Liquid crystalline polyureas with oligo(ethylene glycol) sequences

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi

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.

2010 ◽  
Vol 428-429 ◽  
pp. 126-131
Author(s):  
Wei Zhong Lu ◽  
Chun Wei ◽  
Qui Shan Gao

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°.


2021 ◽  
Vol 1 (1) ◽  
Author(s):  
Badia Imene Cherifi ◽  
Mohammed Belbachir ◽  
Abdelkader Rahmouni

AbstractIn this work, the green polymerization of vinyl acetate is carried out by a new method which consists in the use of clay called Maghnite-Na+ as an ecological catalyst, non-toxic, inexpensive and recyclable by simple filtration. X-ray diffraction (XRD) showed that Maghnite-Na+ is successfully obtained after cationic treatment (sodium) on raw Maghnite. It is an effective alternative to replace toxic catalysts such as benzoyl peroxide (BPO) and Azobisisobutyronitrile (AIBN) which are mostly used during the synthesis of polyvinyl acetate (PVAc) making the polymerization reaction less problematic for the environment. The synthesis reaction is less energetic by the use of recycled polyurethane as container for the reaction mixture and which is considered as a renewable material and a good thermal insulator which maintains the temperature at 0 °C for 6 h. The reaction in bulk is also preferred to avoid the use of a solvent and therefore to stay in the context of green chemistry. In these conditions, the structure of obtained polymer is established by Nuclear Magnetic Resonance Spectroscopy 1H NMR and 13C NMR. Infrared spectroscopy (FT-IR) is also used to confirm the structure of PVAc. Thermogravimetric analysis (TGA) showed that it is thermally stable and it starts to degrade from 330 °C while Differential Scanning calorimetry (DSC) shows that this polymer has a glass transition temperature (Tg  = 50 °C). The composition in PVAc/Maghnite-Na+ (7 wt% of catalyst) is the most tensile resistant with a force of 182 N and a maximum stress of 73.16 MPa, the most flexible (E  = 955 MPa) and the most ductile (εr  = 768%).


2021 ◽  
Vol 15 (2) ◽  
pp. 183-190
Author(s):  
Badia Imene Cherifi ◽  
◽  
Mohammed Belbachir ◽  
Souad Bennabi ◽  
◽  
...  

In this work, the green polymerization of vinyl acetate is carried out by a new method which consists in the use of clay called Maghnite-Na+ as an ecological catalyst, non-toxic, inexpensive and recyclable by a simple filtration. X-ray diffraction and scanning electron microscopy showed that Maghnite-Na+ is successfully obtained after cationic treatment (sodium) on crude maghnite. It is an effective alternative to replace toxic catalysts such as benzoyl peroxide and azobisisobutyronitrile which are mostly used during the synthesis of polyvinyl acetate (PVAc) making the polymerization reaction less problematic for the environment. The synthesis reaction is less energetic by the use of recycled polyurethane as a container for the reaction mixture and is considered as a renewable material and a good thermal insulator maintaining the temperature of 273 K for 6 h. The reaction in bulk is also preferred to avoid the use of a solvent and therefore to stay in the context of green chemistry. In these conditions, the structure of obtained polymer is established by 1H NMR and 13C NMR. Infrared spectroscopy (FT-IR) was also used to confirm the structure of PVAc. Thermogravimetric analysis showed that it is thermally stable and starts to degrade at 603 K while differential scanning calorimetry showed that this polymer has a glass transition temperature Tg of 323 K.


2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat

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).


2009 ◽  
Vol 24 (1) ◽  
pp. 156-163 ◽  
Author(s):  
Rabkwan Chuealee ◽  
Timothy S. Wiedmann ◽  
Teerapol Srichana

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.


1990 ◽  
Vol 45 (7) ◽  
pp. 1084-1090 ◽  
Author(s):  
Klaus Praefcke ◽  
Bernd Kohne ◽  
Andreas Eckert ◽  
Joachim Hempel

Six S,S-dialkyl acetals 2a-f of inosose (1), tripodal in structure, have been synthesized, characterized and investigated by optical microscopy and differential scanning calorimetry (d.s.c.). The four S,S-acetals 2c-f with sufficiently long alkyl chains are thermotropic liquid crystalline; 2 e and 2 f are even dithermomesomorphic. Each of these four inosose derivatives 2c-f exhibits monotropically a most likely cubic mesophase (MI); in addition 2e and 2f show enantiotropically a hexagonal mesophase (Hx) with a non-covalent, supramolecular H-bridge architecture. Whereas the nature of the optically isotropic mesophase MI needs further clarification the stable high temperature mesophase Hx of 2 e and 2 f has been established by a miscibility test using a sugar S,S-dialkyl acetal also tripodal in structure and with a Hx phase proved by X-ray diffraction, but in contrast to 2 with an acyclic hydrophilic part. Similarities of structural features between the Hx-phases of 2e and 2f as well as of other thermotropic and lyotropic liquid crystal systems are discussed briefly.


2018 ◽  
Vol 2018 ◽  
pp. 1-10
Author(s):  
Monica Iliş ◽  
Viorel Cîrcu

Mesomorphic three-coordinate copper(I) complexes ([Cu(BTU)2X], where X = Cl or Br) based on a new N-benzoylthiourea (BTU) ligand with two decyloxy and one perfluorooctyl groups at its periphery were designed and prepared. The BTU ligand coordinates via the S atom in a neutral monodentate fashion as confirmed by IR and NMR spectroscopy data. The liquid crystalline behavior of these copper(I) complexes was investigated by a combination of polarized optical microscopy (POM), differential scanning calorimetry (DSC), and X-ray diffraction analysis (XRD), while their thermal stability was studied by thermogravimetric analysis (TGA). These new copper(I) complexes have mesomorphic properties and exhibit a hexagonal columnar mesophase over a large temperature range, more than 100°C.


2018 ◽  
Vol 73 (6) ◽  
pp. 369-375 ◽  
Author(s):  
Farzin Marandi ◽  
Keyvan Moeini ◽  
Fereshteh Alizadeh ◽  
Zahra Mardani ◽  
Ching Kheng Quah ◽  
...  

AbstractA mixed ligand zinc coordination polymer, {Zn(μ-DPE)(DBM)2}n (1) (HDBM: dibenzoylmethane and DPE: (E)-1,2-di(pyridin-4-yl)ethene), was prepared and identified by elemental analysis, FT-IR, 1H NMR spectroscopy and single-crystal X-ray diffraction. In the 1D linear coordination polymer of 1, the zinc atom has a ZnN2O4 environment with octahedral geometry. These complex units are linked by the bridging of the planar N2 donor DPE ligands. In the coordination network of complex 1, in addition to the hydrogen bonds, the network is more stabilized by π–π stacking interactions between pyridine and β-diketone moieties of the ligands. These interactions increase the ability of the compound to interact with biomacromolecules (BRAF kinase, CatB, DNA gyrase, HDAC7, rHA, RNR, TrxR, TS and Top II) as investigated by docking calculations.


2020 ◽  
Vol 856 ◽  
pp. 190-197
Author(s):  
Pornsit Chaiya ◽  
Thawatchai Phaechamud

Compatibility investigation was performed between magnesium stearate and acidic drug compounds (ibuprofen, indomethacin and valproic acid) and acidic pharmaceutical excipients (lactic acid and citric acid) using differential scanning calorimetry (DSC). DSC study indicated the possible incompatibility for the mixture between magnesium stearate and any compounds. Alteration in DSC thermogram was found in all mixtures. The eutectic phenomenon was found in the powder mixture of magnesium stearate and ibuprofen. In addition, the presence of melting endothermic peak of stearic acid in other powder mixtures except the mixture of magnesium stearate and indomethacin indicating breakage of salt form of magnesium stearate. This alteration could relate to the influence on physicochemical properties of drug compounds and pharmaceutical excipients which powder x-ray diffraction (PXRD) and Fourier Transform Infrared Spectroscopy (FT-IR) should be further analyzed to confirm the interactions between compounds.


Coatings ◽  
2018 ◽  
Vol 8 (9) ◽  
pp. 305 ◽  
Author(s):  
Yan Zhang ◽  
Hui Zhang ◽  
Fang Wang ◽  
Li-Xia Wang

The ginger essential oil/β-cyclodextrin (GEO/β-CD) composite, ginger essential oil/β-cyclodextrin/chitosan (GEO/β-CD/CTS) particles and ginger essential oil/β-cyclodextrin/chitosan (GEO/β-CD/CTS) microsphere were prepared with the methods of inclusion, ionic gelation and spray drying. Their properties were studied by using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermo-gravimetry analysis (TGA), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The results showed that the particle size of GEO/β-CD composite was smaller than that of β-CD and GEO/β-CD/CTS particles were loose and porous, while the microsphere obtained by spray drying had certain cohesiveness and small particle size. Besides, results also indicated that β-CD/CTS could modify properties and improve the thermal stability of GEO, which would improve its application value in food and medical industries.


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