桥联聚倍半硅氧烷杂化材料及其金属配合物的制备与性能研究
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摘要
桥联聚倍半硅氧烷是一类新型的具有特殊性能的杂化材料,其前驱体单体的通式为：(R＇O)3Si-R-Si-(OR＇)3,式中R＇是烷基,R是作为“桥联”的有机功能性基团。有机桥联基团通过Si-C共价键使有机和无机组分相连并均匀分布于整个材料中,不存在普通杂化材料出现的两相分离以及相界面结合性弱的特点。它集无机材料优异的力学性能、高耐热性和有机材料柔韧性好、强度高等特点为一体,较普通的物理填充生成的杂化材料具有更为优异,在手性催化剂载体、介孔材料等领域有了广泛的应用,作为金属吸附材料或金属配位的功能材料的研究已经成为近几年的热点。此类金属配位的功能材料的结构特点是,有机桥联基团中具有与金属离子强烈配位的原子(N、O、S等)。当前,大部分的研究都集中在光电材料以及重金属吸附材料等领域,本文选择了含具有与金属离子强烈配位能力的芳环亚胺及联吡啶基的两类有机桥联的桥联倍半硅氧烷为前驱体,通过溶胶-凝胶法制备了相应的桥联聚倍半硅氧烷及其金属配位聚合物,经过表征,研究了它们的热性能、结构性能并测定相应配位聚合物的磁性能,得到了一些创新性结果。研究的主要内容包括：
(1)以合成的三种含芳基亚胺桥联倍半硅氧烷为单体,加入镍盐(醋酸镍),盐酸作为催化剂,利用溶胶-凝胶法制备了此类桥联聚倍半硅氧烷2,2＇-PSBBS(3a,b)、4,4＇-PSBBS(3＇)及其配合物2,2＇-PSBBSS-Ni(4a,b)、4,4＇-PSBBS-Ni(4＇)。通过红外、紫外等分析手段发现在配合物中相应吸收峰出现一定程度的红移,结合元素分析验证了配合物的结构。同时,运用TGA、SEM、XRD等测试手段对它们相应的性能进行测试,结果表明,这些桥联聚倍半硅氧烷金属配合物的热稳定性较相应的桥联聚倍半硅氧烷有一定程度的提高,聚合物均为均一的球状粒子,有一定的团聚,相应的金属配合物表现出无定形、非晶态结构,在小角XRD中并无衍射信号,为非介孔材料。在低温下对三种金属配合物的磁性能进行研究,它们的居里-外斯温度都为正,表明它们都具有铁磁性,其中2,2'-PSBBS-Ni(4a)具有较大的矫顽力(1820 Oe)、剩余磁感强度(2.51 emu/g)以及磁滞回线面积,表现出硬铁磁性,而2,2'-PSBBS-Ni(4b)和4：4'-PSBBS-Ni(4＇)具有较小的矫顽力(350 Oe和36 Oe)、剩余磁化强度(0.1966 emu/g和0.005 emu/g)以及磁滞回线面积,表现出软铁磁性,但是4,4＇-PSBBS-Ni(4＇)在70K时存在一个从铁磁体到抗磁体的转变温度而表现出特殊的性质。
(2)以合成的含联吡啶基桥联倍半硅氧烷BPYBS(4)为单体,分别加入镍盐(醋酸镍)或铽盐(氯化铽),以盐酸作为催化剂,经过水解缩聚也制备了此类桥联聚倍半硅氧烷BPYPBS及配合物BPYPBS-Ni2+和BPYPBS-Tb3+。运用与上述相同的分析测试手段对它们进行了结构的表征和性能的测试。结果表明,这两种配合物热稳定性较BPYPBS有一定的提高,聚合物为均一的球状粒子,有团聚现象,经XRD分析,BPYPBS及其配合物BPYPBS-Ni2+和BPYPBS-Tb3+为无定形、非晶态结构,并且为非介孔材料。两种配合物的磁性能研究表明两者都具有铁磁性,BPYPBS-Ni2+具有较大的矫顽力、剩余磁感强度以及磁滞回线面积,表现出硬铁磁性,而BPYPBS-Tb3+具有很小的矫顽力、剩余磁感强度以及磁滞回线面积,表现出软铁磁性。
Bridged polysilsesquioxanes are a kind of novel hybrid material, which exhibit many excellent properties. The general formula of their precursors is (R'O)3Si-R-Si-(OR')3, where R' stands for alkyl while R represents an organic functional group. The organic bridging group covalently bond to the component by Si-C bond throughout the whole material. Compared to normal hybrid materials, there is no two-phase separation and weak interfacial bonding occuring in bridged polysilsesquioxanes. It combines excellent mechanical properties, heat resistance of inorganic materials and good flexibility, high intensity of organic materials together and is superior to those of ordinary hybrid materials. Bridged polysilsesquioxanes have been widely applied as chiral catalyst support and mesoporous materials. It also has attracted increasing attention in the field of metal absorption materials and metal-coordinated functional materials in recent years. Generally, this kind of bridged materials always posseses special atoms (N,O, S, etc.), which have a strong coordination ability with metal ions. However, most studies have focused on those of photo-electric materials and heavy metal absorption materials. In this paper, the preparation of two serieses of novel bridged polysilsesquioxanes and their metal coordination polymer based on aromatic imine and bipyridyl are presented. Their thermal properties, structure properties and magnetic properties were investigated. Some significant results were also obtained. The main results are outlined below:
(Ⅰ) Bridged polysilsesquioxanes 2,2'-PSBBS-(3a,b)、4,4'-PSBBS (3') and their metal coordinated polymer 2,2'-PSBBS-Ni (4a,b)、4,4'-PSBBS-Ni (4') were prepared by sol-gel method from three kinds of aromatic imine-bridged silsesquioxanes and Nickle salt (Nickel acetate) under the catalysis of diluted hydrochloric acid. The structures of the coordinated polymers were verified with infrared ray spectrometry, ultraviolet spectrometry and elemental analysis. It was found that the corresponding absorption peak of the coordinated polymer showed an obvious red shift. At the same time, the properties of these polymers were investigated with thermogravimetric analysis (TGA), scanning electron microscope (SEM) and X-ray diffraction (XRD). The TGA results suggested that the thermal stabilities were improved compared to those of corresponding bridged polysilsesquioxanes. Based on the SEM images, it was displayed that the homogeneous and spherical particles were formed. From the XRD investigation, it was found that the coordinated polymer were all amorphous and non-crystalline. The fact that there were no diffractive signals in the small-angle XRD also suggested that they were not mesoporous materials. The magnetic properties of the three imine-bridged polysilsesquioxanes and their coordinated polymers were examined. The Courier temperature was above zero, which means they all showed ferromagnetism. The fact that 2,2'-PSBBS-Ni (4a) exhibited large coercive force (1820 Oe), remanent magnetization (2.51emu/g) and area of magnetic hysteresis loop suggested a hard-ferromagnet. However,2,2'-PSBBS-Ni (4b) and 4,4'-PSBBS-Ni (4') were a soft- ferromagnet. It is worth noting that there existed a transition temperature at 70K for 4,4'-PSBBS-Ni (4'), above which it was a diamagnet and below a ferromagnet.
(Ⅱ) Bridged polysilsesquioxanes BPYPBS together with its metal coordinated polymer (BPYPBS-Ni2+) and (BPYPBS-Tb3+) were also prepared by sol-gel technology from bipyridyl-bridged silses- quioxanes and the nickle salt (Nickel acetate) or terbium salt (Terbium chloride) under the catalysis of diluted hydrochloric acid. The structure and properties of the polymers were characterized through the same method as described in section (Ⅰ). The results showed that the thermal stabilities of the coordinated polymers were also improved compared to those of bridged polysilsesquioxanes. SEM images showed that the surfaces were homogeneous and the globular particles were also congregated together. In addition, all of them were amorphous and had no mesostructure.The magnetic properties of the two coordinated polymers were tested and both exhibited ferromagnetism. BPYPBS-Ni2+ was a hard-ferromagnet due to its large values of coercive force (1290 Oe), remanent magnetization (7.24 emu/g) and area of magnetic hysteresis loop. However, BPYPBS-Tb3+ was a soft-ferromagnet ascribed to its small values of coercive force (18.74 Oe), remanent magnetization (0.01 emu/g) and area of magnetic hysteresis loop.
(1)以合成的三种含芳基亚胺桥联倍半硅氧烷为单体,加入镍盐(醋酸镍),盐酸作为催化剂,利用溶胶-凝胶法制备了此类桥联聚倍半硅氧烷2,2＇-PSBBS(3a,b)、4,4＇-PSBBS(3＇)及其配合物2,2＇-PSBBSS-Ni(4a,b)、4,4＇-PSBBS-Ni(4＇)。通过红外、紫外等分析手段发现在配合物中相应吸收峰出现一定程度的红移,结合元素分析验证了配合物的结构。同时,运用TGA、SEM、XRD等测试手段对它们相应的性能进行测试,结果表明,这些桥联聚倍半硅氧烷金属配合物的热稳定性较相应的桥联聚倍半硅氧烷有一定程度的提高,聚合物均为均一的球状粒子,有一定的团聚,相应的金属配合物表现出无定形、非晶态结构,在小角XRD中并无衍射信号,为非介孔材料。在低温下对三种金属配合物的磁性能进行研究,它们的居里-外斯温度都为正,表明它们都具有铁磁性,其中2,2'-PSBBS-Ni(4a)具有较大的矫顽力(1820 Oe)、剩余磁感强度(2.51 emu/g)以及磁滞回线面积,表现出硬铁磁性,而2,2'-PSBBS-Ni(4b)和4：4'-PSBBS-Ni(4＇)具有较小的矫顽力(350 Oe和36 Oe)、剩余磁化强度(0.1966 emu/g和0.005 emu/g)以及磁滞回线面积,表现出软铁磁性,但是4,4＇-PSBBS-Ni(4＇)在70K时存在一个从铁磁体到抗磁体的转变温度而表现出特殊的性质。
(2)以合成的含联吡啶基桥联倍半硅氧烷BPYBS(4)为单体,分别加入镍盐(醋酸镍)或铽盐(氯化铽),以盐酸作为催化剂,经过水解缩聚也制备了此类桥联聚倍半硅氧烷BPYPBS及配合物BPYPBS-Ni2+和BPYPBS-Tb3+。运用与上述相同的分析测试手段对它们进行了结构的表征和性能的测试。结果表明,这两种配合物热稳定性较BPYPBS有一定的提高,聚合物为均一的球状粒子,有团聚现象,经XRD分析,BPYPBS及其配合物BPYPBS-Ni2+和BPYPBS-Tb3+为无定形、非晶态结构,并且为非介孔材料。两种配合物的磁性能研究表明两者都具有铁磁性,BPYPBS-Ni2+具有较大的矫顽力、剩余磁感强度以及磁滞回线面积,表现出硬铁磁性,而BPYPBS-Tb3+具有很小的矫顽力、剩余磁感强度以及磁滞回线面积,表现出软铁磁性。
Bridged polysilsesquioxanes are a kind of novel hybrid material, which exhibit many excellent properties. The general formula of their precursors is (R'O)3Si-R-Si-(OR')3, where R' stands for alkyl while R represents an organic functional group. The organic bridging group covalently bond to the component by Si-C bond throughout the whole material. Compared to normal hybrid materials, there is no two-phase separation and weak interfacial bonding occuring in bridged polysilsesquioxanes. It combines excellent mechanical properties, heat resistance of inorganic materials and good flexibility, high intensity of organic materials together and is superior to those of ordinary hybrid materials. Bridged polysilsesquioxanes have been widely applied as chiral catalyst support and mesoporous materials. It also has attracted increasing attention in the field of metal absorption materials and metal-coordinated functional materials in recent years. Generally, this kind of bridged materials always posseses special atoms (N,O, S, etc.), which have a strong coordination ability with metal ions. However, most studies have focused on those of photo-electric materials and heavy metal absorption materials. In this paper, the preparation of two serieses of novel bridged polysilsesquioxanes and their metal coordination polymer based on aromatic imine and bipyridyl are presented. Their thermal properties, structure properties and magnetic properties were investigated. Some significant results were also obtained. The main results are outlined below:
(Ⅰ) Bridged polysilsesquioxanes 2,2'-PSBBS-(3a,b)、4,4'-PSBBS (3') and their metal coordinated polymer 2,2'-PSBBS-Ni (4a,b)、4,4'-PSBBS-Ni (4') were prepared by sol-gel method from three kinds of aromatic imine-bridged silsesquioxanes and Nickle salt (Nickel acetate) under the catalysis of diluted hydrochloric acid. The structures of the coordinated polymers were verified with infrared ray spectrometry, ultraviolet spectrometry and elemental analysis. It was found that the corresponding absorption peak of the coordinated polymer showed an obvious red shift. At the same time, the properties of these polymers were investigated with thermogravimetric analysis (TGA), scanning electron microscope (SEM) and X-ray diffraction (XRD). The TGA results suggested that the thermal stabilities were improved compared to those of corresponding bridged polysilsesquioxanes. Based on the SEM images, it was displayed that the homogeneous and spherical particles were formed. From the XRD investigation, it was found that the coordinated polymer were all amorphous and non-crystalline. The fact that there were no diffractive signals in the small-angle XRD also suggested that they were not mesoporous materials. The magnetic properties of the three imine-bridged polysilsesquioxanes and their coordinated polymers were examined. The Courier temperature was above zero, which means they all showed ferromagnetism. The fact that 2,2'-PSBBS-Ni (4a) exhibited large coercive force (1820 Oe), remanent magnetization (2.51emu/g) and area of magnetic hysteresis loop suggested a hard-ferromagnet. However,2,2'-PSBBS-Ni (4b) and 4,4'-PSBBS-Ni (4') were a soft- ferromagnet. It is worth noting that there existed a transition temperature at 70K for 4,4'-PSBBS-Ni (4'), above which it was a diamagnet and below a ferromagnet.
(Ⅱ) Bridged polysilsesquioxanes BPYPBS together with its metal coordinated polymer (BPYPBS-Ni2+) and (BPYPBS-Tb3+) were also prepared by sol-gel technology from bipyridyl-bridged silses- quioxanes and the nickle salt (Nickel acetate) or terbium salt (Terbium chloride) under the catalysis of diluted hydrochloric acid. The structure and properties of the polymers were characterized through the same method as described in section (Ⅰ). The results showed that the thermal stabilities of the coordinated polymers were also improved compared to those of bridged polysilsesquioxanes. SEM images showed that the surfaces were homogeneous and the globular particles were also congregated together. In addition, all of them were amorphous and had no mesostructure.The magnetic properties of the two coordinated polymers were tested and both exhibited ferromagnetism. BPYPBS-Ni2+ was a hard-ferromagnet due to its large values of coercive force (1290 Oe), remanent magnetization (7.24 emu/g) and area of magnetic hysteresis loop. However, BPYPBS-Tb3+ was a soft-ferromagnet ascribed to its small values of coercive force (18.74 Oe), remanent magnetization (0.01 emu/g) and area of magnetic hysteresis loop.
引文
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