scholarly journals Thermotropic Liquid-Crystalline and Light-Emitting Properties of Bis(4-aalkoxyphenyl) Viologen Bis(triflimide) Salts

Molecules ◽  
2020 ◽  
Vol 25 (10) ◽  
pp. 2435
Author(s):  
Pradip K. Bhowmik ◽  
Muhammed Kareem M. Al-Karawi ◽  
Shane T. Killarney ◽  
Erenz J. Dizon ◽  
Anthony Chang ◽  
...  
Keyword(s):  
Liquid Crystalline ◽  
Variable Temperature ◽  
X Ray Diffraction ◽  
Metathesis Reaction ◽  
Scanning Calorimetry ◽  
Thermal Stabilities ◽  
Light Emitting ◽  
Chemical Structures ◽  
Nuclear Magnetic Resonance Spectra ◽  
13C Nuclear Magnetic Resonance

A series of bis(4-alkoxyphenyl) viologen bis(triflimide) salts with alkoxy chains of different lengths were synthesized by the metathesis reaction of respective bis(4-alkoxyphenyl) viologen dichloride salts, which were in turn prepared from the reaction of Zincke salt with the corresponding 4-n-alkoxyanilines, with lithium triflimide in methanol. Their chemical structures were characterized by 1H and 13C nuclear magnetic resonance spectra and elemental analysis. Their thermotropic liquid-crystalline (LC) properties were examined by differential scanning calorimetry, polarizing optical microscopy, and variable temperature X-ray diffraction. Salts with short length alkoxy chains had crystal-to-liquid transitions. Salts of intermediate length alkoxy chains showed both crystal-to-smectic A (SmA) transitions, Tms, and SmA-to-isotropic transitions, Tis. Those with longer length of alkoxy chains had relatively low Tms at which they formed the SmA phases that persisted up to the decomposition at high temperatures. As expected, all of them had excellent thermal stabilities in the temperature range of 330–370 °C. Their light-emitting properties in methanol were also included.

scholarly journals Thermotropic Liquid-Crystalline Properties of Viologens Containing 4-n-alkylbenzenesulfonates

Crystals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 77 ◽  
Author(s):  
Pradip Bhowmik ◽  
Anthony Chang ◽  
Jongin Kim ◽  
Erenz Dizon ◽  
Ronald Principe ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Differential Scanning Calorimetry ◽  
Fourier Transform ◽  
Liquid Crystalline ◽  
Metathesis Reaction ◽  
Scanning Calorimetry ◽  
Chemical Structures ◽  
Nuclear Magnetic Resonance Spectra ◽  
13C Nuclear Magnetic Resonance ◽  
Melting Transitions

A series of viologens containing 4-n-alkylbenzenesulfonates were synthesized by the metathesis reaction of 4-n-alkylbenzenesulfonic acids or sodium 4-n-alkylbezenesulfonates with the respective viologen dibromide in alcohols. Their chemical structures were characterized by Fourier Transform Infrared, 1H and 13C Nuclear Magnetic Resonance spectra and elemental analysis. Their thermotropic liquid-crystalline (LC) properties were examined by differential scanning calorimetry and polarizing optical microscopy. They formed LC phases above their melting transitions and showed isotropic transitions. As expected, all the viologen salts had excellent stabilities in the temperature range of 278–295 °C as determined by thermogravimetric analysis.

Effect of Two Diferrent Mesogens on Liquid-Crystalline Properties of Chiral Side-Chain Liquid-Crystalline Polysiloxanes

2011 ◽  
Vol 415-417 ◽  
pp. 1395-1398
Author(s):  
Ji Wei Wang ◽  
Jun Qing Zi ◽  
Li Xian He ◽  
Guang Yong Chen ◽  
Yan Zhong Yang
Keyword(s):  
Liquid Crystalline ◽  
Proton Nuclear Magnetic Resonance ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Cholesteric Phase ◽  
Long Wavelength ◽  
Crystalline Polymers ◽  
Chemical Structures ◽  
Nuclear Magnetic Resonance Spectra ◽  
Temperature Ranges

Abstract. A series of liquid crystalline polysiloxanes were synthesized by cholesteric LC monomer and nematic LC monomer. The chemical structures and liquid-crystalline properties of the monomers and polymers were characterized by various experimental techniques including Fourier transform infrared (FTIR), proton nuclear magnetic resonance spectra (1H-NMR), differential scanning calorimetry (DSC), thermogravimetric analyses (TGA) , X-ray diffraction measurements (XRD) and polarizing optical microscopy (POM). All the liquid crystalline polymers showed liquid crystalline properties with wide mesophase temperature ranges. For the polymers bearing only of one nematic LC monomer, it showed nematic phase, while others showed cholesteric phase. With increase the content of nematic LC monomer in the polymers from P1 to P7, the glass transition temperature and the isotropic temperature increased on heating circles. Reflection spectra of cholesteric mesophase of the series of polymers showed that the reflected wavelength shifted to long wavelength with increase content of nematic LC monomer in the polymers in the polymer systems, suggesting that helical pitch (P) become long.

Star mesogens — Synthesis and structural characterization using 1D and 2D solution NMR techniques and mesophase characterization

2013 ◽  
Vol 91 (3) ◽  
pp. 196-205 ◽  
Author(s):  
A. Shanavas ◽  
T. Narasimhaswamy ◽  
B.V.N. Phani Kumar ◽  
A. Sultan Nasar
Keyword(s):  
Chain Length ◽  
Liquid Crystalline ◽  
Variable Temperature ◽  
2D Nmr ◽  
Smectic Layer ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Xrd Techniques ◽  
Terminal Chain

Novel star mesogens based on trimesic acid and symmetrical side arm cores with terminal alkoxy groups were synthesized via a divergent approach. The central core and side arms were connected through alkyl spacers. All the synthesized mesogens and their intermediates were characterized thoroughly using Fourier transform infrared (FT-IR), 1H nuclear magnetic resonance (NMR), 13C NMR, and mass spectrometers. One representative mesogen was subjected to the two-dimensional (2D) NMR experiments to ascertain the structure of the mesogens. The mesophase characterization was carried out using hot-stage optical polarizing microscopy (HOPM), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques. Many of the molecules with an ethyloxy spacer were found to be nonmesogenic, whereas all the molecules with a butyloxy spacer showed liquid crystalline phases. The increase of terminal chain length decreased the transition temperatures. The nematic phase was observed for the mesogens with short terminal chain length, whereas smectic polymorphism was observed on increasing the terminal chain length. The results of a variable temperature powder X-ray diffraction of the representative sample support the smectic layer ordering.

scholarly journals Poly(Pyridinium Salt)s Containing 2,7-Diamino-9,9′-Dioctylfluorene Moieties with Various Organic Counterions Exhibiting Both Lyotropic Liquid-Crystalline and Light-Emitting Properties

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1560
Author(s):  
Pradip K. Bhowmik ◽  
Tae S. Jo ◽  
Jung J. Koh ◽  
Jongwon Park ◽  
Bidyut Biswas ◽  
...  
Keyword(s):  
Organic Solvents ◽  
Liquid Crystalline ◽  
Average Molecular Weight ◽  
Pyridinium Salt ◽  
Emission Spectra ◽  
Ionic Polymers ◽  
Scanning Calorimetry ◽  
Light Emitting ◽  
Chemical Structures ◽  
Nonpolar Organic

A series of poly(pyridinium salt)s-fluorene main-chain ionic polymers with various organic counterions were synthesized by using ring-transmutation polymerization and metathesis reactions. Their chemical structures were characterized by Fourier Transform Infrared (FTIR), proton (1H), and fluorine 19 (19F) nuclear magnetic resonance (NMR) spectrometers. These polymers showed a number-average molecular weight (Mns) between 96.5 and 107.8 kg/mol and polydispersity index (PDI) in the range of 1.12–1.88. They exhibited fully-grown lyotropic phases in polar protic and aprotic solvents at different critical concentrations. Small-angle X-ray scattering for one polymer example indicates lyotropic structure formation for 60–80% solvent fraction. A lyotropic smectic phase contains 10 nm polymer platelets connected by tie molecules. The structure also incorporates a square packing motif within platelets. Thermal properties of polymers were affected by the size of counterions as determined by differential scanning calorimetry and thermogravimetric analysis measurements. Their ultraviolet-visible (UV-Vis) absorption spectra in different organic solvents were essentially identical, indicating that the closely spaced π-π* transitions occurred in their conjugated polymer structures. In contrast, the emission spectra of polymers exhibited a positive solvatochromism on changing the polarity of solvents. They emitted green lights in both polar and nonpolar organic solvents and showed blue light in the film-states, but their λem peaks were dependent on the size of the counterions. They formed aggregates in polar aprotic and protic solvents with the addition of water (v/v, 0%–90%), and their λem peaks were blue shifted.

scholarly journals Thermal and Emission Properties of a Series of Lanthanides Complexes with N-Biphenyl-Alkylated-4-Pyridone Ligands: Crystal Structure of a Terbium Complex with N-Benzyl-4-Pyridone

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2017
Author(s):  
Florentina L. Chiriac ◽  
Monica Iliş ◽  
Augustin Madalan ◽  
Doina Manaila-Maximean ◽  
Mihail Secu ◽  
...  
Keyword(s):  
Lanthanide Complexes ◽  
Liquid Crystalline ◽  
Parent Compound ◽  
Emission Spectra ◽  
Lanthanide Ions ◽  
X Ray Diffraction ◽  
Terbium Complex ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Chemical Structures

This work focuses on the investigation of the liquid crystalline behavior and luminescence properties of the lanthanide complexes of Eu(III), Sm(III) and Tb(III) with N-biphenyl-alkylated-4-pyridone ligands. The organic ligands having a biphenyl group attached via a long flexible spacer with either 9 or 10 carbon atoms were synthesized by the reaction between 4-hydroxypyridine and the corresponding bromide compounds. The chemical structures of the organic and lanthanide complexes were assigned based on elemental analysis, single-crystal X-ray diffraction, 1H, 13C NMR and IR spectroscopies, and thermogravimetric analysis (TGA). The X-ray diffraction analysis of a parent compound shows that the lanthanide ions are surrounded by three monodentate pyridone ligands and three bidentate nitrate ions, giving a 9-coordinate environment. The mesogenic behavior and the type of liquid crystalline phases exhibited by the new complexes were analyzed by differential scanning calorimetry (DSC) and polarizing optical microscopy (POM), and powder X-ray diffraction (XRD) studies. Only the lanthanide complexes with longer spacer (10) display a monotropic SmA phase, typically on a short thermal range (less than 10 °C). The complexes with shorter flexible chains (9) show no liquid crystalline properties with melting temperatures lower than their analogs with longer spacers. The emission spectra recorded in solid state at room temperatures show typical emission bands for each lanthanide ion employed (Eu(III), Tb(III) and Sm(III)).

Synthesis and Characterization of Bowl-Shaped Liquid Crystals with a Core of Calix[6]arene

2011 ◽  
Vol 396-398 ◽  
pp. 2202-2205
Author(s):  
Dan Shu Yao ◽  
Feng Li ◽  
Hao Jie Wang ◽  
Xiao Yun Li ◽  
Mei Tian ◽  
...  
Keyword(s):  
Liquid Crystals ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Cholesteric Phase ◽  
Chemical Structures ◽  
Liquid Crystalline Phases ◽  
Clearing Temperature ◽  
Mesomorphic Properties

A new kind of bowl-shaped liquid crystals were designed and synthesized by esterification. They used a calix[6]arene as central unit and ω- cholesteric alkyl diacid monoester as mesogenic arms. Their chemical structures were confirmed by FTIR and 1HNMR spectra, their mesomorphic properties and phase behavior were investigated by differential scanning calorimetry (DSC), polarizing optical microscopy (POM) and X-Ray Diffraction (XRD) measurements. The results showed that the kind of calix[6]arene bowl-shaped liquid crystals N1-N3 exhibited broad range liquid crystalline phases at moderate temperature, and they displayed cholesteric phase focal-conic texture in liquid crystal states. With increasing the flexibility of monomers M1-M3, the melting point and the clearing temperature decreased in the macromolecules.

Liquid crystalline polyureas with oligo(ethylene glycol) sequences

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi
Keyword(s):  
Liquid Crystalline ◽  
Spectroscopic Method ◽  
Polymerization Reaction ◽  
X Ray Diffraction ◽  
Subsequent Reaction ◽  
Scanning Calorimetry ◽  
Polar Solvents ◽  
X Ray ◽  
H Nmr ◽  
Ft Ir

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.

Synthesis and Properties of Thermotropic Liquid Crystalline Polyesters with Flexible Polymethylene Spacer

2010 ◽  
Vol 428-429 ◽  
pp. 126-131
Author(s):  
Wei Zhong Lu ◽  
Chun Wei ◽  
Qui Shan Gao
Keyword(s):  
Optical Microscopy ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Structure Morphology ◽  
Temperature Ranges ◽  
Ft Ir ◽  
Diffraction Peaks ◽  
Ubbelohde Viscometer

Polymethylene bis(p-hydroxybenzoates) were prepared from methyl p-hydroxybenzoate and different diols by melted transesterification reaction. Three liquid crystalline polyesters were synthesized from terephthaloyl dichloride and polymethylene bis(p-hydroxybenzoates). Its structure, morphology and properties were characterized by Ubbelohde viscometer, Fourier transform infrared spectroscopy (FT-IR), Differential scanning calorimetry (DSC), polarized optical microscopy (POM) with a hot stage, and wide-angle X-ray diffraction (WAXD). Results indicated that the intrinsic viscosities were between 0.088 and 0.210 dL/g. Optical microscopy showed that the TLCP has a highly threaded liquid crystalline texture and a high birefringent schlieren texture character of nematic phase and has wider mesophase temperature ranges for all polyesters. DSC analysis were found that the melting point (Tm), isotropic temperature (Ti) of TLCPs decreased and the temperature range of the liquid crystalline phase became wider with increased number of methylene spacers in the polyester. The WAXD results showed that TLCPs owned two strong diffraction peaks at 2θ near 19° and 23°.

scholarly journals Synthesis and mesomorphic properties of calamitic malonates and cyanoacetates tethered to 4-cyanobiphenyls

2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat
Keyword(s):  
Differential Scanning Calorimetry ◽  
Ambient Temperature ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Cyanoacetic Acid ◽  
Scanning Calorimetry ◽  
Isotropic Liquid ◽  
X Ray ◽  
Nematic Phases ◽  
Mesomorphic Properties

4-Cyano-1,1'-biphenyl derivatives bearing ω-hydroxyalkyl substituents were reacted with methyl 3-chloro-3-oxopropionate or cyanoacetic acid, giving liquid-crystalline linear malonates and cyanoacetates. These compounds formed monotropic nematic phases at 62 °C down to ambient temperature upon cooling from the isotropic liquid. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction (WAXS).

Thermotropic behavior of sodium cholesteryl carbonate

2009 ◽  
Vol 24 (1) ◽  
pp. 156-163 ◽  
Author(s):  
Rabkwan Chuealee ◽  
Timothy S. Wiedmann ◽  
Teerapol Srichana
Keyword(s):  
Phase Behavior ◽  
Chemical Structure ◽  
Liquid Crystalline ◽  
Polarized Light ◽  
Wave Number ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
X Ray Scattering ◽  
C Nmr

Sodium cholesteryl carbonate ester (SCC) was synthesized, and its phase behavior was studied. The chemical structure was assessed by solid-state infrared spectroscopy based on vibration analysis. The wave number at 1705 and 1276 cm−1 corresponds to a carbonyl carbonate and O–C–O stretching of SCC, respectively. Molecular structure of SCC was further investigated with 1H and 13C NMR spectroscopy. The chemical shift, for the carbonyl carbonate resonance appeared at 155.5 ppm. A molecular mass of SCC was at m/z of 452. Differential scanning calorimetry (DSC), video-enhanced microscopy (VEM) together with polarized light microscopy, and small-angle x-ray scattering (SAXS) were used to characterize the phase behavior as a function of temperature of SCC. Liquid crystalline phase was formed with SCC. Based on the thermal properties and x-ray diffraction, it appears that SCC forms a structure analogous to the type II monolayer structure observed with cholesterol esters.

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