X-Ray Diffraction Studies of Ionic Liquids: From Spectra to Structure and Back

Author(s):  
Lorenzo Gontrani ◽  
Paolo Ballirano ◽  
Francesca Leonelli ◽  
Ruggero Caminiti
2021 ◽  
Vol 116 ◽  
pp. 5-14
Author(s):  
Marta Babicka ◽  
Magdalena Woźniak ◽  
Kinga Szentner ◽  
Sławomir Borysiak ◽  
Krzysztof Dwiecki ◽  
...  

The aim of this study was to compare parameters of nanocellulose obtained by two different procedures: hydrolysis with ionic liquids (1-allyl-3-methylimidazolium chloride and 1-ethyl-3-methylimidazolium acetate) and hydrolysis with ionic liquids in combination with hydrolysis using a cellulolytic enzyme from Trichoderma reesei. Avicel cellulose was treated with two ionic liquids: 1-allyl-3-methylimidazolium chloride (AmimCl) and 1-ethyl 3-methylimidazolium acetate (EmimOAc). In the two-step hydrolysis cellulose after treatment with ionic liquids was additionally hydrolyzed with a solution of enzymes. In order to characterize the obtained material, the following analyses were used: infrared spectroscopy, X-ray diffraction and dynamic light scattering. The results indicated that cellulose obtained by two-step nanocellulose production methods (first hydrolysis with ionic liquids and then with enzymes) showed similar parameters (particle size, XRD patterns and degree of crystallinity) as the material after the one-step process, i.e. hydrolysis with ionic liquids.


Author(s):  
H. Ohno ◽  
K. Igarashi ◽  
Norimasa Umesaki ◽  
K. Furukawa

Proceedings ◽  
2019 ◽  
Vol 16 (1) ◽  
pp. 26
Author(s):  
Patrycja Wilczewska ◽  
Aleksandra Bielicka-Giełdoń ◽  
Agnieszka Fiszka Borzyszkowska ◽  
Aleksandra Pieczyńska ◽  
Ewa Maria Siedlecka

A series of Bi4O5Br2 photocatalysts were prepared via an innovation method of synthesis with ionic liquids (ILs). The crystal structures were investigated by X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). The Field Emission Scanning Electron Microscope (FE-SEM) images illustrated the unique structure of prepared photocatalysts. The photocatalysts were also characterized by N2 adsorption-desorption analysis, X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra (UV-vis/DRS) and photoluminescence spectra (PL). The role of ILs in synthesis of Bi4O5Br2 on morphology and photocatalytic properties were investigated. Rhodamine B, 5-fluorouracil and chromium (VI) were used as the model micropollutants to evaluated adsorption capacity, photooxidation and photoreduction ability of prepared Bi4O5Br2 under artificial solar light. This work provided a new thought for enhanced photocatalytic activity of bismuth oxybromide photocatalysts.


2013 ◽  
Vol 652-654 ◽  
pp. 1539-1542
Author(s):  
Hou Jie Zhao ◽  
Chun Yan Wei ◽  
Yong Zhu Cui ◽  
Li Hua Lv ◽  
Xiao Wang

In this paper, regeneration of reed leaf fibers that have been degummed pretreatment in high temperature and pressure dissolved in 1-butyl-3-methylimidazolium chloride ionic liquids was studied. The samples containing 5% or 10%(wt/wt)reed leaf fibers in the ionic liquids, at 90°C for 7h.The dissolution process was viewed by polarizing microscope. Fourier-transform infrared spectroscopy(FT-IR) and X-ray diffraction were used to visualize the crystalline of reed leaf fiber transformed completely from cellulose I to cellulose Ⅱ after regenerated directly from 1-butyl-3-methylimidazolium chloride solution.


2019 ◽  
Author(s):  
◽  
Gcinile Pretty Mdletshe

Lignocellulosic materials have the potential to partly replace fossil-based resources as a source of bio-fuels, bio-chemicals, bio-composites and other bio-products. In this study, ionic liquids (ILs) were used in the pre-treatment of ground sugarcane bagasse (SCB). The ILs used were 1-butyl-3-methylimidazolium hydrogen sulphate or 1-butyl-3-methylimidazolium methyl sulphate at varied times. The ILs were able to remove lignin and hemicellulose from biomass. The IL [bmim][HSO4] had the highest amount of lignin removed after 12 h than all samples. Moreover, it resulted in the greatest cellulose amount. Milled SCB was pre-treated with IL/dimethyl sulphoxide (DMSO) mixtures. The IL [bmim][HSO4] was able to produce cellulose nanocrystals (CNCs) at 90 % IL and 100 % IL. The other IL failed to produce CNCs. Freeze drying the CNC suspension showed morphologies of long fibrous structures and rods which were evident in the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images. The crystallinity index of cellulose in the form of CNCs was calculated from powder X-ray diffraction (P-XRD). Thermal analysis of the CNCs was obtained from thermogravimetric analysis (TGA). Attenuated total reflection-Fourier transform infrared (ATR-FTIR) was used to confirm the absence of lignin and hemicellulose in CNCs. The size distribution of CNCs was obtained by using a dynamic light scattering (DLS) which showed that all the CNCs for the 100 % IL [bmim][HSO4] pre-treatment had a length < 500 nm. It was found that [bmim][HSO4], with no DMSO, was the most effective in terms of cellulose dissolution and the crystal sizes of CNCs. The conversion of cellulose to CNCs was successful with a 80 % and 100 % conversion for 90 % [bmim][HSO4]/DMSO and 100 % [bmim][HSO4], respectively.


2019 ◽  
Vol 43 (5) ◽  
pp. 2299-2306 ◽  
Author(s):  
Rakesh Samikannu ◽  
Shashi Kant Shukla ◽  
Ajaikumar Samikannu ◽  
Jyri-Pekka Mikkola

Herein, we have studied the potential of lutidinium-based ionic liquids in the dissolution of cellulose as confirmed by the X-ray diffraction (XRD), scanning electron microscopy (SEM) and 13C CP/MAS NMR, spectroscopic methods.


Molecules ◽  
2019 ◽  
Vol 24 (15) ◽  
pp. 2807 ◽  
Author(s):  
Md. Khalid Anwer ◽  
Mohammad Muqtader ◽  
Muzaffar Iqbal ◽  
Raisuddin Ali ◽  
Bjad K. Almutairy ◽  
...  

Estimating the solubility and solution thermodynamics parameters of aliskiren hemifumarate (AHF) in three different room temperature ionic liquids (RTILs), Transcutol-HP (THP) and water are interesting as there is no solubility data available in the literature. In the current study, the solubility and solution thermodynamics of AHF in three different RTILs, THP and water at the temperature range from 298.2 to 318.2 K under air pressure 0.1 MP were evaluated. The solid phase evaluation by Differential Scanning Calorimetry (DSC) and Powder X-ray Diffraction (PXRD) indicated no conversion of AHF into polymorph. The mole fraction solubility of AHF was found to be highest in 1-hexyl-3-methylimidazolium hexafluorophosphate (HMMHFP) ionic liquid (7.46 × 10−2) at 318.2 K. The obtained solubility values of AHF was regressed by the Apelblat and van’t Hoff models with overall root mean square deviations (RMSD) of 0.62% and 1.42%, respectively. The ideal solubility of AHF was higher compared to experimental solubility values at different temperatures. The lowest activity coefficient was found in HMMHFP, which confirmed highest molecular interaction between AHF–HMMHFP. The estimated thermodynamic parameters confirmed endothermic and entropy driven dissolution of AHF in different RTILs, THP, and water.


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