CN105646554A - 一维镉配合物单晶及其制备方法与应用 - Google Patents
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Abstract
本发明公开了一维镉配合物单晶及其制备方法与应用,其结构:[Cd(py)2(hipt)]·2py·2H2O,其中,py=吡啶;hipt=间羟基间苯二甲酸。同时还公开了单晶的制备方法。它是采用常温挥发法,即py、hipt和Cd(NO3)2·4H2O在水中搅拌半小时后过滤,滤液常温挥发两周后得到适合X-射线单晶衍射的无色块状晶体。其中py:hipt:Cd(NO3)2·4H2O的摩尔比为1:1:1。本发明进一步公开了一维镉配合物单晶作为潜在荧光材料在检测染料或发光剂的吸附量方面的应用。
Description
本发明得到国家自然科学基金面上项目(21471113)、天津市教委面上项目(20140506)和天津师范大学中青年教师学术创新推进计划项目(52XC1401)的资助。
技术领域
本发明属于有机和无机合成技术领域,涉及一维镉配合物单晶[Cd(py)2(hipt)]·2py·2H2O的制备方法及作为潜在的荧光材料的应用,其中,py = 吡啶;hipt =间羟基间苯二甲酸。
背景技术
吡啶类配合物由于其结构的多样性,可调控性、优秀的热稳定性等优点,在分离、手性与催化、非线性光学、分子识别等多个领域都具有潜在的应用前景。因此,作为新一代功能性分子材料,吡啶类配合物的合成与设计、结构及功能特性的研究与开发已经成为功能性分子材料科学发展的前沿领域之一。
本发明即是采用常温挥发法,即py、hipt和Cd(NO3)2·4H2O在水中搅拌半小时后过滤,滤液常温挥发两周后得到适合X-射线单晶衍射的无色块状晶体结构为[Cd(py)2(hipt)]·2py·2H2O,其中,py = 吡啶;hipt = 间羟基间苯二甲酸。该配合物还可作为潜在的荧光材料方面得以应用。
发明内容
为此本发明人提供了如下的技术方案:
一种一维镉配合物的单晶,其特征在于该单晶结构采用APEX II CCD单晶衍射仪,使用经过石墨单色化的Mokα射线,λ = 0.71073 Å为入射辐射,以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,从差值傅立叶电子密度图利用软件解出单晶数据:
其结构如下:
[Cd(py)2(hipt)]·2py·2H2O,其中
py=吡啶;hipt=间羟基间苯二甲酸。
本发明进一步公开了一维镉配合物单晶的制备方法,其特征在于它是采用常温挥发法,将py、hipt和Cd(NO3)2·4H2O在水中搅拌半小时后过滤,滤液常温挥发两周后得到适合X-射线单晶衍射的无色块状晶体;其中py:hipt:Cd(NO3)2·4H2O的摩尔比为1:1:1;
一维镉配合物单晶的结构为[Cd(py)2(hipt)]·2py·2H2O;其中,py = 吡啶;hipt =间羟基间苯二甲酸;
py hipt。
本发明更进一步公开了一维镉配合物单晶作为潜在荧光材料在检测染料或发光剂的吸附量方面的应用,实验结果显示:
(1) 实施例1中的配合物单晶对染料具有很好的选择性和灵敏性,检测限达到0.1ppm。
(2)能够检出痕量的发光剂,检出限达到5.0µg/L。
(3)实施例1制备的配合物单晶对于染料的吸附量为1.4×10-3mol/cm2。
本发明一个优选的例子:
吡啶(py)(0.1mmol)、间羟基间苯二甲酸(hipt)(0.1mmol)和Cd(NO3)2·4H2O(0.1mmol)在水 (10 mL)中搅拌半小时后过滤,滤液常温挥发两周后得到适合X-射线单晶衍射的无色块状晶体。产率:40%。元素分析(C28H28CdN4O7) 理论值(%):C,52.14;H,4.38;N,8.69。实测值:C,52.05;H,4.35;N,8.72。
本发明公开的一种一维镉配合物单晶所具有的优点和特点在于:
(1) 反应操作简便易行。
(2) 反应收率高,所得产品的纯度高。
(3)本发明所制备的一维镉配合物单晶,生产成本低,方法简便,适合大规模生产。在染料或发光剂应用方面可以解决拓宽染料的光电响应范围问题。
附图说明
图1:配合物单晶的晶体结构图;
图2:配合物单晶的一维链状结构图。
具体实施方式
下面结合实施例对本发明做进一步的说明,实施例仅为解释性的,决不意味着它以任何方式限制本发明的范围。所用原料均有市售。所有原料都是从国内外的化学试剂公司进行购买,例如吡啶,间羟基间苯二甲酸等原料,没有经过继续提纯而是直接使用的。
实施例1
吡啶(py)(0.1mmol)、间羟基间苯二甲酸(hipt)(0.1mmol)和Cd(NO3)2·4H2O(0.1mmol)在水 (10 mL)中搅拌半小时后过滤,滤液常温挥发两周后得到适合X-射线单晶衍射的无色块状晶体。产率:40%。元素分析(C28H28CdN4O7) 理论值(%):C,52.14;H,4.38;N,8.69。实测值:C,52.05;H,4.35;N,8.72。
实施例2
晶体结构测定采用APEX II CCD单晶衍射仪,使用经过石墨单色化的Mokα射线,λ =0.71073 Å为入射辐射,以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,从差值傅立叶电子密度图利用软件解出晶体结构,并经洛仑兹和极化效应修正。所有的H原子由差值傅立叶合成并经理想位置计算确定。详细的晶体测定数据:
实施例3
染料或发光剂使用的实际例子
方法:染料溶液的微分脉冲伏安(DPV)曲线通过美国普林斯顿应用研究所研制的PARSTAT 2273电化学工作站测量。溶液的DPV测试采用三电极体系,玻碳电极为工作电极,辅助电极为铂片电极,自制的Ag/AgNO3电极为参比电极;电解液为0.1mol·L-1TBAP的乙腈溶液。以二茂铁氧化还原可逆点对为内标,得到测试体系与标准氢电极体系之间的校正值。
单色入射光光电转换效率(IPCE)描述DSCs在单色光作用下的光电转换效率,是转移到外电路的电子数与入射光子数之比。测量时,使用500 W氙灯作为光源,入射光经过WDS-5型组合式多功能光栅光谱仪得到不同波长λ下的单色光;单色光照射于电池的光阳极,由Keithley2400数字源表读取电流值I。单色光的福照度由USB4000 plug-and-play微型光线光谱仪测量。
步骤:为了确切了解染料在TiO2膜上的吸附量,将实施例1制备的配合物单晶染料敏化TiO2纳米晶膜(几何面积约为1 cm2)浸泡在10 mL 0.01 mol·L-1的氢氧化钠的甲醇溶液中过夜,待染料完全解附后测定溶液的吸光度。根据吸光度和摩尔吸光洗漱可以计算出单位面积纳米晶膜上染料的吸附量。该配合物单晶的吸附量为1.4 × 10-3 mol/cm2。
结果:与染料的甲醇溶液相比,配合物单晶染料在TiO2膜上的吸收光谱均明显变宽和红移。这表明染料分子在TiO2形成了首并尾的J-聚集体。从DSCs的工作原理讲,染料聚集引起的光谱宽化和红移对于染料的光电响应范围的拓宽是十分有利的。但与此同时,染料聚集体会大大降低其电子注入效率,从而导致DSCs的性能低下。所以,通常在染料溶液中加入共吸附剂来抑制染料的聚集。该配合物单晶在甲醇溶液中及其在TiO2膜电极上的紫溶液的荧光测试采用2.5×10-5 mol/L的甲醇溶液,最大荧光发射波长位于500 nm。
实施例4
一维镉配合物单晶作为制备发光材料的应用。
方法:通过荧光分光光度计,分别进行该化合物单晶(实施例1)的激发波长和发射波长的扫描,选择并确定最佳波长。
结论:该化合物的激发波长和发射波长分别为340 nm和500 nm。
步骤:将一维镉配合物单晶研磨压片成外径为27 mm、厚度约3 mm的片状样品,放入MPF-4荧光光谱仪的样品池进行测量。
结果:该化合物的激发波长λex = 340 nm,发射波长λem= 500 nm。
在详细说明的较佳实施例之后,熟悉该项技术人士可清楚地了解,在不脱离上述申请专利范围与精神下可进行各种变化与修改,凡依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均属于本发明技术方案的范围。且本发明亦不受说明书中所举实例实施方式的限制。
Claims (3)
1.一种一维镉配合物的单晶,其特征在于该单晶结构采用APEXIICCD单晶衍射仪,使用经过石墨单色化的Mokα射线,λ = 0.71073 Å为入射辐射,以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,从差值傅立叶电子密度图利用软件解出单晶数据:
其结构如下:
[Cd(py)2(hipt)]·2py·2H2O,其中
py = 吡啶;hipt = 间羟基间苯二甲酸。
2.权利要求1所述一维镉配合物单晶的制备方法,其特征在于它是采用常温挥发法,将py、tpa和Cd(NO3)2·4H2O在水中搅拌半小时后过滤,滤液常温挥发两周后得到适合X-射线单晶衍射的无色块状晶体;其中py:tpa:Cd(NO3)2·4H2O的摩尔比为1:1:1;
一维镉配合物单晶的结构为[Cd(py)2(hipt)]·2py·2H2O;其中py = 吡啶;hipt = 间羟基间苯二甲酸;
py hipt。
3.权利要求1所述一维镉配合物单晶作为潜在荧光材料在检测染料或发光剂的吸附量方面的应用。
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CN112142765A (zh) * | 2020-09-29 | 2020-12-29 | 桂林理工大学 | 间苯二甲酸镉配合物的晶体结构及其荧光性质 |
CN115582099A (zh) * | 2022-09-20 | 2023-01-10 | 池州学院 | 一种镉配合物吸附材料的制备方法与所得材料及其应用 |
CN115582099B (zh) * | 2022-09-20 | 2023-08-25 | 池州学院 | 一种镉配合物吸附材料的制备方法与所得材料及其应用 |
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