含离子液体微乳液的构建和性质研究
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摘要
离子液体以其低挥发性、高热稳定性和可设计性等优点成为一种极具吸引力的新型溶剂。将离子液体引入到微乳液,一方面有助于改善微乳液的性质、扩大其应用范围,另一方面也有利于拓展离子液体的应用领域。本文在现有研究基础上,进一步考察了以离子液体为极性相的非水微乳液的性质,构建了以离子液体和极性溶剂为混合极性相的非水微乳液体系,研究了离子液体对传统含水微乳液体系性质的影响。论文主要内容如下：
1.研究了以离子液体为极性相的非水微乳液的性质。首先,考察了离子液体在叔辛基酚聚氧乙烯醚(TX系列)表面活性剂微乳液体系中的增溶量。结果表明,离子液体阴离子氢键碱性越强、阳离子链长越短、体系温度越高越有利于离子液体增溶。在此基础上,选取离子液体1-乙基-3-甲基咪唑醋酸盐(emimCH3COO),研究了25℃下emimCH3COO、表面活性剂TX-45以及环已烷三元体系的相行为。用电导法划分出emimCH3COO/环已烷(IL/O)、双连续以及环已烷/emimCH3COO (O/IL)三种微乳液的微观结构区域。粒径实验证实了离子液体微乳液的形成。通过紫外-可见光谱实验,以甲基橙(MO)和亚甲基蓝(MB)为探针,研究了IL/O微乳液的微观极性。研究结果表明离子液体微乳液的微观极性随emimCH3COO含量的增加而增大,但当离子液体池形成以后,微乳液极性保持不变。另外,光谱实验也表明IL/O微乳液可以增溶金属盐COCl2、 CuCl2和生物分子核黄素。对IL/O微乳液的电导渗透行为进行研究,发现体系活化能较低,不出现温度渗透现象。但体系具有体积渗透现象,加入金属盐CuCl2和聚合物聚乙二醇400有利于体积渗透。
2.构建了以离子液体和极性溶剂为混合极性相的非水微乳液,拓展了离子液体的选择范围。研究了25℃下离子液体bmimCl与极性溶剂(甲酰胺或乙二醇)、表面活性剂TX-100以及环已烷体系的相行为。通过电导研究发现该类微乳液也具有三种不同的微观结构区域。以bmimCl和极性溶剂为混合内相的微乳液的粒径与混合内相和表面活性剂的摩尔比呈线性关系,证实了这类离子液体微乳液的形成。红外光谱实验表明,表面活性剂TX-100与混合内相间存在较强的氢键作用,该作用有利于微乳液的形成。这类微乳液的微观极性随混合内相含量的增加而持续增大,这与单以离子液体为内相的微乳液不同。微乳液极性只与混合内相和表面活性剂的摩尔比有关,与表面活性剂的浓度无关。光谱实验表明金属盐CoCl2和生物分子核黄素都能增溶到微乳液的混合内相中。
3.考察了离子液体对非离子型表面活性剂形成的含水微乳液性质的影响。研究了25℃下两种离子液体bmimBF4和bmimCl对TX-100形成的含水微乳液极性、电导、粘度和粒径等性质的影响。研究结果表明,离子液体使微乳液极性增大,同时使微乳液极性达到最大所需的水量减少。微乳液电导率随水含量的增加逐渐增加并出现体积渗透现象,渗透水量随离子液体浓度增加而减小。离子液体的存在会增加微乳液的粘度。bmimBF4对微乳液以上性质的影响均大于bmimCl.粒径的数据表明,bmimBF4基本增溶到了微乳液内核,而bmimCl只有部分增溶到微乳液中,以此解释两种离子液体对微乳液性质影响的差异。
4.研究了离子液体对阴离子表面活性剂AOT形成的含水微乳液电导渗透行为和增溶水量的影响。AOT含水微乳液具有明显的温度渗透现象,微乳液渗透温度(Tp)随离子液体浓度的增加而增大。离子液体阳离子链长、取代数和末端基团对渗透温度影响较大,而阴离子的影响较小。微乳液粒径和粘度均随离子液体的加入而降低。体系粒径、渗透温度和粘度具有很好的相关性,粒径越小,其粘度也越小,渗透温度则越高。离子液体推迟了微乳液的体积渗透,提高了微乳液的渗透体积分率(Φp)。Φp随离子液体浓度的增加而增大。但较高的离子液体浓度下,由于微乳液增溶水量较小,无法观察到渗透现象。离子液体链长对Φp影响较大。微乳液增溶水量随离子液体浓度的增加先增大后减小,出现最大值。离子液体链长越长,达到最大增溶水量所需离子液体含量越低。同时,在较低离子液体浓度下,增溶水量随离子液体链长的增加而增大。
Ionic liquids (ILs) are receiving great attention as a class of neoteric solvents because of their special physical and chemical properties, such as low volatility. high thermal stability and designable property. In recent years, the microemulsions containing ILs have become an interesting topic. It revealed that ILs can act as effective additives to modify the properties of microemulsions, which expands the utilization of microemulsions. Meanwhile, the application of ILs is also expanded. Based on the previous studies by other groups, the properties of nonaqueous microemulsions, which use ILs as polar phase, was investigated in this dissertation. Also, using the mixture of an IL and nonaqueous polar solvents instead of pure IL to form ionic liquid microemulsions had been described. Additionally, the effect of ILs on the traditional water-based microemulsions was investigated. The contents of this dissertation are as follows:
1. The properties of IL microemulsions were investigated in detail. Firstly, the solubilizations of ILs in polyoxyethylene tert-octylphenyl ether surfactants systems were studied. It indicated that the IL which had higher hydrogen-bond basicity, longer alkyl chain length of cation, possessed a higher solubilization. On the basis of these results, the phase behavior of the1-ethyl-3-methylimidazolium acetate (emimCHbCOO), polyoxyethylene tert-octylphenyl ether (TX-45) and cyclohexane system at25℃was studied. And, microregions of emimCH3COO-in-cyclohexane (IL/O), bicontinuous and cyclohexane-in-emimCH3COO (O/IL) were identified by electrical conductivity measurements. The experiments of droplet size revealed the formation of the IL microemulsions. The micropolarities of the emimCH3COO-in-cyclohexane microemulsions were investigated by the UV-vis spectroscopy using methyl orange (MO) and methylene blue (MB) as absorption probes. The results showed that, with the addition of IL, the polarity of the microemulsions was increased, but it didn't change any more when the IL pools began to form. Moreover, the study of spectroscopy also indicated that biological molecule riboflavin and metal salts such as CoCl2, CuCl2could be solubilized into the microemulsions droplets. Conductivity measurements indicated that the microemulsions didn't have temperature-induced percolation, which showed very low activation energy. However, the systems possessed volume-induced percolation, which could be assisted by the metal salt CuCl2and polyethylene glycol400.
2. The formation of nonaqueous microemulsions containing the mixture of IL and polar solvent as the polar phase was studied. The phase behavior of the bmimCl, polar solvent (formamide or ethylene glycol), polyoxyethylene tert-octylphenyl ether (TX-100) and cyclohexane system at25℃was investigated. Electrical conductivity measurement was used to identify the three microregions of the nonaqueous microemulsions. Dynamic light scattering (DLS) studies revealed that the droplet size of reverse microemulsions of bmimCl-polar solvent in cyclohexane increased linear with the increase of the polar phase-to-TX-100molar ratio, which confirmed the formation of reverse microemulsions. FTIR spectra showed that there were hydrogen-bond interactions between the mixed polar phase and the surfactant. The interactions might be the driving force for solubilizing polar phase into the microemulsions. The polarity of these microemulsions was increased with the increasing amount of polar phase, which was different from the microemulsions containing IL as the only polar phase. The polarity was dependent of the polar phase-to-TX-100molar ratio (R), and nearly independent of the surfactant concentration. UV-vis studies indicated that the nonaqueous reverse microemulsions could dissolve metal salt CoCl2and biological molecule riboflavin.
3. A study was carried out concerning the effects of ILs (bmimBF4and bmimCl) on the properties of nonionic surfactant-based H2O/TX-100/hexanol/cyclohexane microemulsions at25℃. Several properties of microemulsions, such as polarity, conductivity, viscosity and droplet size, were investigated. With the addition of IL, the polarity of the microemulsions was increased, and the water needed to form water pool was decreased. Conductivity results revealed that the onset water content of electrical percolation was decreased with the presence of IL and continued to decrease as the amount of IL increased. The viscosity of microemulsions was increased with the increasing amount of IL. The influence of bmimBF4on the properties of microemulsions was greater than bmimCl. The measurement of droplet sizes of microemulsions indicated that the bmimBF4was almost all solubilized into the polar core of microemulsions, but the bmimCl wasn't. This explained the difference of the two IL's effect on the properties of microemulsions.
4. The effects of ILs on temperature-induced and volume-induced percolation as well as water solubilization capacity of anionic surfactant AOT-based microemulsions were investigated. The temperature-induced percolation phenomena of microemulsions were delayed with the addition of IL. And the percolation temperature threshold (Tp) of microemulsions was increased with an increase of the IL's concentration. The alkyl chain length, hydrogen-bond acidity and end group of cation had great effect on the Tp. However. Tp was slightly affected by the ILs anions. The viscosity and droplet size of microemulsions were all decreased when addition of ILs and the observed decrease correlated roughly with an increase in Tp. The volume-induced percolation phenomena of microemulsions were also delayed by the ILs. The volume percolation threshold (Φp) was increased in the presence of IL, and increased with the increase of the concentration of IL at low IL's concentration, whereas no percolation phenomena could be observed at high IL's concentration. The Φp value was increased with increasing chain length of ILs under the same conditions. Additionally. the water solubilization capacity was enhanced as function of IL concentration at low concentration of IL. reached a maximum and decreased for high IL's concentration. For the microemulsions, the water solubilization capacity was increased with the increase of chain length of ILs at low IL's concentration.
1.研究了以离子液体为极性相的非水微乳液的性质。首先,考察了离子液体在叔辛基酚聚氧乙烯醚(TX系列)表面活性剂微乳液体系中的增溶量。结果表明,离子液体阴离子氢键碱性越强、阳离子链长越短、体系温度越高越有利于离子液体增溶。在此基础上,选取离子液体1-乙基-3-甲基咪唑醋酸盐(emimCH3COO),研究了25℃下emimCH3COO、表面活性剂TX-45以及环已烷三元体系的相行为。用电导法划分出emimCH3COO/环已烷(IL/O)、双连续以及环已烷/emimCH3COO (O/IL)三种微乳液的微观结构区域。粒径实验证实了离子液体微乳液的形成。通过紫外-可见光谱实验,以甲基橙(MO)和亚甲基蓝(MB)为探针,研究了IL/O微乳液的微观极性。研究结果表明离子液体微乳液的微观极性随emimCH3COO含量的增加而增大,但当离子液体池形成以后,微乳液极性保持不变。另外,光谱实验也表明IL/O微乳液可以增溶金属盐COCl2、 CuCl2和生物分子核黄素。对IL/O微乳液的电导渗透行为进行研究,发现体系活化能较低,不出现温度渗透现象。但体系具有体积渗透现象,加入金属盐CuCl2和聚合物聚乙二醇400有利于体积渗透。
2.构建了以离子液体和极性溶剂为混合极性相的非水微乳液,拓展了离子液体的选择范围。研究了25℃下离子液体bmimCl与极性溶剂(甲酰胺或乙二醇)、表面活性剂TX-100以及环已烷体系的相行为。通过电导研究发现该类微乳液也具有三种不同的微观结构区域。以bmimCl和极性溶剂为混合内相的微乳液的粒径与混合内相和表面活性剂的摩尔比呈线性关系,证实了这类离子液体微乳液的形成。红外光谱实验表明,表面活性剂TX-100与混合内相间存在较强的氢键作用,该作用有利于微乳液的形成。这类微乳液的微观极性随混合内相含量的增加而持续增大,这与单以离子液体为内相的微乳液不同。微乳液极性只与混合内相和表面活性剂的摩尔比有关,与表面活性剂的浓度无关。光谱实验表明金属盐CoCl2和生物分子核黄素都能增溶到微乳液的混合内相中。
3.考察了离子液体对非离子型表面活性剂形成的含水微乳液性质的影响。研究了25℃下两种离子液体bmimBF4和bmimCl对TX-100形成的含水微乳液极性、电导、粘度和粒径等性质的影响。研究结果表明,离子液体使微乳液极性增大,同时使微乳液极性达到最大所需的水量减少。微乳液电导率随水含量的增加逐渐增加并出现体积渗透现象,渗透水量随离子液体浓度增加而减小。离子液体的存在会增加微乳液的粘度。bmimBF4对微乳液以上性质的影响均大于bmimCl.粒径的数据表明,bmimBF4基本增溶到了微乳液内核,而bmimCl只有部分增溶到微乳液中,以此解释两种离子液体对微乳液性质影响的差异。
4.研究了离子液体对阴离子表面活性剂AOT形成的含水微乳液电导渗透行为和增溶水量的影响。AOT含水微乳液具有明显的温度渗透现象,微乳液渗透温度(Tp)随离子液体浓度的增加而增大。离子液体阳离子链长、取代数和末端基团对渗透温度影响较大,而阴离子的影响较小。微乳液粒径和粘度均随离子液体的加入而降低。体系粒径、渗透温度和粘度具有很好的相关性,粒径越小,其粘度也越小,渗透温度则越高。离子液体推迟了微乳液的体积渗透,提高了微乳液的渗透体积分率(Φp)。Φp随离子液体浓度的增加而增大。但较高的离子液体浓度下,由于微乳液增溶水量较小,无法观察到渗透现象。离子液体链长对Φp影响较大。微乳液增溶水量随离子液体浓度的增加先增大后减小,出现最大值。离子液体链长越长,达到最大增溶水量所需离子液体含量越低。同时,在较低离子液体浓度下,增溶水量随离子液体链长的增加而增大。
Ionic liquids (ILs) are receiving great attention as a class of neoteric solvents because of their special physical and chemical properties, such as low volatility. high thermal stability and designable property. In recent years, the microemulsions containing ILs have become an interesting topic. It revealed that ILs can act as effective additives to modify the properties of microemulsions, which expands the utilization of microemulsions. Meanwhile, the application of ILs is also expanded. Based on the previous studies by other groups, the properties of nonaqueous microemulsions, which use ILs as polar phase, was investigated in this dissertation. Also, using the mixture of an IL and nonaqueous polar solvents instead of pure IL to form ionic liquid microemulsions had been described. Additionally, the effect of ILs on the traditional water-based microemulsions was investigated. The contents of this dissertation are as follows:
1. The properties of IL microemulsions were investigated in detail. Firstly, the solubilizations of ILs in polyoxyethylene tert-octylphenyl ether surfactants systems were studied. It indicated that the IL which had higher hydrogen-bond basicity, longer alkyl chain length of cation, possessed a higher solubilization. On the basis of these results, the phase behavior of the1-ethyl-3-methylimidazolium acetate (emimCHbCOO), polyoxyethylene tert-octylphenyl ether (TX-45) and cyclohexane system at25℃was studied. And, microregions of emimCH3COO-in-cyclohexane (IL/O), bicontinuous and cyclohexane-in-emimCH3COO (O/IL) were identified by electrical conductivity measurements. The experiments of droplet size revealed the formation of the IL microemulsions. The micropolarities of the emimCH3COO-in-cyclohexane microemulsions were investigated by the UV-vis spectroscopy using methyl orange (MO) and methylene blue (MB) as absorption probes. The results showed that, with the addition of IL, the polarity of the microemulsions was increased, but it didn't change any more when the IL pools began to form. Moreover, the study of spectroscopy also indicated that biological molecule riboflavin and metal salts such as CoCl2, CuCl2could be solubilized into the microemulsions droplets. Conductivity measurements indicated that the microemulsions didn't have temperature-induced percolation, which showed very low activation energy. However, the systems possessed volume-induced percolation, which could be assisted by the metal salt CuCl2and polyethylene glycol400.
2. The formation of nonaqueous microemulsions containing the mixture of IL and polar solvent as the polar phase was studied. The phase behavior of the bmimCl, polar solvent (formamide or ethylene glycol), polyoxyethylene tert-octylphenyl ether (TX-100) and cyclohexane system at25℃was investigated. Electrical conductivity measurement was used to identify the three microregions of the nonaqueous microemulsions. Dynamic light scattering (DLS) studies revealed that the droplet size of reverse microemulsions of bmimCl-polar solvent in cyclohexane increased linear with the increase of the polar phase-to-TX-100molar ratio, which confirmed the formation of reverse microemulsions. FTIR spectra showed that there were hydrogen-bond interactions between the mixed polar phase and the surfactant. The interactions might be the driving force for solubilizing polar phase into the microemulsions. The polarity of these microemulsions was increased with the increasing amount of polar phase, which was different from the microemulsions containing IL as the only polar phase. The polarity was dependent of the polar phase-to-TX-100molar ratio (R), and nearly independent of the surfactant concentration. UV-vis studies indicated that the nonaqueous reverse microemulsions could dissolve metal salt CoCl2and biological molecule riboflavin.
3. A study was carried out concerning the effects of ILs (bmimBF4and bmimCl) on the properties of nonionic surfactant-based H2O/TX-100/hexanol/cyclohexane microemulsions at25℃. Several properties of microemulsions, such as polarity, conductivity, viscosity and droplet size, were investigated. With the addition of IL, the polarity of the microemulsions was increased, and the water needed to form water pool was decreased. Conductivity results revealed that the onset water content of electrical percolation was decreased with the presence of IL and continued to decrease as the amount of IL increased. The viscosity of microemulsions was increased with the increasing amount of IL. The influence of bmimBF4on the properties of microemulsions was greater than bmimCl. The measurement of droplet sizes of microemulsions indicated that the bmimBF4was almost all solubilized into the polar core of microemulsions, but the bmimCl wasn't. This explained the difference of the two IL's effect on the properties of microemulsions.
4. The effects of ILs on temperature-induced and volume-induced percolation as well as water solubilization capacity of anionic surfactant AOT-based microemulsions were investigated. The temperature-induced percolation phenomena of microemulsions were delayed with the addition of IL. And the percolation temperature threshold (Tp) of microemulsions was increased with an increase of the IL's concentration. The alkyl chain length, hydrogen-bond acidity and end group of cation had great effect on the Tp. However. Tp was slightly affected by the ILs anions. The viscosity and droplet size of microemulsions were all decreased when addition of ILs and the observed decrease correlated roughly with an increase in Tp. The volume-induced percolation phenomena of microemulsions were also delayed by the ILs. The volume percolation threshold (Φp) was increased in the presence of IL, and increased with the increase of the concentration of IL at low IL's concentration, whereas no percolation phenomena could be observed at high IL's concentration. The Φp value was increased with increasing chain length of ILs under the same conditions. Additionally. the water solubilization capacity was enhanced as function of IL concentration at low concentration of IL. reached a maximum and decreased for high IL's concentration. For the microemulsions, the water solubilization capacity was increased with the increase of chain length of ILs at low IL's concentration.
引文
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