离子液体的合成与应用
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摘要
近年来,离子液体的研究日趋活跃,因其具有几乎可忽略的饱和蒸气压、低毒、宽的液相范围和电化学窗口、对有机物和无机物有良好的溶解性等特殊性能,已被广泛地应用于有机合成、分离、电化学和无机物的制备中。
在本论文中,我们合成了几种离子液体,并以离子液体为反应介质合成了氯化亚铜、硫化锌和硫化镉,并对反应后的离子液体进行了回收、表征和再利用的研究。利用X-射线衍射(XRD)表征样品的结构;用透射电子显微镜(TEM)和扫描电子显微镜(SEM)观测样品的粒径和微观形貌;用紫外-可见光谱(UV-Vis)和荧光光谱(PL)表征样品的光学性能、能带宽度和粒径大小。XRD和TEM分析揭示了以离子液体为反应溶剂的体系中,目标产物达到纳米级,且离子液体的应用对纳米化合物的结晶度和样品的颗粒大小有一定的影响。SEM分析表明离子液体对目标产物的形貌起到了修饰作用。UV-Vis分析表明在离子液体/水的反应体系中得到的目标产物的吸收峰位向短波方向偏移,表现出了明显的蓝移,展现了纳米材料的量子尺寸效应。PL分析表明在离子液体/水的反应体系中得到的目标产物发光强度有不同程度的增强。
众所周知,在水溶液中,Cu~Ⅱ(φ_(Cu2+/Cu+)/V=+0.17),Cu~Ⅰ(φ_(Cu+/Cu)/V=+0.521),因此氯化亚铜易歧化,但在离子液体中却合成了氯化亚铜纳米晶,这为解决传统工业生产氯化亚铜中大量的无机酸等给环境带来的影响提供了一种经济而环保的可行的方法。在硫化锌和硫化镉的合成中,以硫化钠为硫源,反应速度快,易于生产硫化物,离子液体的辅助作用使样品粒径达到纳米级,同时,目标产物发光强度有不同程度的增强。本文对样品的合成机理也进行了初步的探讨。
Room-temperature ionic liquids(RTILs),which have been intensively studied,had wide applications in the organic chemical reactions,separations,electrochemical and inorganic material synthesis due to their negligible vapor pressure,low toxicity,broad liquid temperature range,large electrochemical window,high specific solvent abilities for many organic and inorganic materials,and so on.
In this paper,several RTILs were synthesized,and then were used as reaction media for CuCl,ZnS and CdS nanoparticles.The refreshed RTILs were studied after the reactions.The structure of samples was characterized by X-ray diffraction(XRD).The particle sizes and morphologies of samples were observed by transmission electron microscopy(TEM)and scanning electron microscopy(SEM).The optical properties,band gap energy and size of nanocrystals were studied by PL and UV-Vis spectrophotometer measurements.XRD and TEM analysis revealed that the samples obtained from ionic liquids reaction systems were in nanosize.And it was found that the the ionic liquids had the influence on the crystallinity and particle sizes of samples.SEM analysis revealed that the morphology of the samples was modified by ionic liquids media.UV-Vis spectra revealed that the absorbance peaks of the samples obtained from ionic liquids/H_2O had blue shift,which showed the quantum size effect.PL analysis revealed that the samples obtained from ionic liquids/H_2O contained reaction media had stronger excitation peaks.
It is known that Cu~Ⅱ(φ_(Cu2+/Cu+)/V=+0.17)and Cu can not react to form Cu~Ⅰ(φ_(Cu+/Cu)/V = +0.521)in aqueous systems,whereas RTIL here acted as both a nonaqueous medium and an electrical conductor drove the above reaction.So this study may promise an economical and ecologically benign method for CuCl in the traditional industrial synthesis.In the synthesis of ZnS and CdS,Na_2S used as S source made it possible to get sulfides in short time.Meantimes,the RTILs in these systems acted as adjuvant made the sizes of these samples to nanometer, and the samples had stronger excitation peaks.The possible formation mechanism of samples had been studied as well.
在本论文中,我们合成了几种离子液体,并以离子液体为反应介质合成了氯化亚铜、硫化锌和硫化镉,并对反应后的离子液体进行了回收、表征和再利用的研究。利用X-射线衍射(XRD)表征样品的结构;用透射电子显微镜(TEM)和扫描电子显微镜(SEM)观测样品的粒径和微观形貌;用紫外-可见光谱(UV-Vis)和荧光光谱(PL)表征样品的光学性能、能带宽度和粒径大小。XRD和TEM分析揭示了以离子液体为反应溶剂的体系中,目标产物达到纳米级,且离子液体的应用对纳米化合物的结晶度和样品的颗粒大小有一定的影响。SEM分析表明离子液体对目标产物的形貌起到了修饰作用。UV-Vis分析表明在离子液体/水的反应体系中得到的目标产物的吸收峰位向短波方向偏移,表现出了明显的蓝移,展现了纳米材料的量子尺寸效应。PL分析表明在离子液体/水的反应体系中得到的目标产物发光强度有不同程度的增强。
众所周知,在水溶液中,Cu~Ⅱ(φ_(Cu2+/Cu+)/V=+0.17),Cu~Ⅰ(φ_(Cu+/Cu)/V=+0.521),因此氯化亚铜易歧化,但在离子液体中却合成了氯化亚铜纳米晶,这为解决传统工业生产氯化亚铜中大量的无机酸等给环境带来的影响提供了一种经济而环保的可行的方法。在硫化锌和硫化镉的合成中,以硫化钠为硫源,反应速度快,易于生产硫化物,离子液体的辅助作用使样品粒径达到纳米级,同时,目标产物发光强度有不同程度的增强。本文对样品的合成机理也进行了初步的探讨。
Room-temperature ionic liquids(RTILs),which have been intensively studied,had wide applications in the organic chemical reactions,separations,electrochemical and inorganic material synthesis due to their negligible vapor pressure,low toxicity,broad liquid temperature range,large electrochemical window,high specific solvent abilities for many organic and inorganic materials,and so on.
In this paper,several RTILs were synthesized,and then were used as reaction media for CuCl,ZnS and CdS nanoparticles.The refreshed RTILs were studied after the reactions.The structure of samples was characterized by X-ray diffraction(XRD).The particle sizes and morphologies of samples were observed by transmission electron microscopy(TEM)and scanning electron microscopy(SEM).The optical properties,band gap energy and size of nanocrystals were studied by PL and UV-Vis spectrophotometer measurements.XRD and TEM analysis revealed that the samples obtained from ionic liquids reaction systems were in nanosize.And it was found that the the ionic liquids had the influence on the crystallinity and particle sizes of samples.SEM analysis revealed that the morphology of the samples was modified by ionic liquids media.UV-Vis spectra revealed that the absorbance peaks of the samples obtained from ionic liquids/H_2O had blue shift,which showed the quantum size effect.PL analysis revealed that the samples obtained from ionic liquids/H_2O contained reaction media had stronger excitation peaks.
It is known that Cu~Ⅱ(φ_(Cu2+/Cu+)/V=+0.17)and Cu can not react to form Cu~Ⅰ(φ_(Cu+/Cu)/V = +0.521)in aqueous systems,whereas RTIL here acted as both a nonaqueous medium and an electrical conductor drove the above reaction.So this study may promise an economical and ecologically benign method for CuCl in the traditional industrial synthesis.In the synthesis of ZnS and CdS,Na_2S used as S source made it possible to get sulfides in short time.Meantimes,the RTILs in these systems acted as adjuvant made the sizes of these samples to nanometer, and the samples had stronger excitation peaks.The possible formation mechanism of samples had been studied as well.
引文
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