离子液体用于己内酰胺萃取和氧氟沙星拆分的研究
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摘要
离子液体对许多有机物、无机物具有良好的溶解性能,蒸汽压较低,不易挥发,在室温下可呈现液态,具有广阔的应用前景。在有机物分离方面,离子液体已用于萃取水中苯、苯酚等芳香类物质,但是在大宗非芳香族化学品和高附加值化学品分离方面,离子液体的萃取应用研究还处于起步阶段。本文以提高萃取分配系数、对映体分离的对映体选择性系数,降低分离过程中萃取剂用量和能耗为目的,利用离子液体为萃取剂分离大宗非芳香族化学品己内酰胺和高附加值化学品氧氟沙星消旋体。
主要研究内容如下：
1.选择离子液体1-丁基-3-甲基咪唑六氟磷酸盐、1-己基-3-甲基咪唑六氟磷酸盐、1-辛基-3-甲基咪唑六氟磷酸盐、1-丁基-3-甲基咪唑双三氟甲烷磺酰亚胺盐和1-己基-3-甲基咪唑四氟硼酸盐分别萃取水中己内酰胺,测定了不同条件下己内酰胺的分配系数,研究了离子液体的结构、萃取温度及硫酸铵浓度对己内酰胺分配系数的影响。采用NRTL方程关联了己内酰胺在离子液体-水体系中的液液平衡特性。
2.利用L-二苯甲酰酒石酸和手性离子液体1-乙基-3-甲基咪唑L-酒石酸在双相识别萃取拆分体系中共同拆分氧氟沙星消旋体。研究了L-二苯甲酰酒石酸浓度、手性离子液体浓度、氧氟沙星消旋体浓度、水相pH值和萃取拆分温度等因素对拆分效果的影响,在适当的工艺条件下氧氟沙星对映体的对映体选择性系数最大可达到3.6,明显优于文献中使用混合溶剂L-对甲基二苯甲酰酒石酸和L-二苯甲酰酒石酸时的萃取拆分效果。
3.为减小离子液体黏度对萃取的影响,采用微管挤出法和溶剂挥发一步法制备了包裹离子液体1-丁基-3-甲基咪唑六氟磷酸盐的微胶囊高分子颗粒。研究了不同壳材料、微管管径、离子液体在溶剂中的浓度、明胶在水相中的浓度和搅拌速度等因素对微胶囊形状、粒径以及包裹率的影响。
4.利用溶剂挥发一步法制得的包裹离子液体1-丁基-3-甲基咪唑六氟磷酸盐的聚砜微胶囊萃取吸附水中己内酰胺。考察了壳材料聚砜和芯材料离子液体对己内酰胺的萃取吸附效果,研究了硫酸铵浓度、温度对微胶囊萃取吸附效果的影响,以及微胶囊萃取前后的包裹率变化。采用吸附动力学模型和等温吸附模型对实验数据进行了关联。
Most organic and inorganic substances have good solubilities in ionic liquids. Since ionic liquids have the properties of low vapor pressure as well as volatility and usually exist as liquid form at room temperature, they have already been used in extracting aromatic organics, such as benzene, phenol, from water. Studies of using ionic liquids in separating nonaromatic organics or substances with high value are little performed at present. In this study, ionic liquids are used to separate caprolactam and ofloxacin enantiomers, respectively, to increase the distribution ratio, enantioselectivity, and decrease the cost of energy and extractant during the extraction process.
The main contents are as follows:
1.1-butyl-3-methy-limidazolium hexa-fluorophosphate,1-hexyl-3-methy-limidazolium hexa-fluorophosphate,1-octyl-3-methy-limidazolium hexa-fluorophosphate,1-butyl-3-methy-limidazolium bis[(trifluoromethyl)sulfonyl]imide and1-hexyl-3-methy-limidazolium tetrafluoroborate have been used to extract caprolactam from water, respectively. The distribution ratios of caprolactam under different operating conditions have been measured. The effects of structure of ionic liquids, extraction temperature and concentration of ammonium sulfate solution have been investigated. A model has been developed to correlate the obtained experimental data.
2. Dibenzoyl-tartaric and chiral ionic liquid1-ethyl-3-methylimidazolium L-tartrate acid have been used as chiral selectors to separate ofloxacin enantiomers. The effects of concentration of [Emim][Ta] in water, concentration of DBTA in decanol, concentration of ofloxacin enantiomers, pH in aqueous phase and temperature have been investigated, respectively. Under certain operating condition, the enantioselectivity can reach3.6, which is larger than the value when using co-extrants.
3. In order to decrease the negative effect of viscosity of ionic liquids in extraction, ionic liquids1-butyl-3-methylimidazolium hexafluorophosphate have been encapsulated into polymer to form microcapsules using microtube extrusion and solvent evaporation methods. The effects of shell material, diameter of microtube, concentration of ionic liquid in oil phase, concentration of gelatin in aqueous phase and stirring speed have been investigated.
4. Polysulfone microcapsules containing ionic liquid1-butyl-3-methylimidazolium hexafluorophosphate as extractant have been successfully prepared using solvent evaporation method and used in removing caprolactam from water. The extraction performances of shell material polysulfone and ionic liquid have been studied, respectively. The effects of ammonium sulfate concentration and temperature have been investigated. The kinetic model and adsorption isotherm model have been used to correlate the experiment data.
主要研究内容如下：
1.选择离子液体1-丁基-3-甲基咪唑六氟磷酸盐、1-己基-3-甲基咪唑六氟磷酸盐、1-辛基-3-甲基咪唑六氟磷酸盐、1-丁基-3-甲基咪唑双三氟甲烷磺酰亚胺盐和1-己基-3-甲基咪唑四氟硼酸盐分别萃取水中己内酰胺,测定了不同条件下己内酰胺的分配系数,研究了离子液体的结构、萃取温度及硫酸铵浓度对己内酰胺分配系数的影响。采用NRTL方程关联了己内酰胺在离子液体-水体系中的液液平衡特性。
2.利用L-二苯甲酰酒石酸和手性离子液体1-乙基-3-甲基咪唑L-酒石酸在双相识别萃取拆分体系中共同拆分氧氟沙星消旋体。研究了L-二苯甲酰酒石酸浓度、手性离子液体浓度、氧氟沙星消旋体浓度、水相pH值和萃取拆分温度等因素对拆分效果的影响,在适当的工艺条件下氧氟沙星对映体的对映体选择性系数最大可达到3.6,明显优于文献中使用混合溶剂L-对甲基二苯甲酰酒石酸和L-二苯甲酰酒石酸时的萃取拆分效果。
3.为减小离子液体黏度对萃取的影响,采用微管挤出法和溶剂挥发一步法制备了包裹离子液体1-丁基-3-甲基咪唑六氟磷酸盐的微胶囊高分子颗粒。研究了不同壳材料、微管管径、离子液体在溶剂中的浓度、明胶在水相中的浓度和搅拌速度等因素对微胶囊形状、粒径以及包裹率的影响。
4.利用溶剂挥发一步法制得的包裹离子液体1-丁基-3-甲基咪唑六氟磷酸盐的聚砜微胶囊萃取吸附水中己内酰胺。考察了壳材料聚砜和芯材料离子液体对己内酰胺的萃取吸附效果,研究了硫酸铵浓度、温度对微胶囊萃取吸附效果的影响,以及微胶囊萃取前后的包裹率变化。采用吸附动力学模型和等温吸附模型对实验数据进行了关联。
Most organic and inorganic substances have good solubilities in ionic liquids. Since ionic liquids have the properties of low vapor pressure as well as volatility and usually exist as liquid form at room temperature, they have already been used in extracting aromatic organics, such as benzene, phenol, from water. Studies of using ionic liquids in separating nonaromatic organics or substances with high value are little performed at present. In this study, ionic liquids are used to separate caprolactam and ofloxacin enantiomers, respectively, to increase the distribution ratio, enantioselectivity, and decrease the cost of energy and extractant during the extraction process.
The main contents are as follows:
1.1-butyl-3-methy-limidazolium hexa-fluorophosphate,1-hexyl-3-methy-limidazolium hexa-fluorophosphate,1-octyl-3-methy-limidazolium hexa-fluorophosphate,1-butyl-3-methy-limidazolium bis[(trifluoromethyl)sulfonyl]imide and1-hexyl-3-methy-limidazolium tetrafluoroborate have been used to extract caprolactam from water, respectively. The distribution ratios of caprolactam under different operating conditions have been measured. The effects of structure of ionic liquids, extraction temperature and concentration of ammonium sulfate solution have been investigated. A model has been developed to correlate the obtained experimental data.
2. Dibenzoyl-tartaric and chiral ionic liquid1-ethyl-3-methylimidazolium L-tartrate acid have been used as chiral selectors to separate ofloxacin enantiomers. The effects of concentration of [Emim][Ta] in water, concentration of DBTA in decanol, concentration of ofloxacin enantiomers, pH in aqueous phase and temperature have been investigated, respectively. Under certain operating condition, the enantioselectivity can reach3.6, which is larger than the value when using co-extrants.
3. In order to decrease the negative effect of viscosity of ionic liquids in extraction, ionic liquids1-butyl-3-methylimidazolium hexafluorophosphate have been encapsulated into polymer to form microcapsules using microtube extrusion and solvent evaporation methods. The effects of shell material, diameter of microtube, concentration of ionic liquid in oil phase, concentration of gelatin in aqueous phase and stirring speed have been investigated.
4. Polysulfone microcapsules containing ionic liquid1-butyl-3-methylimidazolium hexafluorophosphate as extractant have been successfully prepared using solvent evaporation method and used in removing caprolactam from water. The extraction performances of shell material polysulfone and ionic liquid have been studied, respectively. The effects of ammonium sulfate concentration and temperature have been investigated. The kinetic model and adsorption isotherm model have been used to correlate the experiment data.
引文
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