scholarly journals Dissolution of cotton by 1-ethyl-3-methylimidazolium acetate studied with time–temperature superposition for three different fibre arrangements

Cellulose ◽  
2020 ◽  
Author(s):  
Yunhao Liang ◽  
James E. Hawkins ◽  
Michael E. Ries ◽  
Peter J. Hine

Abstract This study has investigated the dissolution of cotton fibres in the ionic liquid 1-ethyl-3-methylimidazolium acetate ([C2mim][OAc]) for three fibre arrangements. Dissolution was carried out with excess [C2mim][OAc] at various temperatures and times followed by coagulation with water. Optical microscopy (OM) of the resulting processed and dried cotton fibres indicated that this procedure produced a coagulated fraction surrounding the original fibres. X-ray diffraction (XRD) showed that the crystal structure of this coagulated fraction was predominantly cellulose II, as opposed to the original fibres—mostly cellulose I. The OM and XRD results showed that growth of the coagulated fraction obeyed time–temperature superposition (TTS) and displayed an Arrhenius behaviour allowing a dissolution activation energy to be determined. Although the growth of the coagulated fraction with time were different for these distinct three arrangements, all could be individually shifted to form master curves using TTS, leading to very similar activation energies, 96 ± 3 kJ/mol (23 ± 1 kcal/mol). Graphic abstract

2020 ◽  
Vol 990 ◽  
pp. 225-230
Author(s):  
Kraiwit Pakutsah ◽  
Duangdao Aht-Ong

In this work, we described an effective approach to prepare nanofibrillated cellulose (NFC) with cellulose II structure under mild condition. Firstly, the water hyacinth (WH) was subjected to a series of a two-step chemical treatment, NaOH/urea pretreatment, and mechanical defibrillation at different defibrillation times. After that, raw water hyacinth fiber (RWF), bleached water hyacinth fiber (BWF), NaOH/urea pretreated water hyacinth fiber (PWF), and the resulting NFC were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD) as well as rheological measurements. It was found that RWF and BWF exhibited cellulose I crystal structure, whereas PWF and the obtained NFC possessed cellulose II crystal structure. FTIR analysis confirmed the evidence that no other chemical reactions preferentially occurred during both NaOH/urea pretreatment and mechanical defibrillation. As evidenced by rheological properties analysis, the NFC aqueous suspension with a gel-like structure demonstrated a shear-thinning behavior. The obtained NFC could potentially be utilized as a reinforcement for polymeric composites.


2017 ◽  
Vol 14 (27) ◽  
pp. 10-18
Author(s):  
Adewale ADEWUYI ◽  
Fabiano Vargas PEREIRA

Polythia longifolia seed (PL), an underutilized seed in Nigeria was used as a starting material to prepare Polythia longifolia cellulose nanocrystals (PLN). Polythia longifolia cellulose (PLC) was first isolated and subjected to sulfuric acid hydrolysis followed by ultrasonication and homogenization. PL, PLC and PLN were characterized using Fourier transformed infrared (FTIR), x-ray diffraction (XRD), thermogravimetric analysis (TG) and scanning electron microscopy (SEM). PLC and PLN were evaluated for their heavy metal adsorption capacity, swelling capacity, water holding capacity and oil holding capacity. SEM images reveal elliptical granules of PLN while XRD shows a mixture of polymorphs of cellulose I and cellulose II. PLN displayed a better water holding, oil holding and swelling capacities. PLN also exhibited a higher adsorption capacity towards Cu2+ and Pb2+ ions than PLC. The results showed that Polythia longifolia seed can serve as a potential source of cellulose nanocrystals which might be useful in other applications.


2016 ◽  
Vol 34 (2) ◽  
pp. 386-392 ◽  
Author(s):  
H.A.M. Ali ◽  
Magdy A. Ibrahim

AbstractThe crystal structure of (4E)-2-amino-3-cyanobenzo[b]oxocin-6-one, denoted as 4(E)-ACBO, was analyzed using X-ray diffraction technique. The dielectric and AC electrical conductivity measurements of the bulk 4(E)-ACBO in the form of pellet were studied in the range of frequency 42 Hz to 5 MHz and the temperature range of 303 K to 373 K. The temperature and frequency dependence of dielectric constant (∊1), dielectric loss (∊2) and AC electrical conductivity (σAC) were investigated. The relaxation time (τ) for electrons to hop over a barrier of height WH was calculated at different temperatures. The AC activation energy was determined from the temperature dependence of σAC at different frequencies.


Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


2002 ◽  
Vol 67 (4) ◽  
pp. 479-489 ◽  
Author(s):  
Michal Hušák ◽  
Bohumil Kratochvíl ◽  
Ivana Císařová ◽  
Ladislav Cvak ◽  
Alexandr Jegorov ◽  
...  

Two new structures of semisynthetic ergot alkaloid terguride created by unusual number of symmetry-independent molecules were determined by X-ray diffraction methods at 150 K. Form A (monoclinic, P212121, Z = 12) contains three symmetry-independent terguride molecules and two molecules of water in the asymmetric part of the unit cell. The form CA (monoclinic, P21, Z = 8) is an anhydrate remarkable by the presence of four symmetry-independent molecules in the crystal structure. Conformations of twelve symmetry-independent molecules that were found in four already described terguride structures are compared with torsion angles obtained by ab initio quantum-mechanical calculations for the simplified model of N-cyclohexyl-N'-diethylurea.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.


2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.


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