1,3-二正丁基咪唑六氟磷酸盐离子液体的微波辅助合成与结构表征

以三甲基硅烷咪唑和1-溴代正丁烷作为原料,采用未经改装的家用微波炉在无溶剂条件下经季铵化反应合成了中间体溴化1,3-二正丁基咪唑([DnBIM][Br]),此步反应产率可以达到92%.再将第一步制得的中间体与六氟磷酸钾经复分解反应,得到1,3-二正丁基咪唑六氟磷酸盐离子液体([DnBIM][PF6]),收率为68%.提...     

微波法合成离子液体1-羟乙基-3-甲基咪唑四氟硼酸盐的研究

由1-甲基咪唑和2-氯乙醇通过微波法合成中间体氯化1-羟乙基-3-甲基咪唑,考察了原料配比、微波功率、加热方式和加热时间对中间体产率的影响。中间体经阴离子交换得到1-羟乙基-3-甲基咪唑四氟硼酸盐离子液体。通过测定中间体的相对分子量分析其纯度,目标产物的结构通过IR1、H-NMR表征。     

离子液体溴代1-丁基-3-甲基咪唑盐合成的红外光谱分析

本实验建立以红外光谱法,利用特征吸收频率处的红外吸收率测得合成离子液体1-丁基-3-甲基咪唑六氟磷酸盐的中间产物溴代1-丁基-3-甲基咪唑盐的含量,应用于探索1-丁基-3-甲基溴代咪唑盐合成的最佳反应条件,结果表明反应温度为65℃,时间50分钟时产物得率高。     

离子液体溴代1-丁基-3-甲基咪唑盐合成的红外光谱分析

本实验建立以红外光谱法,利用特征吸收频率处的红外吸收率测得合成离子液体1-丁基-3-甲基咪唑六氟磷酸盐的中间产物溴代1-丁基-3-甲基咪唑盐的含量,应用于探索1-丁基-3-甲基溴代咪唑盐合成的最佳反应条件,结果表明反应温度为65℃,时间50分钟时产物得率高.     

微波辐照合成固载咪唑鎓离子液体中间体:1-甲基-3-(3-三乙氧硅基丙基)咪唑氯鎓

采用家用微波炉,在无溶剂的状态下,以1-甲基咪唑和3-氯丙基三乙氧基硅烷为原料,合成了固载咪唑鎓离子液体中间体:1-甲基-3-(3-三乙氧硅基丙基)咪唑氯鎓。考察了微波辐照方式、辐照时间、微波功率以及投料比对产物收率的影响。与传统加热方法相比,微波辐照法不仅大大缩短了反应时间,而且提高了收率;为中间体1-甲基-3-(3-三乙氧硅基丙基)咪唑氯鎓离子液体的合成提供了一个快速、高效、环保绿色的方法。     

系列功能化离子液体的合成表征及其性质研究

通过两步法合成了含不同阴离子的系列含酯基官能团的咪唑类离子液体,用核磁共振、红外光谱、元素分析对其进行了结构表征,证明了该合成方法的可靠性;对功能化离子液体的基本物化性质及热稳定性等进行了全面研究,并选择了含有相同烷基的未功能化离子液体1-丁基-3-甲基咪唑四氟硼酸盐进行对比,发现酯基官能团的引入,使烷基咪唑类离子液体展现出不同的物化特性。所合成的含酯基功能化离子液体为进一步开展离子液体的各方面研究提供了全新的材料并打下了一定基础。     

烯丙基咪唑离子液体的合成与溶液性能

室温离子液体氯化1-烯丙基-3-甲基咪唑被合成,利用质谱和NMR对其结构进行了表征。该离子液体与水或乙醇的二相混合液在293.2K的粘度被测定并计算了该混合体系的过量粘度,建立了过量粘度与水或乙醇的摩尔分数的关系。另外,电导率随组分及温度的变化以及电导活化能也被测定,溶液的电导率随温度的升高及溶剂量的增加而增大。     

1-丁基-3-甲基咪唑碘对液体、凝胶电解质及染料敏化太阳电池性能的影响

采用季铵化反应成功合成了[Bmim]I，并制备了含有[Bmim]I、KI和I2的离子液体液体电解质和凝胶电解质。通过对比[Bmim]I浓度对液体和凝胶电解质电导率的影响及液体、凝胶电解质DSC的各项光电性能，发现液体电解质有更高的电导率，其组装的DSC的光电性能均高于凝胶电解质体系，通过对DSC稳定性的对比，发现离子液体凝胶电解质显示了更好的长期稳定性。     

1-丁基-3-甲基咪唑氯盐离子液体中副反应电沉积锌的机理

利用在离子液体中电合成Zn4O13C24H12(MOF-5)时的副反应沉积Zn2+,形成锌层,目前国内外尚无报道。应用循环伏安、交流阻抗、极化曲线等方法研究了在离子液体1-丁基-3-甲基咪唑氯盐体系中Zn2+的阴极电沉积过程、沉积机理。结果表明:Zn2+的沉积机理是一个不可逆的反应,且在一定范围内,其还原峰电流与扫描速度的平方根v1/2成明显的线性关系,该反应属于扩散控制;离子液体与有机配体的协同作用促进了反应电极上的电子转移;用极化曲线和电化学理论推导式计算出的该反应的阴、阳极表观传递系数、反应级数均为1,反应历程有3步,第2步为控制步骤。     

六氟磷酸盐吡啶离子液体的合成及电导率研究

采用二溴丁烷和3-甲基吡啶(物质的量之比为1.0∶2.2)为原料,以异丙醇为溶剂,温度控制在70～80℃,反应4～6h,得到吡啶溴盐离子液体。用吡啶溴盐与六氟磷酸盐发生置换反应,搅拌反应4h,得到六氟磷酸盐吡啶离子液体。测定了[C4(MPy)2][PF6]2离子液体在有机溶剂中的电导率;及离子液体在不同溶剂、不同浓度、不同温度下的电导率。结果表明:溶液的电导率随着温度升高而增大;随着浓度的增大而增大。相同温度、浓度下,乙腈的电导率最大;环丁砜的电导率最小。     

新型电解质材料[BMIM]ClO3离子液体的合成及其物化性能

以N-甲基咪唑为原料合成了室温离子液体1-丁基-3-甲基咪唑氯酸盐([BMIM]ClO3),用IR、NMR、DSC-TGA等手段对产物进行了表征,测定了相关物化性能,如密度、表面张力、黏度、电导率和电化学窗口等,并考察了该离子液体的溶剂性能。结果表明,该离子液体作为新型的电解质材料,具有低黏度、高电导率,密度、表面张力、黏度均随温度升高而减小,电导率随温度升高而增大,与温度符合Arrhenius方程。该离子液体与多数常规溶剂互溶,并对某些金属氧化物具有较高的溶解度,为离子液体在选矿、电解金属氧化物等方面的应用奠定了基础。     

Thermal Conductivities of [bmim][PF<Subscript>6</Subscript>], [hmim][PF<Subscript>6</Subscript>], and [omim][PF<Subscript>6</Subscript>] from 294 to 335 K at Pressures up to 20 MPa

Thermal conductivities are reported for a series of 1-alkyl-3-methylimidazolium hexafluorophosphates having butyl, hexyl, and octyl groups, which are expressed by [bmim][PF₆], [hmim][PF₆], and [omim][PF₆], respectively. The experimental method used was a transient short-hot-wire method. Since only a small amount of sample liquid is required, this method was found to be effective for the thermal-conductivity measurements of ionic liquids (ILs). The experimental temperatures ranged from 294 to 335 K at pressures up to 20 MPa. The values of the thermal conductivities of ILs at normal pressure are similar to those of benzene. It was found that an effect of the length of the alkyl chain on the thermal conductivities in ILs is negligible. From the data for the thermal conductivity and viscosity at 293.15 K and 0.1 MPa of ILs and normal alkanes, a simple correlation was developed based on the Mohanty theory. From comparisons between the thermal conductivities of ILs and those of organic liquids (n-hexane, benzene, and methanol), the temperature and pressure dependences of the thermal conductivity of ILs are relatively weak.     

Effect of ionic liquid dispersion on performance of a conducting polymer based Schottky diode

The effect of ionic liquid (IL) dispersion on the performance of Schottky diode fabricated with poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) has been investigated. Two kinds of ILs including 1-butyl-3-methylimidazolium hexafluorophosphate (BMIPF6, hydrophobic IL) and 1-butyl-3-methylimidazolium chloride (BMICL, hydrophilic IL) were dispersed to the PEDOT:PSS by mechanical stirring and sonication processes. Schottky diodes were fabricated with these mixtures. The forward current of Schottky diodes fabricated with PEDOT:PSS dispersed BMI PF6 (SD-BMIPF6)/BMICL (SD-BMICL) by mechanical stirring is slightly reduced compared with that of Schottky diodes fabricated with pristine PEDOT:PSS (SD-PEDOT). However, SD-BMIPF6 and SD-BMICL by sonication technique show higher forward current with respect to SD-PEDOT. Compared with SD-BMIPF6 and SD-BMICL, the forward current of SD-BMICL is much higher than that of SD-BMIPF6. Since the BMICL has hydrophilic nature, the enhancement of forward current might be due to the uniform dispersion of the BMICL on the PEDOT:PSS matrix.     

Direct extraction of double-stranded DNA into ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate and its quantification

Ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate (BmimPF6), as a green solvent, was successfully used for the direct extraction of dsDNA. The extraction efficiency and the distribution coefficient values indicated that trace amounts of DNA at the levels of <5 ng microL-1 facilitate quantitative fast extraction, while proteins and metal species do not interfere. A total of 30% of the DNA in ionic liquid at approximately 20 ng microL-1 was back extracted into aqueous phase in phosphate-citrate buffer with a single-stage extraction. The extraction is demonstrated to be endothermic with an enthalpy of 34.3 kJ moL-1. The extraction mechanisms were proposed and verified by 31P NMR and FT-IR spectra. Interactions between cationic 1-butyl-3-methylimidazolium (Bmim+) and P-O bonds of phosphate groups in the DNA strands take place both in the dissolved BmimPF6 in aqueous phase and at the interface of the two phases. This interaction consequently led to the transformation of DNA conformations, along with a reduction of ethidium resonance light scattering at 510 nm, and a procedure for DNA quantification in ionic liquid was developed based on this observation.     

Facile and green synthesis of ZnO nanostructures in a room-temperature ionic liquid 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide

Pure hexagonal phase of ZnO nanoparticles have been successfully synthesized via microwave assisted decomposition of zinc acetate precursor in a green solvent, the ionic liquid, 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide in a very short time scale. The ZnO nanoparticles were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction.     

离子液体的设计合成

离子液体具有非常好的物理、化学性质 ,正引起人们越来越多的重视。作为一种可设计溶剂 ,可以调整离子液体的结构 ,设计出一些有独特功能的任务适应性离子液体。本文就目前发展的一些特殊用途的离子液体合成设计进行了介绍 ,为人们更好的应用与设计提供参考。     

室温离子液体在材料合成中的应用

室温离子液体的物理和化学性质相对稳定,具有结构可调的特性.作为一种新功能材料广泛用于材料合成领域.根据离子液体在材料合成中的不同作用,本文从离子液体作为反应溶剂、模板剂、电解液、以及同时作为溶剂和模板剂这4个方面介绍了其在材料合成中的应用研究进展.