摘要
室温离子液体被公认为绿色化工领域的新一代介质和“软”功能材料,有望代替传统重污染介质并广泛改变传统的化学工艺。近年来的研究表明,离子液体作为“促沉淀剂”在电解质结晶分离、清洁溶剂等方面已表现出潜在的应用前景,但其研究还处于起步阶段。传统的有机溶剂作为分离介质,例如有机溶剂捕集天然气中的硫,存在一定的缺陷。离子液体能否调控介质的性质继而为开发新的分离介质和分离工艺提供新思路也值得我们关注。本论文围绕离子液体调控介质的溶解性能等开展了如下研究工作：
1、利用激光浊点法测定了常压、不同温度下氯化物MCl(M=Na,K)在不同浓度的离子液体1-甲基-3-丁基咪唑氯化盐([Bmim]Cl)水溶液中的溶解度,以及溴化物MBr(M=Na,K)分别在不同浓度离子液体1-甲基-3-丁基咪唑溴化盐([Bmim]Br)水溶液中的溶解度,考察了温度和离子液体浓度对溶解度的影响,并采用Pitzer混合电解质溶液模型对实验数据进行了关联,得到了新的离子间相互作用参数、电解质的平均活度系数和溶剂的渗透系数。实验发现,在溶剂水中添加离子液体会降低无机盐的溶解度,离子液体表现出强烈的盐析效应,但对钾盐的盐析作用要高于对钠盐的盐析作用。Pitzer混合电解质溶液模型能满意关联溶解度数据,预测的NaCl(Br)-KCl(Br)-[Bmim]Cl(Br)-H2O四元相图显示,离子液体能改变钾盐和钠盐的结晶区,预示着可通过离子液体调控无机盐的结晶。
2、在常压和293.15-343.15K温度范围内,利用激光浊点法分别测定了氯化钾(KCl)和硫酸钾(K2SO4)在离子液体1-甲基-3-丁基咪唑四氟硼酸盐([Bmim][BF4])(?)水混合溶剂中的溶解度,考察了温度和溶剂配比对溶解度的影响,分别绘制出不同温度下KCl-[Bmim][BF4]-H2O和K2SO4-[Bmim][BF4]-H2O四元混合系统固-液平衡相图。结果表明,在混合体系中发生了复分解反应。利用得到的溶解度实验数据计算了两种钾盐从纯水中迁移至混合溶剂中的标准迁移热力学函数。钾盐从纯水中到离子液体混合溶剂中的标准迁移自由能计算结果说明,离子液体浓度越大,迁移能越大,越不利于钾盐的溶解。
3、研究了离子液体的加入对水盐系统热力学性质的影响。测定了常压下不同温度(T=298.15-328.15K)、不同组成的MX+[Bmim]X+H2O三元系统的密度、粘度和折光率。结果表明,相同温度下,MX+[Bmim]X+H2O系统的密度、粘度和折光率都会随离子液体质量分数和无机盐的质量摩尔浓度的增大而增加。在定组成下,系统的密度、折光率和粘度会随温度的升高而逐渐降低。采用经验模型关联系统的密度、粘度和折光率,相关系数R2均在0.98以上。在此基础上,计算了MX在[Bmim]X+水混合溶液中的表观摩尔体积,无限稀释农观摩尔体积,以及MX从纯水中迁移到离子液体水溶液中的标准迁移偏摩尔体积。结果表明,随着无机盐的质量摩尔浓度的增加,其表观摩尔体积也随之增大,但在离子强度较大的范围内,两者并未表现出良好的线性关系。定组成下,溶液中MX的VΦ0。和△trVΦ0都随[Bmim]Br浓度增大而增大
4、利用激光浊点法测定了常压、不同温度下(293.15-353.15K)硫磺在甲苯、氯苯、对二甲苯、环己烷和正辛烷,以及不同咪唑类离子液体[Cnmim][PF6]和[Cnmim][BF4](n=4,6)与甲苯混合溶剂中的溶解度。实验结果表明,在所选有机溶剂中,硫在甲苯溶剂中的溶解度最大,而离子液体的加入会显著降低硫磺的溶解度。离子液体阴、阳离子的种类,浓度以及温度都会影响硫磺在混合溶剂中的溶解度。在此基础上,采用不同模型关联了实验数据,得到了硫磺从甲苯中迁移到混合溶剂中的迁移自由能、迁移熵和迁移焓。计算发现,离子液体对硫磺溶解度的影响程度要比温度大。在较低温度下,硫磺的溶解为熵驱动过程,较高温度范围为焓驱动过程。
Room temperature ionic liquids (RTILs) considered as novel benign solvent and "soft" functional material in green chemical industry, are expected to replace the traditional solvent that causes a heavy pollution to the environment, and to innovate the traditional chemical techniques. Recently, many researches demonstrated that IL as "drowning-out agent" would have a potential application in the fileds of electrolyte crystallization process and solution separation. It is pity that its rearch and application is still at a beginning step. The traditional organic solvent as a medium of separation in the current chemical engineering industry exists some critical defects, in particular the organic solvent at the industry of the extraction and capture of the sulfur from exhausted gases. Thus, a new thought about the use of IL to mediate the property of solution and then to develop a new separation medium and separation process, comes up and deserves us to focus on it. In this thesis, we have done some basic experimental work and theoretical studies on the solid-liquid equilibrium, thermodynamic properties and thermodynamic models of the mixture system with ionic liquid. The highlights of this thesis are following:
1. Solubility of potassium chloride (KCl) and sodium chloride (NaCI) in ionic liquid1-butyl-3-methylimidazolium chloride ([Bmim]Cl) aqueous solution and solubility of bromide MBr (M=Na,K) in1-Butyl-3-methylimidazolium bromine [Bmim]Br aqueous solutions were determined by cloud-point method through using the laser beam scattering instrument at different temperatures and standard atmospheric pressures. The effect of temperature and ionic liquid concentration on the solubility of salt was studied. We observed that ionic liquid has "salting-out effect" on salt. The solubility data in our experiments was correlated and calculated with the modified Pitzer electrolyte model. Several interaction parameters of the mixed-electrolyte solution such as θM,[Bmim],ΨM,[Bm,m],Cl, and ΨM,[Bmim].Br, and the average activity coefficient γ±of salts, and osmotic coefficient Φ of solvents, can be obtained on a basis of the experiments. Further, we used these physical parameters to evaluate the solid-liquid phase behavior in a quaternary system KCl-NaCl-[Bmim]Cl-H2O. Finally, we plotted the phase diagram of the quaternary mixture system.
2. The solubilities of KCl (and K2SO4) in ionic liquid1-Butyl-3-methyl imidazolium tetrafluoroborate ([Bmim][BF4]) aqueous solution were measured at standard atmospheric pressure, but different temperatures by utilizing laser-cloud point method. An empirical expression of the solubility m as a function of the temperature T was produced. Based on the measured solubility data in the quaternary system composed of KCl (or K2SO4) and [Bmim][BF4], we calculated the standard thermodynamic quantities of transfer of KCl (and K2SO4) when moving from water to the mixed solvent.
3. Thermodynamic properties such as density, viscosity, and refractive index in the MX-[Bmim]X-H2O (M=K, Na; X=Cl, Br) aqueous solution were measured in a temperature range of (T=298.15-328.15K) at standard atmospheric pressure. Our experiments indicate that density, viscosity, and the refractive index arise along with the increase of ionic liquids and salt concentration; wheras they decline along with the increase of temperature. In addition, we also calculated the apparent molar volumes VΦ, the limiting partial molar volumes VΦ0, and transfer partial molar volumes△trVΦ0of MX in mixed solutions. All the thermodynamic quantities can give a good interpretation how the solute molecules and the solvent molecules are interacting with each other in the ternary mixture systerm.
4. The solubility of the element sulfur in several pure aromatic hydrocarbons, pure aliphatic hydrocarbons as well as their mixtures with ionic liquids were measured by using cloud-point method in a temperature range of (7=293.15to353.15K) at standard atmospheric pressure. Although the measured solubilities of the element sulfur increase as the temperature increases in all cases, the solvent toluene exhibits a best capability to dissolve the element sulfur. Four different imidazolium ionic liquids:1-butyl-3-methylimidazolium hexafluorophosphate ([C4mim][PF6]),1-hexyl-3-methy limidazolium hexafluorophosphate ([C6mim][PF6]),1-butyl-3-methylimidazolium tetrafluoroborate ([C4mim][BF4]), and1-hexyl-3-methylimidazolium tetrafluoroborate ([C6mim][BF4]) were added separately into pure toluene solvent in order to investigate the impact of the addition of IL on the solubility of the element sulfur. The experimental results show that the chemical structure of the IL's cation and the concentration of ionic liquid are critical to the solubility of the element sulfur in the organic solvents. We employed several different empirical equations to correlate the solubility data measured in the toluene+[C6mim][PF6] mixture system, and calculated the free energy of transfer△trG, the entropy of transfer△trS, and the enthalpy of transfer△trH of the element sulfur moving from the pure toluene to the mixture solution.
引文
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