摘要
近年来,金属-有机框架(Metal-Organic Frameworks, MOFs)材料在能源气体储存及分离、生物及环境荧光探测等领域显示出重要的潜在应用而受到广泛关注。但是,传统MOFs材料通过较弱且选择性差的范德华力吸附气体分子,限制了其气体吸附容量和选择性的提高,因此需要对MOFs材料进行功能化修饰以增加其与目标气体分子的吸附强度及选择性。然而目前MOFs材料功能化修饰的研究开展还较少,采用多种功能修饰策略的研究更是较少涉及。同时,研制兼具高气体吸附容量和高吸附选择性的优异综合吸附性能的MOFs材料尚存在较大困难。而在MOFs材料荧光探测领域,MOFs材料的研究主要集中在块体MOFs的制备和应用,块体材料较大的尺寸限制了其在细胞及生物活体内的应用。但对MOFs材料的尺寸调控及纳米MOFs的研究尚在起步阶段。
针对上述科学问题,本文开展了金属-有机框架材料的功能修饰、尺寸调控和性能研究：设计并合成了一种采用阳离子型框架的新型MOF材料,探索了离子型框架功能修饰策略对烷烃气体吸附与分离性能的影响；开发了采用多功能修饰并具有优异乙炔气体吸附与分离性能的新型MOF材料；研究阐明了MOFs材料中功能修饰策略对气体吸附和分离性能的协同作用和作用机理；探索了稀土-有机框架材料的尺寸调控方法,并成功研制了纳米稀土-有机框架材料,研究了其对细菌孢子及硝基爆炸物的荧光探测性能,为进一步开发可直接应用于细胞及生物活体内生物荧光探针奠定了基础。
设计并合成了一种具有阳离子型框架功能修饰的新型MOF材料Zn8O(EDDA)4(ad)4·(HEDDA)2·6DMF·27H2O (ZJU-48; H2EDDA=二甲基-(E)-均二苯代乙烯-4,4-乙二酸;ad=腺嘌呤)。并采用气体吸附测试研究了阳离子型框架功能修饰策略对样品气体吸附性能的作用。ZJU-48是具有阳离子型框架的三维多孔结构,孔洞尺寸为9.1×9.1A2。N2吸附测试表明ZJU-48a是I型等温吸附线,BET比表面积1450m2g-1。ZJU-48a对乙炔的吸附量(57cm3g-1)远高于具有类似结构并得到大量研究的中性MOF材料MOF-5(26cm3g-1),表明离子型框架可以显著增强MOFs材料的气体吸附容量。ZJU-48a对乙烷／甲烷的吸附选择性约为6.0,对C1/C2烷烃气体可以进行有效分离。ZJU-48a对乙烷的吸附焓高达28.0KJ mol-1,是目前报道的MOFs材料乙烷吸附焓最高值之一。这主要是因为ZJU-48a的离子型骨架自身的电荷可以诱导气体分子发生极化从而产生静电作用,有效增强了烷烃气体与MOF材料孔洞内壁之间的作用。进一步采用吸附床分离和脉冲色谱柱分离等理论计算方法模拟了ZJU-48a对烷烃气体的实际分离过程,结果表明ZJU-48a对C1/C2烷烃气体可进行有效的实际分离。离子型框架功能修饰策略为烷烃气体吸附与分离材料的设计研究提供了一种新的思路。
设计并合成了一种兼具开放金属位和Lewis吡啶位的多功能修饰位点的新型MOF材料Cu6(PDC)6·2.6H20(UTSA-50；PDC=3,5-吡啶二羧酸),并采用气体吸附测试研究了多功能修饰位点对乙炔气体吸附性能的作用机理。UTSA-50是孔洞中具有Cu(II)开放金属位和Lewis比啶位的多功能修饰位点的三维结构,其孔洞尺寸大小为6～11A。N2吸附测试表明UTSA-50a是I型等温吸附线,BET比表面积为865.09m2g-1。UTSA-50a的乙炔吸附量(90.6cm3g-1)远高于没有功能位点修饰的MOF-5(26cm3g-1).ZIF-8(25cm3g-1)及具有阳离子框架功能修饰的ZJU-48(57.07cm3g-1).UTSA-50a对乙炔的吸附焓高达39.4kJmo1-1。开放金属位和Lewis吡啶位通过与乙炔气体形成静电及氢键作用极大地增加了其的乙炔吸附作用力。296K下UTSA-50a对C2H2/CH4的吸附选择性高达68.0,是迄今为止报道的最高值。研究表明,将开放金属位和Lewis吡啶位相结合的多功能修饰策略可以显著提高MOFs材料的吸附容量和选择性,为设计与制备具有高效气体吸附与分离性能的MOFs材料提供了重要的指导作用。
采用微乳液体系对稀土-有机框架材料Eu2(Fuma)2(Oxa)·8H20(EuFO；Fuma=富马酸；Oxa=草酸)的尺寸进行调控,利用BFDH理论对EuFO的可控生长机理进行了理论模拟,并研究了纳米EuFO材料对细菌孢子的主要成分2,6-吡啶二羧酸(简称DPA)的荧光探测性能。通过水和表面活性剂的摩尔比(简称W值)可对EuFO晶体的尺寸和形貌进行调控,实现了EuFO从大尺寸晶体、微米晶体到纳米晶体的一系列制备过程。其中,当W=15时,得到尺寸约为100nm的六边形片状纳米晶。利用BFDH理论计算得到EuFO晶体的三个生长晶面族{111}、{004}和{022｝,并通过模拟添加表面活性剂后三个生长晶面族生长速率的变化而得到与实验结果一致的晶体形貌。该理论模拟的结果可以阐明EuFO晶体的形貌变化过程,对纳米MOFs材料的可控制备具有重要的指导意义。荧光测试结果表明,EuFO六边形纳米片晶对DPA具有高灵敏度和高选择性的荧光增强探测性能。通过瞬态光谱测试对样品的荧光探测机理进行了研究。结果表明,EuFO对DPA探测的荧光增强效应主要是DPA与Eu(III)离子发生配位引起的。研究表明,MOFs材料的尺寸和形貌可以通过微乳液法进行精确调控并制备纳米MOFs材料,成功实现对细菌孢子的高灵敏度及高选择性的荧光探测。该研究为细胞及生物活体内的生物荧光探针应用奠定了基础。
采用微乳液法制备了稀土-有机框架材料Eu2(BDC)3(H2O)4(EuBDC；BDC=对苯二甲酸)的纳米晶体,并研究了其对硝基爆炸物的荧光探测性能。在W=15的条件下,得到尺寸约为100nn的EuBDC纳米棒。荧光探测实验结果表明,EuBDC纳米棒对硝基爆炸物具有高灵敏度和高选择性的荧光淬灭探测性能。通过瞬态光谱测试和紫外-可见吸收光谱研究了样品的荧光探测机理。结果表明,EuBDC中的有机配体BDC和硝基苯衍生物对激发光能量存在竞争吸收,引起BDC所能吸收的能量被“过滤”,因而其通过天线效应传递给EU(Ⅲ)离子的能量减少,Eu(Ⅲ)离子的发光发生淬灭。上述研究结果表明,纳米MOFs材料可以实现高灵敏度、高选择性和快速便捷的荧光探测。MOFs材料的尺寸调控和纳米MOFs制备作为一种重要的策略有望制备出性能优异、具有广泛应用前景的新型生物及环境荧光探针。
Recent years, Metal-Organic Framework (MOF) materials have drawn great attentions due to their potential applications in gas sorption/separation and luminescent sensing. In this dissertation, the recent progress of MOF materials is reviewed, with specific focus on the functionalization, size control and properties of MOF materials. A cationic MOF material was synthesized, and small hydrocarbons C1/C2sorption/separation properties were studied. A MOF with both open metal sites and Lewis basic pyridyl sites was developed, and C2H2, CO2and CH4gas sorption/separation properties were explored. A nanoscale MOF material with controllable size was realized whose morphology has been simulated base on the BFDH method, and the sensing of bacteria endospores was research in detail. We also report the synthesis and sensing of nitroaromatic explosives of a nanoscale MOF material.
A new cationic MOF material ZJU-48(ZngO (EDDA)4(ad)4·(HEDDA)2·6DMF·27H2O; H2EDDA=(E)-4,4'-(ethene-1,2-diyl) dibenzoic acid; ad=adenine) was solvothermally synthesized and the gas sorption/separation properties for small hydrocarbons was studied. ZJU-48features a three-dimensional structure with cationic skeleton and has one-dimensional pores of about9.1×9.1A2. The N2sorption isotherm at77K showed that ZJU-48a displayed Type-I sorption behavior with a BET surface area of1450m2g-1. ZJU-48a takes up C2H2(57cm3g-1), and this value is higher than the one with similar Zn4O structure MOF-5(26cm3g-1), which revealed that the structrue feature of charged skeleton in ZJU-48a played an important role in its acetylene storage. The enthalpy of C2H6is28.0KJmol-1, which is very high and is even comparable to that of Mg-MOF-74. This indicated that the charged skeleton in ZJU-48a do enhance the affinity between MOF and small hydrocarbon molecules, presumably by charge-induced forces between the charged skeleton and polarized gas molecules. Moreover, the adsorption selectivities of C2H6with respect to CH4are in excess of6.0for a range of pressure to100KPa, indicating the feasibility of this MOF for the practical application on C2/C1separation. To further demonstrate the feasibility for the practical separation, the breakthrough and pulse chromatographic experiments were simulated and the result showed that ZJU-48a has the ability of separating CH4in pure form from this quaternary mixture. The results indicated that the charged skeleton strategy can enhance the affinity between MOF material and polarized C2gas molecules, this strategy provided a new design approach for MOF materials.
To immobilize both open metal sites and Lewis basic pyridyl sites into a microporous MOF material, UTSA-50(Cu6(PDC)6-2.6H2O; PDC=3,5-pyridine-dicarboxylate) was solvothermally synthesized and the C2H2, CO2and CH4gas sorption/separation properties were explored. UTSA-50features a three-dimensional structure with both open metal sites and Lewis pyridyl sites. The pore size is6-11A. The N2sorption isotherm at77K showed that UTSA-50a displayed Type-I sorption behavior with a BET surface area of604m2g"'. The amount of C2H2absorbed in UTSA-50(90.6cm3g-1) is higher than the ones without functionalization sites such as MOF-5, ZIF and cationic MOF ZJU-48. The storage density of adsorbed acetylene in UTSA-50a micropores is0.30g cm-3, which is among the high end for MOF materials. The enthalpy for acetylene reached a high value of39.4KJmol-1, which indicated that the high density of open metal sites and Lewis basic pyridyl sites do enhance the affinity between the MOF surface and acetylene molecules, presumably by Coulomb interactions and hydrogen bonding. The most remarkable feature of UTSA-50a is the significant high C2H2/CH4selectivity of68.0, which is the highest one ever reported. The results illustrated the power of collaborative immobilization of multiple functional sites and further realize both high acetylene capacity and selectivity. This research initiated an important design approach for highly effective gas sorption/separation MOF materials.
A nanoscale MOF material EuFO (Eu2(FMA)2(OX)(H2O)4-4H2O; FMA=fumarate, OX=oxalate) with controllable size and morphology is realized whose morphology has been simulated based on the BFDH method, and the sensing properties of bacteria spores was researched in detail. The sizes and morphologies can be tuned by the molar ratio of surfactant and H2O molar ratio (W value), which resulted the EuFO evolution from large to micro crystals, and finally became nano crystals. Hexagonal nanoplates with size of100nm can be synthesized at W=15. The BFDH method calculation showed that there were three possible growing facets for EuFO crystals, they are{022},{004} and {111}, and the addition of surfactant makes different facets growth rates, which finally leads to different sizes and morphologies of EuFO crystals. The hexagonal nanoplates showed highly sensitive and selective sensing of bacteria spore. Luminescent lifetime showed that the DPA molecules are involved in the binding with Eu(III) which can significantly enforce the intramolecule energy transfer. It is foreseen that functional nanoscale MOF will establish the foundation for in vivo biosensors.
A nanoscale MOF EuBDC (Eu2(BDC)3(H2O)2·(H2O)2; BDC=benzene-1,4-dicarboxylate) has been realized for sensing of nitroaromatic explosives. EuBDC nanorods with size of100nm can be synthesize by microemulsion method at W=15. The nanoscale EuBDC showed both highly sensitive and selective sensing of nitroaromatic explosives. Luminescent lifetime and UV-Vis showed that luminescence change of the nanoscale EuBDC was attributed to a competition of absorption of the light source energy, which decreased the probability of energy transferr from ligand to Eu(Ⅲ) and subsequently quenched the luminescence of Eu(Ⅲ). The results showed that size control of MOF materials is an important strategy to realize straightforward and high sensitive environmental and biological sensing.
引文
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