CN108165256A - 一种定向识别二氯甲烷、三氯甲烷、四氯甲烷的荧光变色材料及其制备方法 - Google Patents
一种定向识别二氯甲烷、三氯甲烷、四氯甲烷的荧光变色材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种新型定向识别CH2Cl2,CHCl3,CCl4的有机溶剂致荧光变色材料及其制备方法,属于纳米材料和配位化学的交叉领域。所述材料是以10核银硫簇为结点,双齿有机配体桥联的银硫簇基多孔配位聚合物。该化合物的化学式为:[Ag10(S t Bu)6(CF3COO)2(PhPO3H)2(bpy)2] n 。属于三斜晶系;空间群为P‑1。该材料能定向识别CH2Cl2,CHCl3,CCl4有机溶剂,孔隙率从9.8%达到最大的32%,灵敏高、响应速度快,并且具有长的检测寿命,能够循环使用,稳定性好等特点。在有机溶剂识别、检测方面具有巨大的应用前景。
Description
技术领域
本发明属于纳米材料和配位化学的交叉领域,具体涉及一种新型定向识别CH2Cl2,CHCl3,CCl4有机溶剂致荧光变色材料及其制备方法。
背景技术
CH2Cl2,CHCl3,CCl4都是具有挥发性、可溶性和易燃性,对人体有害,特别是CHCl3,CCl4具有致癌性。目前,还没有简单有效的方法来检测识别这三种溶剂。因此,小型化、低成本、安全可靠的有机溶剂识别和检测装置具有巨大的商业价值。近年来,开发出快速响应、稳定性好、灵敏度高、识别范围广的有机溶剂识别、检测材料是化学工作者们孜孜以求的目标。基于荧光变色的有机溶剂检测材料具有无侵入性、高灵敏性、安全性等优点,吸引了材料科学和化学等领域的关注。
多孔配位聚合物是以金属离子或者金属簇为结点通过有机配体的桥联,自组装形成高度有序的晶态多孔材料。而相对于单一金属离子,以多核金属簇为结点更易于组装形成对溶剂分子敏感的多孔结构。此外,为了进一步提高簇基多孔配合物对溶剂分子的吸附性能从而提高灵敏性及响应速度,可以通过调节有机桥联配体的尺寸来调控孔道的大小,为溶剂分子进入孔道提供足够的空间;还可以通过对完全裸露于孔道中的有机配体进行功能化修饰,得到稳定检测性能优异的多孔材料。
由于巯基纳米银簇独特的刚性分子几何构型可以有效地控制其配位模式,加之其具有优异的光物理和光化学性能,基于巯基银簇多孔配位聚合物在有机溶剂分子敏感材料领域的应用展现出了巨大的前景。
发明内容
为开发灵敏高、响应速度快等性能更优异的荧光变色有机溶剂检测材料,本发明的目的在于提供基于10核纳米巯基银簇的具有定向检测CH2Cl2,CHCl3,CCl4性能的多孔簇基配位聚合物及其制备方法。
为实现本发明目的,本发明公开了一种定向检测CH2Cl2,CHCl3,CCl4的有机溶剂致荧光变色性能的簇基多孔配位聚合物,所述簇基多孔配位聚合物的化学式是:[Ag10(StBu)6(CF3COO)2(PhPO3H)2(bpy)2]n,属于三斜晶系;空间群为P-1。
其中bpy为4,4'-联吡啶,结构简式如下:
该定向检测CH2Cl2,CHCl3,CCl4的有机溶剂致荧光变色材料的制备方法通过如下步骤实现:
将叔丁基硫银加入到丙酮和乙醇混合溶液中,快速搅拌;加入三氟乙酸银,搅拌至溶液澄清;再加入苯基膦酸,最后加入bpy,继续搅拌反应。反应结束后,将溶液在室温下避光挥发,得晶体,过滤、用乙醇洗涤、室温晾干后得新型有机溶剂致荧光变色材料。
各组分摩尔范围:叔丁硫银(0.05mmol~0.15mmol),三氟乙酸银(0.05mmol~0.15mmol),苯基膦酸(0.1mmol~0.26mmol),bpy(0.1mmol~0.24mmol),乙醇/丙酮(1:1,6ml~12ml)。
所述材料是一个独一无二的以10核巯基银簇为结点,通过bpy双齿配体桥联形成的二维层状结构;层和层之间以ABAB形式堆积,且通过强的氢键作用形成稳定的三维超分子结构;该材料是一个柔性框架,具有动态的闭合的孔道,通过氢键的作用层可以发生滑移调节孔隙,孔隙率从9.8%达到最大的32%(图2所示)。
本发明有机溶剂致荧光变色材料用于CH2Cl2,CHCl3,CCl4的识别与检测。由于材料具有柔性的框架,在有机溶剂分子的刺激下结构展现明显的呼吸效应,对溶剂小分子具有较强的吸附能力。孔道中溶剂分子与配体相互作用,影响材料激发态能级,导致不同溶剂中,材料荧光性质发生变化,即材料的荧光颜色及最大发射峰波长位置不同。因此,可根据荧光颜色及光谱来识别、检测有机溶剂。
具体描述如下:
有机溶剂的识别:
CH2Cl2,CHCl3,CCl4的识别检测:在本发明材料上分别滴加CH2Cl2,CHCl3,CCl4,分别测其荧光光谱。将上述材料放置在空气中,待有机溶剂挥发完全,再测材料的荧光光谱。这样循环数次后,材料的荧光发射性质没有发生任何变化,说明材料在长时间、多次循环有机溶剂检测中能保持优异的稳定性。
本发明优点:所制备的新型多孔簇基配位聚合物荧光变色材料能定向识别CH2Cl2,CHCl3,CCl4有机溶剂,孔隙率从9.8%达到最大的32%,响应速度快(响应时间小于1s)。并且具有长的检测寿命,能够循环使用,稳定性好等特点。是制作小型化,低成本有机溶剂检测装置的极具潜力的安全可靠材料,在有机溶剂识别、检测方面具有巨大的应用前景。合成方法简单可行,产率较高,达75%以上。
附图说明
图1为本发明所述定向识别CH2Cl2,CHCl3,CCl4的有机溶剂致荧光变色材料的结构单元图。
图2为本发明所述定向识别CH2Cl2,CHCl3,CCl4的有机溶剂致荧光变色材料的结构示意图。
图3为本发明所述定向识别CH2Cl2,CHCl3,CCl4的有机溶剂致荧光变色材料的XRD图,图中,1-本发明材料,2-模拟。
图4为本发明所述有机溶剂致荧光变色材料滴加CH2Cl2,CHCl3,CCl4溶剂后的荧光光谱(激发波长为365nm,室温),图中,1-CH2Cl2,2-CCl4,3-CHCl3。
图5为本发明所述有机溶剂致荧光变色材料365nm紫外灯下滴加CH2Cl2,CHCl3,CCl4溶剂后的荧光照片,图中,1-CH2Cl2,2-CCl4,3-CHCl3。
图6为本发明所述有机溶剂致荧光变色材料的CH2Cl2,CHCl3,CCl4溶剂的吸附曲线(室温)图中,1-CHCl3,2-CH2Cl2,3-CCl4。
具体实施方式
下面通过实例对本发明做进一步的说明:
实施例1:合成有机溶剂致荧光变色材料
将0.02g(0.1mmol)叔丁基硫银(ButSAg)置于3mL丙酮和3mL乙醇的混合溶液中,快速搅拌;加入0.02g(0.1mmol)三氟乙酸银(CF3COOAg),搅拌至溶液澄清;加入0.02g(0.13mmol)苯基膦酸,最后加入0.02g(0.12mmol)4,4'-联吡啶(bpy),继续搅拌5分钟。反应结束后,将溶液在室温下避光挥发,3天后得约20mg浅黄色块状晶体,产率75%,过滤、用乙醇洗涤、室温晾干后得有机溶剂致荧光变色材料。
实施例2:本发明材料对有机溶剂识别、检测现象
取实施例1制得的有机溶剂致荧光变色材料样品,在365nm紫外灯的照射下,在材料上分别滴加CH2Cl2,CHCl3,CCl4,材料的荧光颜色分别是绿色,橘黄色,黄绿色。从图4和5可以看出本材料实现了对这三种溶剂的检测肉眼可识别。
实施例3:本发明材料有机溶剂识别荧光光谱测定和溶剂吸附测试。
取实施例1制得的机溶剂致荧光变色材料粉末样品20mg,装入荧光测试固体样品槽中,往样品上滴加25μL有机溶剂(CH2Cl2,CHCl3,CCl4,将材料润湿完全),测其荧光光谱(激发波长365nm)。不同有机溶剂下本发明材料的荧光最大发射峰波长不一样,氯仿及四氯化碳与二氯甲烷相比,对该材料的激发态有更好的稳定作用,所以荧光发射位置红移,二氯甲烷作用下,该材料的荧光发射位置与本身的荧光发射位置相比没有变化。待样品中的有机溶剂挥发干后,测其无溶剂的荧光光谱。如此在加入溶剂和挥发溶剂的循环中,测其荧光光谱,证明其稳定性。同时,取经过抽真空处理的该材料的粉末样品250mg,分别测试其室温下的有机溶剂(CH2Cl2,CHCl3,CCl4)的吸附曲线,进一步证明这些溶剂分子可以打开该材料闭合的孔道,并且与该材料发生作用。
取实施例1制得的有机溶剂致荧光变色材料做进一步表征,其过程如下:
(1)晶体结构测定
本发明聚合物的X射线单晶衍射数据用大小合适的单晶样品在Rigaku XtaLAB Pro转靶单晶仪上测定。数据均用经石墨单色化的Cu-Kα射线(λ=1.54184)为衍射源通过ω扫描方式在室温下收集,并经过Lp因子校正和半经验吸收校正。结构解析是先通过SHELXT-2015程序用直接法得到初结构,然后使用SHELXT-2015程序用全矩阵最小二乘法精修。所有非氢原子均采用各向异性热参数法精修。配位水和配体的氢原子坐标由理论加氢得到,溶剂上的氢原子则通过差值Fourier法得到,所有的氢原子都采用各向同性热参数法精修。详细的晶体测定数据见表1;重要的键长数据见表2。
表1本发明有机溶剂致荧光变色材料的主要晶体学数据
表1主要晶体学数据
aR1=∑IIFoI-IFcII/∑IFoI.bwR2=[∑w(Fo 2-Fc 2)2/∑w(Fo 2)2]1/2
表2重要的键长
对称代码:11-x,1-y,1-z.
本发明有机溶剂致荧光变色材料的X射线粉末衍射(XRD)表征
本发明有机溶剂致荧光变色材料的XRD图见图3。用该材料的单晶结构数据模拟所得的XRD数据和实验所测的XRD数据作图,{仪器型号:Rigaku D/max-3B衍射仪(Cu-Kα,λ=1.5418)},结果一样。
Claims (4)
1.一种荧光变色材料,其特征在于:所述荧光变色材料的化学式为:[Ag10(StBu)6(CF3COO)2(PhPO3H)2(bpy)2]n,属于三斜晶系;空间群为P-1,其中bpy为4,4'-联吡啶,其结构单元如下:
2.制备如权利要求1所述的荧光变色材料的方法,其特征在于,通过以下步骤实现:将叔丁基硫银加入到丙酮和乙醇混合溶液中,快速搅拌;加入三氟乙酸银,搅拌至溶液澄清;再加入苯基膦酸,最后加入4,4'-联吡啶,继续搅拌反应;反应结束后,将溶液在室温下避光挥发,得晶体,过滤、经洗涤、晾干后得荧光变色材料。
3.如权利要求1所述的荧光变色材料在有机溶剂识别及检测中的应用,其特征在于,将其应用于CH2Cl2,CHCl3,CCl4的定向识别与检测。
4.如权利要求3所述的荧光变色材料在有机溶剂识别及检测中的应用,其特征在于,在365nm紫外灯的照射下,在荧光变色材料上分别滴加CH2Cl2,CHCl3,CCl4,荧光颜色分别是绿色,橘黄色,黄绿色,对这三种溶剂肉眼检测识别。
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CN116102738A (zh) * | 2022-11-23 | 2023-05-12 | 周口师范学院 | 一种新型高量子效率的绿色发光材料及制备方法 |
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