NDLI: Thermal stability and crystallization of N-alkyl-N-alkyl′-pyrrolidinium imides

Content Provider	Springer Nature Link
Author	Stefan, Claudia Simona Lemordant, Daniel Biensan, Philippe Siret, Clémence Claude Montigny, Bénédicte
Copyright Year	2010
Abstract	A series of N-alkyl-N-alkyl′-pyrrolidinium-bis(trifluoromethanesulfonyl) imide (TFSI$^{−}$) room temperature ionic liquids (RTILs) has been investigated by means of thermogravimetric analysis (TG), differential scanning calorimetry, FT-IR spectroscopy, and X-ray diffraction analysis. These compounds exhibit a thermal stability up to 548–573 K. The mass loss starting temperature, T $_{ml}$, falls in a narrow range of temperatures: 578–594 K. FT-IR spectra, performed before and after 24 h isothermal experiments at 553 and 573 K, have confirmed their great thermal stability. Below the ambient temperature, these compounds exhibit a complex behavior. N-methyl-N-propyl-pyrrolidinium-TFSI is the sole liquid which crystallizes without forming any amorphous phase even after quenching in liquid nitrogen. Its crystalline phase has a melting point, T $_{m}$, of 283 ± 1 K. When the amorphous solid is heated, the N-butyl-N-ethyl-pyrrolidinium-TFSI presents a glass transition temperature, T $_{g}$, at 186 K followed by a cold crystallization, T $_{cc}$, at 225 K, and a final T $_{m}$ at 262 K. The N-butyl-N-methyl-pyrrolidinium-TFSI exhibits a T $_{g}$ between 186 and 181 K, its cold crystallization leading to two different solid phases. Solid phase I has a melting point T $_{I,m}$ = 252 K and phase II, T $_{II,m}$ = 262 K. When the amorphous phase is obtained at a cooling rate of 10 K/min, its T $_{cc}$ is 204 K, and a metastable solid phase (III) is obtained which transforms into the phase II at 226 K. However, when the sample is quenched, the amorphous phase transforms into phase II at T $_{cc}$ = 217 K and phase I at 239 K. P$_{15}$-TFSI exhibits the most complicated pattern as, on cooling, it leads to both a crystallized phase at 237 K and an amorphous phase at 191 K. On heating, after a T $_{g}$ at 186 K and a T $_{cc}$ at 217 K, two solid–solid phase transitions are observed at 239 K and 270 K, the final T $_{m}$ being 279 K.
Starting Page	685
Ending Page	693
Page Count	9
File Format	PDF
ISSN	13886150
Journal	Journal of thermal analysis
Volume Number	102
Issue Number	2
e-ISSN	15728943
Language	English
Publisher	Springer Netherlands
Publisher Date	2010-05-28
Publisher Place	Dordrecht
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Room temperature ionic liquids Flammability Thermal stability DSC TG Isothermal test Measurement Science and Instrumentation Inorganic Chemistry Polymer Sciences Analytical Chemistry Physical Chemistry
Content Type	Text
Resource Type	Article
Subject	Physical and Theoretical Chemistry Condensed Matter Physics

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