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Institute
- Institut für Chemie (122) (remove)
Magnetic ionogels (MagIGs) were prepared from organosilane-coated iron oxide nanoparticles, N-isopropylacrylamide, and the ionic liquid trihexyl(tetradecyl)phosphonium dicyanamide. The ionogels prepared with the silane-modified nanoparticles are more homogeneous than ionogels prepared with unmodified magnetite particles. The silane-modified particles are immobilized in the ionogel and are resistant tonanoparticle leaching. The modified particles also render the ionogels mechanically more stable than the ionogels synthesized with unmodified nanoparticles. The ionogels respond to external permanent magnets and are therefore prototypes of a new soft magnetic actuator.
4-Methyl-1-vinyl-1,2,4-triazolium triiodide ionic liquid and its polymer poly(4-methyl-1-vinyl-1,2,4-triazolium) triiodide were prepared for the first time from their iodide precursors via the reaction of iodide (I-) with elemental iodine (I-2). The change from iodide to triiodide (I-3(-)) was found to introduce particular variations in the physical properties of these two compounds, including lower melting point/glass transition temperature and altered solubility. The compounds were characterized by single-crystal X-ray diffraction, elemental analysis, and their electrochemical properties examined in solution and in the solid-state. Compared with their iodide analogues, the triiodide salts exhibited lower electrical impedance and higher current in the cyclic voltammetry. We found that poly(4-methyl-1,2,4-triazolium triiodide) was proven to be a promising solid polymer electrolyte candidate. (C) 2017 Elsevier Ltd. All rights reserved.
New ionogels (IGs) were prepared by combination of a series of sulfonate-based ionic liquids (ILs), 1-methyl-3-(4-sulfobutyl)imidazolium para-toluenesulfonate [BmimSO(3)][pTS], 1-methyl-1-butylpiperidiniumsulfonate para-toluenesul-fonate [BmpipSO(3)] [pTS], and 1-methyl-3-(4-sulfobutyl) imidazolium methylsulfonate [BmimSO(3)H][MeSO3] with a commercial stereolithography photoreactive resin. The article describes both the fundamental properties of the ILs and the resulting IGs. The IGs obtained from the ILs and the resin show high ionic conductivity of up to ca. 0.7.10(-4) S/cm at room temperature and 3.4-10(-3) S/cm at 90 degrees C. Moreover, the IGs are thermally stable to about 200 degrees C and mechanically robust. Finally, and most importantly, the article demonstrates that the IGs can be molded three-dimensionally using stereolithography. This provides, for the first time, access to IGs with complex 3D shapes with potential application in battery or fuel cell technology.
Ionogels (IGs) based on poly(methyl methacrylate) (PMMA) and the metal-containing ionic liquids (ILs) bis-1-butyl-3-methlimidazolium tetrachloridocuprate(II), tetrachloride cobaltate(II), and tetrachlorido manganate(II) have been synthesized and their mechanical and electrical properties have been correlated with their microstructure. Unlike many previous examples, the current IGs show a decreasing stability in stress-strain experiments on increasing IL fractions. The conductivities of the current IGs are lower than those observed in similar examples in the literature. Both effects are caused by a two-phase structure with micrometer-sized IL-rich domains homogeneously dispersed an IL-deficient continuous PMMA phase. This study demonstrates that the IL-polymer miscibility and the morphology of the IGs are key parameters to control the (macroscopic) properties of IGs.
Commercially available 1,2-PB was transformed into a well-defined reactive intermediate by quantitative bromination. The brominated polymer was used as a polyfunctional macroinitiator for the cationic ring-opening polymerization of 2-ethyl-2-oxazoline to yield a water-soluble brush polymer. Nucleophilic substitution of bromide by 1-methyl imidazole resulted in the formation of polyelectrolyte copolymers consisting of mixed units of imidazolium, bromo, and double bond. These copolymers, which were soluble in water without forming aggregates, were used as stabilizers in the heterophase polymerization of styrene and were also studied for their ionic conducting properties.
Transparent, ion-conducting, luminescent, and flexible ionogels based on the room temperature ionic liquid (IL) 1-butyl-3-methylimidazolium bis(trifluoromethane sulfonyl) imide [Bmim][N(Tf)(2)], a PtEu2 chromophore, and poly(methylmethacrylate) (PMMA) have been prepared. The thermal stability of the PMMA significantly increases with IL incorporation. In particular, the onset weight loss observed at ca. 229 degrees C for pure PMMA increases to 305 degrees C with IL addition. The ionogel has a high ionic conductivity of 10(-3) S cm(-1) at 373 K and exhibits a strong emission in the red with a long average luminescence decay time of tau = 890 mu s. The resulting material is a new type of soft hybrid material featuring useful thermal, optical, and ion transport properties.
We report on the ionothermal synthesis of porous carbon materials from a variety of carbohydrate precursors (i.e. D-glucose, D-fructose, D-xylose, and starch) using 1-butyl-3-methylimidazolium tetrachloroferrate(III), [Bmim][FeCl(4)] as a reusable solvent and catalyst. The carbon materials derived from these different carbohydrates are similar in terms of particle size and chemical composition, possessing relatively high surface areas from 44 to 155 m(2) g(-1) after ionothermal processing, which can be significantly increased to > 350 m(2) g(-1) by further thermal treatment (e. g. post-carbonization at 750 degrees C). CO(2) and N(2) sorption analysis, combined with Hg intrusion porosimetry, reveals a promising hierarchical pore structuring to these carbon materials. The ionic liquid [Bmim][FeCl(4)] has a triple role: it acts as both a soft template to generate the characterized pore structuring, solvent and as a catalyst resulting in enhanced ionothermal carbon yields. Importantly from a process point of view, the ionic liquid can be successfully recovered and reused. The current work shows that ionothermal synthesis has the potential to be an effective, low cost, and green reusable synthetic route towards sustainable porous carbon materials.
The iron-containing ionic liquids 1-butyl-3-methylimidazolium tetrachloroferrate(III) [C(4)mim][FeCl4] and 1-dodecyl-3-methylimidazolium tetrachloroferrate(III) [C(12)mim][FeCl4] exhibit a thermally induced demixing with water (thermomorphism). The phase separation temperature varies with IL weight fraction in water and can be tuned between 100 degrees C and room temperature. The reversible lower critical solution temperature (LCST) is only observed at IL weight fractions below ca. 35% in water. UV/Vis, IR, and Raman spectroscopy along with elemental analysis prove that the yellow-brown liquid phase recovered after phase separation is the starting IL [C(4)mim][FeCl4] and [C(12)mim][FeCl4], respectively. Photometry and ICP-OES show that about 40% of iron remains in the water phase upon phase separation. Although the process is thus not very efficient at the moment, the current approach is the first example of an LCST behavior of a metal-containing IL and therefore, although still inefficient, a prototype for catalyst removal or metal extraction.
The iron-containing ionic liquid (IL) 1-butyl-3-methylimidazolium tetrachloroferrate(III) [Bmim][FeCl4] has been used as a building block in the synthesis of transparent, ion-conducting, and paramagnetic ionogels. UV/Vis spectroscopy shows that the coordination around the Fe(III) ion does slightly change upon incorporation of the IL into PMMA. The thermal stability of the PMMA increases significantly with IL incorporation. In particular, the onset weight loss observed at ca. 265 degrees C for pure PMMA is completely suppressed. The ionic conductivity shows a strong temperature dependence and increases with increasing IL weight fractions. The magnetic properties are similar to those reported for the pure IL and are not affected by the incorporation into the PMMA matrix. The resulting ionogel is thus an interesting prototype for soft, flexible, and transparent materials combining the mechanical properties of the matrix with the functionality of the metal-containing IL, such as magnetism.
The large-scale green synthesis of graphene-type two-dimensional materials is still challenging. Herein, we describe the ionothermal synthesis of carbon-based composites from fructose in the iron-containing ionic liquid 1-butyl-3-methylimidazolium tetrachloridoferrate(III), [Bmim][FeCl4] serving as solvent, catalyst, and template for product formation. The resulting composites consist of oligo-layer graphite nanoflakes and iron carbide particles. The mesoporosity, strong magnetic moment, and high specific surface area of the composites make them attractive for water purification with facile magnetic separation. Moreover, Fe3Cfree graphite can be obtained via acid etching, providing access to fairly large amounts of graphite material. The current approach is versatile and scalable, and thus opens the door to ionothermal synthesis towards the larger-scale synthesis of materials that are, although not made via a sustainable process, useful for water treatment such as the removal of organic molecules.
The large-scale green synthesis of graphene-type two-dimensional materials is still challenging. Herein, we describe the ionothermal synthesis of carbon-based composites from fructose in the iron-containing ionic liquid 1-butyl-3-methylimidazolium tetrachloridoferrate(III), [Bmim][FeCl4] serving as solvent, catalyst, and template for product formation. The resulting composites consist of oligo-layer graphite nanoflakes and iron carbide particles. The mesoporosity, strong magnetic moment, and high specific surface area of the composites make them attractive for water purification with facile magnetic separation. Moreover, Fe3Cfree graphite can be obtained via acid etching, providing access to fairly large amounts of graphite material. The current approach is versatile and scalable, and thus opens the door to ionothermal synthesis towards the larger-scale synthesis of materials that are, although not made via a sustainable process, useful for water treatment such as the removal of organic molecules.
Transparent, ion-conducting, and flexible ionogels based on the room temperature ionic liquid (IL) 1-butyl-3-methylimidazolium bis(trifluoromethane sulfonyl) imide [Bmim][N(Tf)(2)], the dye-IL (DIL) 1-butyl-3-methylimidazolium methyl orange [Bmim][MO], and poly(methylmethacrylate) (PMMA) are prepared. Upon IL incorporation the thermal stability of the PMMA matrix significantly increases from 220 to 280 degrees C. The ionogels have a relatively high ionic conductivity of 10(-4) S cm(-1) at 373 K. Most importantly, the ionogels exhibit a strong and reversible color change when exposed to aqueous or organic solutions containing protons or hydroxide ions. The resulting material is thus a prototype of soft multifunctional matter featuring ionic conductivity, easy processability, response to changes in the environment, and a strong readout signal, the color change, that could be used in optical data storage or environmental sensing.
The use of acidic ionic liquids and solids as electrolytes in fuel cells is an emerging field due to their efficient proton conductivity and good thermal stability. Despite multiple reports describing conducting properties of acidic ILs, little is known on the charge-transport mechanism in the vicinity of liquid-glass transition and the structural factors governing the proton hopping. To address these issues, we studied two acidic imidazolium-based ILs with the same cation, however, different anions-bulk tosylate vs small methanesulfonate. High-pressure dielectric studies of anhydrous and water-saturated materials performed in the close vicinity of T-g have revealed significant differences in the charge-transport mechanism in these two systems being undetectable at ambient conditions. Thereby, we demonstrated the effect of molecular architecture on proton hopping, being crucial in the potential electrochemical applications of acidic ILs.
We present and discuss the results of crystallographic and electron paramagnetic resonance (EPR) spectroscopic analyses of five tetrachloridocuprate(II) complexes to supply a useful tool for the structural characterisation of the [CuCl4]2− moiety in the liquid state, for example in ionic liquids, or in solution. Bis(benzyltriethylammonium)-, bis(trimethylphenylammonium)-, bis(ethyltriphenylphosphonium)-, bis(benzyltriphenylphosphonium)-, and bis(tetraphenylarsonium)tetrachloridocuprate(II) were synthesised and characterised by elemental, IR, EPR and X-ray analyses. The results of the crystallographic analyses show distorted tetrahedral coordination geometry of all [CuCl4]2− anions in the five complexes and prove that all investigated complexes are stabilised by hydrogen bonds of different intensities. Despite the use of sterically demanding ammonium, phosphonium and arsonium cations to obtain the separation of the paramagnetic Cu(II) centres for EPR spectroscopy no hyperfine structure was observed in the EPR spectra but the principal values of the electron Zeeman tensor, g∥ and g⊥, could be determined. With these EPR data and the crystallographic parameters we were able to carry out a correlation study to anticipate the structural situation of tetrachloridocuprates in different physical states. This correlation is in good agreement with DFT calculations.
We present and discuss the results of crystallographic and electron paramagnetic resonance (EPR) spectroscopic analyses of five tetrachloridocuprate(II) complexes to supply a useful tool for the structural characterisation of the [CuCl4](2-) moiety in the liquid state, for example in ionic liquids, or in solution. Bis(benzyltriethylammonium)-, bis(trimethylphenylammonium)-, bis(ethyltriphenylphosphonium)-, bis(benzyltriphenylphosphonium)-, and bis(tetraphenylarsonium) tetrachloridocuprate(II) were synthesised and characterised by elemental, IR, EPR and X-ray analyses. The results of the crystallographic analyses show distorted tetrahedral coordination geometry of all [CuCl4](2-) anions in the five complexes and prove that all investigated complexes are stabilised by hydrogen bonds of different intensities. Despite the use of sterically demanding ammonium, phosphonium and arsonium cations to obtain the separation of the paramagnetic Cu(II) centres for EPR spectroscopy no hyperfine structure was observed in the EPR spectra but the principal values of the electron Zeeman tensor, g(parallel to) and g(perpendicular to), could be determined. With these EPR data and the crystallographic parameters we were able to carry out a correlation study to anticipate the structural situation of tetrachloridocuprates in different physical states. This correlation is in good agreement with DFT calculations.
A class of adsorbents currently receiving growing attention is the clay-polymer nanocomposite (CPN) adsorbents. CPNs effectively treat water by adsorption and flocculation of both inorganic and organic micropollutants from aqueous solutions. Some of these CPNs - when modified with biocides - also have the ability to efficiently remove microorganisms such as Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Candida albicans from water. CPNs are far more easily recovered from aqueous media than neat clay. They also exhibit far better treatment times than either polymer or clay adsorbents. They have higher adsorption capacity and better life cycles compared with clay alone. CPNs therefore show an excellent potential as highly efficient water and waste treatment agents.
This article reviews the various CPNs that have been prepared recently and used as adsorbents in the removal of micropollutants (inorganic, organic and biological) from aqueous solutions. A special focus is placed on CPNs that are not only interesting from an academic point of view but also effectively reduce the concentration of micropollutants in water to safe limits and also on new developments bordering on CPN use as water treatment agent that have not yet realized their full potential. (C) 2014 Elsevier B.V. All rights reserved.
A new sulfonated aniline-modified poly(vinyl alcohol)/K-feldspar (SAPK) composite was prepared. The cation-exchange capacity of the composite was found to be S times that of neat feldspar. The specific surface area and point of zero charge also changed significantly upon modification, from 15.6 +/- 0.1 m(2)/g and 2.20 (K-feldspar) to 73.6 +/- 0.3 m(2)/g and 1.91 (SAPK). Zn2+, Cd2+, and Pb2+ adsorption was found to be largely independent of pH, and the metal adsorption rate on SAPK was higher than that on neat feldspar. This particularly applies to the initial adsorption rates. The adsorption process involves both film and pore diffusion; film diffusion initially controls the adsorption. The Freundlich and Langmuir models were found to fit metal-ion adsorption on SAPK most accurately. Adsorption on neat feldspar was best fitted with a Langmuir model, indicating the formation of adsorbate monolayers. Both pure feldspar and SAPK showed better selectivity for Pb2+ than for Cd2+ or Zn2+.
A new micro/mesoporous hybrid clay nanocomposite prepared from kaolinite clay, Carica papaya seeds, and ZnCl2 via calcination in an inert atmosphere is presented. Regardless of the synthesis temperature, the specific surface area of the nanocomposite material is between approximate to 150 and 300 m(2)/g. The material contains both micro- and mesopores in roughly equal amounts. X-ray diffraction, infrared spectroscopy, and solid-state nuclear magnetic resonance spectroscopy suggest the formation of several new bonds in the materials upon reaction of the precursors, thus confirming the formation of a new hybrid material. Thermogravimetric analysis/differential thermal analysis and elemental analysis confirm the presence of carbonaceous matter. The new composite is stable up to 900 degrees C and is an efficient adsorbent for the removal of a water micropollutant, 4-nitrophenol, and a pathogen, E. coli, from an aqueous medium, suggesting applications in water remediation are feasible.