磁性离子液体的合成表征及磁性研究
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摘要
基于磁性离子液体的优良特性,本文设计并合成了一系列功能化的磁性离子液体,研究了磁性离子液体的物理化学性质,并对磁性离子液体的磁性进行了研究,概括总结了阴阳离子结构对磁性离子液体磁性的影响。同时将特殊功能化的磁性离子液体与碳纳米管结合,得到了具有磁性的碳纳米管。论文的主要内容如下:
1)合成了[C4mim]Cl/FeCl3体系磁性离子液体,通过改变原料配比考察了磁性离子液体阴离子的存在形式。研究表明原料配比是导致不同阴离子构型的主要因素,不同的阴离子构型使磁性离子液体具有不同的物理性质和电化学性质。另外,通过对[C4mim]Br/FeCl3体系磁性离子液体的研究,证明了磁性离子液体阴离子络合物形成的过程中有离子相互交换现象,从而揭示了磁性离子液体的形成机理。
2)设计并合成了一种乙烯基咪唑类离子液体[Vmim]X(X=Cl、Br),通过对反应条件的优化,得到了较高的转化率和选择性,通过对合成的乙烯基功能化的咪唑类离子液体进行物性研究,发现乙烯基的引入使该离子液体的物理化学性质发生了很大改变。再者,以[Vmim]X为原料,合成了具有π-π共轭阳离子结构的磁性离子液体[Vmim]X/FeCl3,进一步,将[Vmim]FeCl4聚合制备出了聚合磁性离子液体PMIL。
3)以单壁碳纳米管SCNT为载体,以[Vmim]FeCl4为原料制备出了磁性碳纳米管MCNT,通过Raman、IR和SEM等测试手段对磁性碳纳米管的结构进行了表征,初步结果表明,聚合阳离子包裹在了碳纳米管表面,而磁性阴离子[FeCl4]-则进入了碳纳米管管内。
4)合成了一系列含金属铁离子的双咪唑类磁性离子液体:[C2(mim)2][FeCl4]2、[C4(mim)2][FeCl4]2、[C2(mim)2]Br2/FeCl3、[C4(mim)2]Br2/FeCl3,并对其热力学性质进行了研究。另外合成了一系列含镝的双咪唑磁性离子液体: [C2(mim)2]2[Dy(SCN)7]、[C4(mim)2]2[Dy(SCN)7]、[C6(mim)2]2[Dy(SCN)7]、[C8(mim)2]2[Dy(SCN)7]、[C10(mim)2]2[Dy(SCN)7]。培养出了[C4(mim)2]2[Dy(SCN)7]和[C6(mim)2]2[Dy(SCN)7]的单晶,并对其晶体结构进行了表征分析。结果表明,金属离子Dy3+在磁性离子液体中属于七配位,属首次报道。
5)对所合成的所有磁性离子液体进行了磁性表征,分析并总结了磁性离子液体阳离子结构、阴离子结构对磁性大小的影响。同时对负载型磁性离子液体的磁性进行了研究,初步结果表明,碳纳米管的特殊结构使磁性离子液体显示出了铁磁性。
A novel series of magnetic ionic liquids (MILs) have been synthesized by introducing complex ions of metals into ionic liquids. The physicochemical properties, such as density, viscosity, melting point and onset temperatures etc, were investigated. Through researches on magnetic properties of these MILs, several magnetic theories were founded. And magnetic carbon nanotubes (MCNT) as the combination of single-walled carbon nanotube and special-designed MIL were prepared. The major work and innovative results for this dissertation are as follows:
1) Two MILs systems [C4mim]Cl/FeCl3 and [C4mim]Br/FeCl3 were designed. And three magnetic ionic liquids, [C4mim]FeCl4, [C4mim]FeCl4+[C4mim]Fe2Cl7 and [C4mim]FeBrCl3 (main material in [C4mim]Br/FeCl3) were synthesized using standard method, which indicated that the molar ratio [C4mim]Cl/FeCl3 has crucial influence on the structure of complex ions, and there were ion exchange among complex ions.
2) A novel route was designed for the synthesis of vinyl-functionalized imidazolium-based ionic liquids, and the reaction conditions such as reaction temperature, selection of nucleophile etc were optimized. Moreover, magnetic ionic liquids [Vmim]FeCl4 and [Vmim]Br/FeCl3 havingπ-πconjunction structure were synthesized from vinyl-functionalized imidazolium-based ionic liquids, and PMIL was prepared by polymerization of [Vmim]FeCl4.
3) The single-walled carbon nanotubes functionalized by magnetic ionic liquid [Vmim]FeCl4 have been synthesized through the polymerization reaction of [Vmim]FeCl4 in methanol. And the structure of the functionalized single-walled carbon nanotubes was investigated by IR and Roman spectrum, which indicated that cation [Vmim]+ were supported on the surfaces of SCNTs, and anion [FeCl4]+ moved inside.
4) A series of high stability geminal dicationic magnetic ionic liquids [Cn(mim)2]X2/FeCl3 (n=1, 2, X=Br, Cl) and [Cn(mim)2]2[Dy(SCN)7] (n=2, 4, 6, 8, 10) were prepared and their thermal properties were investigated. By slow evaporation method single crystals of [C4(mim)2]2[Dy(SCN)7] and [C6(mim)2]2[Dy(SCN)7] were obtained and characterized, which indicated that geminal dicationic structure resulted in an absolute different coordination environment of Dy3+ from that of [C6mim]2[Dy(SCN)7H2O].
5) All the magnetic ionic liquids were characterized by SQUID, and influences of MILs structures on magnetic properties were investigated. Moreover, magnetic properties of MCNT were investigated, which indicated that the magnetic ionic liquid PMIL appeared an abvious transformation from paramagnetism to ferromagnetism, this might be due to the specialπ-πstructures of carbon nanotubes that could perfectly transfer electrons.
1)合成了[C4mim]Cl/FeCl3体系磁性离子液体,通过改变原料配比考察了磁性离子液体阴离子的存在形式。研究表明原料配比是导致不同阴离子构型的主要因素,不同的阴离子构型使磁性离子液体具有不同的物理性质和电化学性质。另外,通过对[C4mim]Br/FeCl3体系磁性离子液体的研究,证明了磁性离子液体阴离子络合物形成的过程中有离子相互交换现象,从而揭示了磁性离子液体的形成机理。
2)设计并合成了一种乙烯基咪唑类离子液体[Vmim]X(X=Cl、Br),通过对反应条件的优化,得到了较高的转化率和选择性,通过对合成的乙烯基功能化的咪唑类离子液体进行物性研究,发现乙烯基的引入使该离子液体的物理化学性质发生了很大改变。再者,以[Vmim]X为原料,合成了具有π-π共轭阳离子结构的磁性离子液体[Vmim]X/FeCl3,进一步,将[Vmim]FeCl4聚合制备出了聚合磁性离子液体PMIL。
3)以单壁碳纳米管SCNT为载体,以[Vmim]FeCl4为原料制备出了磁性碳纳米管MCNT,通过Raman、IR和SEM等测试手段对磁性碳纳米管的结构进行了表征,初步结果表明,聚合阳离子包裹在了碳纳米管表面,而磁性阴离子[FeCl4]-则进入了碳纳米管管内。
4)合成了一系列含金属铁离子的双咪唑类磁性离子液体:[C2(mim)2][FeCl4]2、[C4(mim)2][FeCl4]2、[C2(mim)2]Br2/FeCl3、[C4(mim)2]Br2/FeCl3,并对其热力学性质进行了研究。另外合成了一系列含镝的双咪唑磁性离子液体: [C2(mim)2]2[Dy(SCN)7]、[C4(mim)2]2[Dy(SCN)7]、[C6(mim)2]2[Dy(SCN)7]、[C8(mim)2]2[Dy(SCN)7]、[C10(mim)2]2[Dy(SCN)7]。培养出了[C4(mim)2]2[Dy(SCN)7]和[C6(mim)2]2[Dy(SCN)7]的单晶,并对其晶体结构进行了表征分析。结果表明,金属离子Dy3+在磁性离子液体中属于七配位,属首次报道。
5)对所合成的所有磁性离子液体进行了磁性表征,分析并总结了磁性离子液体阳离子结构、阴离子结构对磁性大小的影响。同时对负载型磁性离子液体的磁性进行了研究,初步结果表明,碳纳米管的特殊结构使磁性离子液体显示出了铁磁性。
A novel series of magnetic ionic liquids (MILs) have been synthesized by introducing complex ions of metals into ionic liquids. The physicochemical properties, such as density, viscosity, melting point and onset temperatures etc, were investigated. Through researches on magnetic properties of these MILs, several magnetic theories were founded. And magnetic carbon nanotubes (MCNT) as the combination of single-walled carbon nanotube and special-designed MIL were prepared. The major work and innovative results for this dissertation are as follows:
1) Two MILs systems [C4mim]Cl/FeCl3 and [C4mim]Br/FeCl3 were designed. And three magnetic ionic liquids, [C4mim]FeCl4, [C4mim]FeCl4+[C4mim]Fe2Cl7 and [C4mim]FeBrCl3 (main material in [C4mim]Br/FeCl3) were synthesized using standard method, which indicated that the molar ratio [C4mim]Cl/FeCl3 has crucial influence on the structure of complex ions, and there were ion exchange among complex ions.
2) A novel route was designed for the synthesis of vinyl-functionalized imidazolium-based ionic liquids, and the reaction conditions such as reaction temperature, selection of nucleophile etc were optimized. Moreover, magnetic ionic liquids [Vmim]FeCl4 and [Vmim]Br/FeCl3 havingπ-πconjunction structure were synthesized from vinyl-functionalized imidazolium-based ionic liquids, and PMIL was prepared by polymerization of [Vmim]FeCl4.
3) The single-walled carbon nanotubes functionalized by magnetic ionic liquid [Vmim]FeCl4 have been synthesized through the polymerization reaction of [Vmim]FeCl4 in methanol. And the structure of the functionalized single-walled carbon nanotubes was investigated by IR and Roman spectrum, which indicated that cation [Vmim]+ were supported on the surfaces of SCNTs, and anion [FeCl4]+ moved inside.
4) A series of high stability geminal dicationic magnetic ionic liquids [Cn(mim)2]X2/FeCl3 (n=1, 2, X=Br, Cl) and [Cn(mim)2]2[Dy(SCN)7] (n=2, 4, 6, 8, 10) were prepared and their thermal properties were investigated. By slow evaporation method single crystals of [C4(mim)2]2[Dy(SCN)7] and [C6(mim)2]2[Dy(SCN)7] were obtained and characterized, which indicated that geminal dicationic structure resulted in an absolute different coordination environment of Dy3+ from that of [C6mim]2[Dy(SCN)7H2O].
5) All the magnetic ionic liquids were characterized by SQUID, and influences of MILs structures on magnetic properties were investigated. Moreover, magnetic properties of MCNT were investigated, which indicated that the magnetic ionic liquid PMIL appeared an abvious transformation from paramagnetism to ferromagnetism, this might be due to the specialπ-πstructures of carbon nanotubes that could perfectly transfer electrons.
引文
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