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Imidazolium decyl sulfate: a very promising selfmade ionic hydrogel†
Materials Chemistry Frontiers ( IF 6.0 ) Pub Date : 2017-12-26 00:00:00 , DOI: 10.1039/c7qm00510e Oscar Cabeza 1, 2, 3, 4 , Esther Rilo 1, 2, 3, 4 , Luisa Segade 1, 2, 3, 4 , Montserrat Domínguez-Pérez 1, 2, 3, 4 , Sandra García-Garabal 1, 2, 3, 4 , David Ausín 1, 2, 3, 4 , Elena López-Lago 4, 5, 6, 7 , Luis Miguel Varela 4, 6, 7, 8 , Miguel Vilas 4, 9, 10, 11 , Pedro Verdía 4, 9, 10, 11 , Emilia Tojo 4, 9, 10, 11
Materials Chemistry Frontiers ( IF 6.0 ) Pub Date : 2017-12-26 00:00:00 , DOI: 10.1039/c7qm00510e Oscar Cabeza 1, 2, 3, 4 , Esther Rilo 1, 2, 3, 4 , Luisa Segade 1, 2, 3, 4 , Montserrat Domínguez-Pérez 1, 2, 3, 4 , Sandra García-Garabal 1, 2, 3, 4 , David Ausín 1, 2, 3, 4 , Elena López-Lago 4, 5, 6, 7 , Luis Miguel Varela 4, 6, 7, 8 , Miguel Vilas 4, 9, 10, 11 , Pedro Verdía 4, 9, 10, 11 , Emilia Tojo 4, 9, 10, 11
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In this paper, we show, for the first time, the synthesis, structural characterization, phase diagram and physical properties of the ionic liquid, 1-ethyl-3-methyl imidazolium decyl sulfate [EMIm][DSO4]. At 25 °C it is either a crystalline solid or a liquid depending on the thermal history as its melting point is about 33 °C and its point of solidification is about 22 °C. The interest of this new IL lies in its ability to become a rigid hydrogel when mixed with water. As observed in many ILs, the as-prepared IL is hygroscopic and it adsorbs about 14 wt% of water at usual laboratory conditions and up to 27 wt% in a 100% saturated atmosphere. Due to the H-bonds between water and the amphiphilic [DSO4] anions, a lyotropic HI liquid crystalline phase is formed in the hydrated state, which can be observed in micrographs recorded using white polarized light. The moisture adsorption is a completely reversible process; thus, the rigid-gel sample loses all adsorbed water when it is left in a dry atmosphere for a few hours, transitioning to the liquid state. Phase diagrams of the temperature-water concentration is presented and compared with that of the parent compound [EMIm] octyl sulfate, [OSO4]. X-ray diffraction revels that below 15 °C the hydrated compound crystallizes into a P2/m monoclinic structure. The structure of the new compound was confirmed by NMR, FTIR and mass spectroscopy (MS). In addition, the temperature behavior of ionic conductivity was experimentally measured and analyzed for the pure compound and for two samples hydrated with 10 wt% and 39 wt% of water. Viscosity and density were also measured vs. temperature for the pure sample. The as-prepared IL shows great potential for numerous practical applications.
中文翻译：
咪唑癸基硫酸盐：非常有前途的自制离子水凝胶†
本文首次展示了离子液体1-乙基-3-甲基咪唑鎓癸基硫酸盐[EMIm] [DSO 4 ]的合成，结构表征，相图和物理性质。在25°C下，根据其热历史，它可以是结晶固体，也可以是液体，因为其熔点约为33°C，凝固点约为22°C。这种新型IL的兴趣在于与水混合后能变成刚性水凝胶的能力。如在许多离子液体中所观察到的，如此制备的离子液体具有吸湿性，并且在通常的实验室条件下可吸收约14 wt％的水，在100％的饱和气氛中可吸收高达27 wt％的水。由于水和两亲性[DSO 4 ]阴离子之间存在氢键，因此溶致的H I在水合状态下形成液晶相，这可以在使用白色偏振光记录的显微照片中观察到。水分的吸附是一个完全可逆的过程。因此，当硬质凝胶样品在干燥的气氛中放置数小时后，所有的吸附水都会流失，从而转变为液态。给出了温度-水浓度的相图，并将其与母体化合物[EMIm]辛基硫酸盐[OSO 4 ]的相图进行了比较。X射线衍射表明，低于15°C时，水合化合物结晶为P 2 / m单斜结构。新化合物的结构通过NMR，FTIR和质谱（MS）确认。另外，通过实验测量和分析了纯化合物以及两个分别用水和10 wt％和39 wt％水合的样品的离子电导率的温度行为。还测量了纯样品的粘度和密度与温度的关系。所制备的IL在众多实际应用中显示出巨大的潜力。
更新日期：2017-12-26
中文翻译：
咪唑癸基硫酸盐：非常有前途的自制离子水凝胶†
本文首次展示了离子液体1-乙基-3-甲基咪唑鎓癸基硫酸盐[EMIm] [DSO 4 ]的合成，结构表征，相图和物理性质。在25°C下，根据其热历史，它可以是结晶固体，也可以是液体，因为其熔点约为33°C，凝固点约为22°C。这种新型IL的兴趣在于与水混合后能变成刚性水凝胶的能力。如在许多离子液体中所观察到的，如此制备的离子液体具有吸湿性，并且在通常的实验室条件下可吸收约14 wt％的水，在100％的饱和气氛中可吸收高达27 wt％的水。由于水和两亲性[DSO 4 ]阴离子之间存在氢键，因此溶致的H I在水合状态下形成液晶相，这可以在使用白色偏振光记录的显微照片中观察到。水分的吸附是一个完全可逆的过程。因此，当硬质凝胶样品在干燥的气氛中放置数小时后，所有的吸附水都会流失，从而转变为液态。给出了温度-水浓度的相图，并将其与母体化合物[EMIm]辛基硫酸盐[OSO 4 ]的相图进行了比较。X射线衍射表明，低于15°C时，水合化合物结晶为P 2 / m单斜结构。新化合物的结构通过NMR，FTIR和质谱（MS）确认。另外，通过实验测量和分析了纯化合物以及两个分别用水和10 wt％和39 wt％水合的样品的离子电导率的温度行为。还测量了纯样品的粘度和密度与温度的关系。所制备的IL在众多实际应用中显示出巨大的潜力。
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