 | 华东师范大学 | 一种喹啉锌类发光材料及含有该材料的电致发光器件 |
CN105503965A (zh) * | 2016-01-11 | 2016-04-20 | 天津师范大学 | 稀土(iii)-过渡(ii)混金属荧光配合物及其制备方法与应用 |
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