scholarly journals Original Macromolecular Architectures Based on poly(ε-caprolactone) and poly(ε-thiocaprolactone) Grafted onto Chitosan Backbone

2018 ◽  
Vol 19 (12) ◽  
pp. 3799 ◽  
Author(s):  
Cüneyt Ünlü ◽  
Eric Pollet ◽  
Luc Avérous
Keyword(s):  
Ring Opening ◽  
Ring Opening Polymerization ◽  
Hexamethylene Diisocyanate ◽  
Proton Nuclear Magnetic Resonance ◽  
High Yield ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Molar Ratios ◽  
Grafting Onto

Polyester and/or polythioester grafted chitosan copolymers were synthesized. For that, poly(ε-caprolactone) (PCL), poly(ε-thiocaprolactone) (PTCL), and their copolymers were first synthesized by ring opening polymerization. Copolymers with caprolactone:thiocaprolactone (CL:TCL) molar ratios of 2:1, 1:1, 1:2 were synthesized. All of the synthesized macromolecular architectures were characterized using different spectral (Fourier transform infrared (FTIR), proton nuclear magnetic resonance (1H-NMR), X-Ray diffraction (XRD)) and thermal (Differential scanning calorimetry (DSC), Thermogravimetric analysis (TGA)) methods. Grafting was then performed according two distinct routes: (i) using a blend of both homopolymers (PCL and PTCL) or (ii) using pre-synthesized copolymers with controlled CL:TCL ratios. Hexamethylene diisocyanate was used as a grafting/coupling agent through urethane bonds with high yield. Grafting preferentially occurred at sulfur sites. The results indicated that PTCL is more reactive and favorable than PCL for grafting onto chitosan. With the homopolymers blend grafting route, the corresponding materials mostly had a higher PTCL portion than expected. To obtain polyester grafted chitosan with a determined CL:TCL ratio, the copolymer grafting route would yield better results.

Synthesis, characterization, and structures of zircona- and boracyclosiloxanes with ferrocenyl substituents

2002 ◽  
Vol 80 (11) ◽  
pp. 1469-1480 ◽  
Author(s):  
Karena Thieme ◽  
Sara C Bourke ◽  
Juan Zheng ◽  
Mark J MacLachlan ◽  
Fojan Zamanian ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Differential Scanning Calorimetry ◽  
Thermogravimetric Analysis ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
The Novel ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy

The novel zirconatetraferrocenylcyclotrisiloxane Cp2Zr(OSiFc2)2O (6), dizirconatetraferrocenylcyclotetrasiloxane [Cp2Zr(OSiFc2)O]2 (7), boratetraferrocenylcyclotrisiloxane (C6H5)B(OSiFc2)2O (8), and diboratetraferrocenylcyclotetrasiloxane [(C6H5)B(OSiFc2)O]2 (9) with ferrocenyl (Fc = Fe(η-C5H4)(η-C5H5)) substituents at silicon have been prepared from the reactions of Cp2Zr(NMe2)2 and PhBCl2 with diferrocenylsilanediol Fc2Si(OH)2 (3) and tetraferrocenyldisiloxanediol [Fc2SiOH]2O (5). The compounds were characterized by mass spectrometry, elemental analysis, UV–vis, IR, Raman, and multinuclear NMR spectroscopy, as well as single crystal X-ray diffraction. Thermogravimetric analysis and differential scanning calorimetry investigation of 6–9 showed that the cycles decompose before they can undergo any thermal ring-opening polymerization. In addition, no polymerization was detected in the presence of either KOSiMe3 or HOTf. The bulky ferrocenyl substituents on the Si atoms are likely to be at least partially responsible for the inability of these heterocycles to undergo ring-opening polymerization. Key words: heterocyclosiloxanes, ferrocenyl.

Novel surface treatment for natural fiber composites

2017 ◽  
Vol 31 (16-19) ◽  
pp. 1744092 ◽  
Author(s):  
Wendy Zhang ◽  
Xiaowen Yuan
Keyword(s):  
Ring Opening ◽  
Natural Fiber ◽  
Fiber Composites ◽  
Proton Nuclear Magnetic Resonance ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Dsc Studies ◽  
Flax Fibers ◽  
H Nmr

Poly(lactide) (PLA) — flax fibers stereocomplex composites were prepared by casting commercial poly(L-lactide) (PLA) and flax-g-poly(D-lactide) (flax-g-PDLA), where flax-g-PDLA was synthesized via ring-opening polymerization. Successful surface grafting was revealed by Proton Nuclear Magnetic Resonance (1H NMR) spectroscopy, wide angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC) studies. DSC results showed that stereocomplex crystallites formed between the PLA matrix and flax-g-PDLA, resulting in good fiber/PLA interfacial adhesion.

Synthesis and properties of polyimides from 1,4-bis(4-amino-2-phenylphenoxy) benzene and 4,4′-bis(4-amino-2-phenylphenoxy) biphenyl

2012 ◽  
Vol 24 (8) ◽  
pp. 783-792 ◽  
Author(s):  
Atsushi Morikawa ◽  
Fumi Miyata ◽  
Jun Nishimura
Keyword(s):  
Ring Opening ◽  
Mechanical Analysis ◽  
Ring Opening Polymerization ◽  
Dielectric Constants ◽  
Structure Property ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Structure Property Relationships ◽  
Step Procedure

Diamines, namely, 1,4-bis(4-amino-2-phenylphenoxy) benzene (1) and 4,4′-bis(4-amino-2-phenylphenoxy) biphenyl (2), were synthesized from 4-fluoro-3-phenyl nitrobenzene. Two series of polyimides were synthesized from these diamines with nine types of dianhydrides by a conventional two-step procedure that included ring-opening polymerization in N-methyl-2-pyrrolidone and subsequent thermal cyclic dehydration. The polyimides were characterized by x-ray diffraction, differential scanning calorimetry, thermogravimetry and dynamic mechanical analysis. The polyimides from 1 and 2 had a glass transition temperature in the range of 221–254°C and 222–271°C, respectively, and all the polymers were amorphous. The structure–property relationships of these polyimides were examined and compared with those of the previously prepared analogous polyimides from the bis(4-amino-2-biphenyl)ether (3). Water absorption and dielectric constants ( ∊) of the polyimides were compared and discussed on the basis of imide content per repeating unit.

The synthesis and polymerization behaviour of silicon-bridged [1]- and [2]ferrocenophanes with sterically demanding trimethylsilyl substituents attached to the cyclopentadienyl rings

1995 ◽  
Vol 73 (11) ◽  
pp. 2069-2078 ◽  
Author(s):  
Timothy J. Peckham ◽  
Daniel A. Foucher ◽  
Alan J. Lough ◽  
Ian Manners
Keyword(s):  
Molecular Weight ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
Monoclinic Space Group ◽  
Organometallic Polymers ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cyclopentadienyl Ligands ◽  
Sterically Demanding ◽  
High Molecular Weight Poly

The silicon-bridged [1]ferrocenophane Fe(η-C5H3SiMe3)2(SiMe2) (5) was synthesized via the reaction of Li2[Fe(η-C5H3SiMe3)2]•tmeda (tmeda = tetramethylethylenediamine) with Me2SiCl2 in hexanes. The disilane-bridged [2]ferrocenophane Fe(η-C5H3SiMe3)2(Si2Me4) (7) was prepared using a similar route from the disilane ClMe2SiSiMe2Cl. Despite the presence of sterically demanding SiMe3 substituents on the cyclopentadienyl rings, compound 5 was found to undergo thermal ring-opening polymerization at 170 °C to produce very soluble, high molecular weight poly(ferrocenylsilane) 6 with Mw = 1.4 × 105, Mn = 8.4 × 104. However, the [2]ferrocenophane 7 was found to be resistant to thermal ring-opening polymerization even at 350 °C and decomposed above 380 °C. A single-crystal X-ray diffraction study of 7 revealed that the steric interactions between the bulky SiMe3 groups are relieved by a significant twisting of the disilane bridge with respect to the plane defined by the centroids of the cyclopentadienyl ligands and the metal atom. The angle between the planes of the cyclopentadienyl rings in 7 was found to be 5.4(6)°, slightly greater than that in the non-silylated analogue Fe(η-C5H4)2(Si2Me4) (4a) (4.19(2)°), and dramatically less than the corresponding tilt angle of the strained, polymerizable, silicon-bridged [1]ferrocenophane Fe(η-C5H4)2(SiMe2) (1) (20.8(5)°). The length of the Si—Si bond in 7 (2.342(3) Å) was found to be close to the sum of the covalent radii (2.34 Å). Crystals of 7 are monoclinic, space group C2/c, with a = 23.689(3) Å, b = 11.174(1) Å, c = 31.027(3) Å, β = 109.16(1)°, V = 7758(2) Å3, and Z = 12. Keywords: ring-opening polymerization, ferrocenophane, organometallic polymers.

Synthesis, Characterization and Optical Properties of PLA / P3HT Blends Thin Films

2021 ◽  
Vol 19 (5) ◽  
pp. 132-138
Author(s):  
Maan Abd-Alameer Salih ◽  
Q.S. Kareem ◽  
Mohammed Hadi Shinen
Keyword(s):  
Thin Films ◽  
Optical Properties ◽  
Spin Coating ◽  
Ring Opening ◽  
Energy Gap ◽  
Ring Opening Polymerization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Conductivity Increase ◽  
Ft Ir

In this exploration Poly lactic corrosive (PLA) was orchestrated the ring-opening polymerization Poly lactic corrosive (PLA) blended with poly(3-hexylthiophene) (P3HT) which prepared by solution. Blends thin films Synthesis by spin coating technique and using Tetrahydrofuran (THF) as solvent. PLA powder was 'characterized by' 'X-ray' 'diffraction', '(FT-IR)'. pure Optical properties (PLA), (PLA)/P3HT blends thin films with different percentage of P3HT (0, 1, 2, and 3) wt% were investigated using UV-VS spectroscopy The results showed that the absorption, absorption coefficient, extinction coefficient and conductivity increase with increasing the rate of deformation P3HT, The energy gap decreases with increasing deformation.

The Effect of Sample Substrate on the Structural Properties of Co-Deposited Films of A-Ge:H

1990 ◽  
Vol 192 ◽  
Author(s):  
S.J. Jones ◽  
W.A. Turner ◽  
D. Pang ◽  
W. Paul
Keyword(s):  
Yield Strength ◽  
Crystallization Process ◽  
Exothermic Peak ◽  
High Yield ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Strength Differential ◽  
Substrate Temperatures ◽  
Deposited Films

ABSTRACTResults from structural measurements on r.f. glow discharge produced a-Ge:H films have been found to be substrate dependent. The variations in the results were found to depend on both the substrate temperature, Ts, and the substrate yield strength. Differential scanning calorimetry results were particularly affected by these parameters. For films prepared at Ts = 150°C, the DSC spectra contain two exothermic peaks when the films are deposited on low yield strength substrates while only one exothermic peak is present for films deposited on high yield strength substrates. One exothermic DSC peak is seen in spectra for all films prepared at Ts = 300°C no matter what substrates were used. This DSC spectral dependence is attributed to differences in the microstructure of films deposited at the two substrate temperatures, as seen in TEM micrographs. X-ray diffraction measurements performed on films annealed to various temperatures show that all of the exothermic DSC peaks described above are associated with the crystallization process. Thus, for the films prepared at low Ts, crystallization is either a one or two step process depending on the yield strength of the substrate.

scholarly journals Yttrium and Lithium Keto-β-Diketiminate Complexes [{2,6-Me2C6H3N=C(Me)}2CС(tert-Bu)=O]2Y(μ2-Cl)2Li(THF)2 and {[{2,6-Me2C6H3N=C(Me)}2CС(tert-Bu)=O]Li(THF)}n. Synthesis, Molecular Structures, and Catalytic Activity in ε-Caprolactone Polymerization

2021 ◽  
Vol 47 (2) ◽  
pp. 144-154
Author(s):  
G. G. Skvortsov ◽  
A. V. Cherkasov ◽  
D. L. Vorozhtsov ◽  
E. S. Shchegravina ◽  
A. A. Trifonov
Keyword(s):  
Catalytic Activity ◽  
Diffraction Analysis ◽  
Exchange Reaction ◽  
Ring Opening ◽  
Crystalline State ◽  
Ring Opening Polymerization ◽  
Molecular Structures ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray

Abstract The reaction of lithium β-diketiminate [{2,6-Me2C6H3N=CMe}2CH]Li with benzophenone in toluene at 25°C affords the coordination complex [{2,6-Me2C6H3N=CMe}2CH]Li(Ph2C=O) (I). New keto-β-diketimine {2,6-Me2C6H3N=C(Me)}2CHC(tert-Bu)=O (II) is synthesized by the reaction of tert-Bu(C=O)Cl with [{2,6-Me2C6H3N=CMe}2CH]Li. The metallation of keto-β-diketimine II with n-butyllithium in THF at 0°C gives lithium keto-β-diketiminate {[{2,6-Me2C6H3N=C(Me)}2CС(tert-Bu)=O]Li(THF)}n (III). The exchange reaction of YCl3 with compound III (molar ratio 1 : 2, THF) affords the yttrium bis(keto-diketiminate) complex [{2,6-Me2C6H3N=C(Me)}2CС(tert-Bu)=O]2Y(μ2-Cl)2L-(THF)2 (IV). The molecular structures of complexes I, III, and IV are determined by X-ray diffraction analysis (CIF files CCDC nos. 2001131 (I), 2001132 (III), and 2001133 (IV)). Complex IV in the crystalline state exists as an ate complex with one LiCl molecule. Complexes I, III, and IV are catalysts of ring-opening polymerization of ε-caprolactone in toluene at 25°С.

scholarly journals Preparation and Application of Polyurethane Coating Material Based on Epoxycyclohexane-Tetrahydrofuran in Paper Conservation

Coatings ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 1143
Author(s):  
Juan Liu ◽  
Shan-Shan Jin ◽  
Ying-Ping Qi ◽  
Yong-Feng Shen ◽  
Hua Li
Keyword(s):  
Ring Opening ◽  
Ring Opening Polymerization ◽  
Hexamethylene Diisocyanate ◽  
Proton Nuclear Magnetic Resonance ◽  
Cultural Resources ◽  
Historical Records ◽  
The World ◽  
Folding Endurance ◽  
Paper Conservation ◽  
1Hnmr Spectroscopy

Paper cultural heritages are valuable historical records and also abound in cultural resources. Due to its organic property, paper is susceptible to aging, destruction by environmental pollution and human factors. At present, many countries in the world are facing the problem of paper conservation. Coating reinforcement is one of the methods for paper conservation, in which the choice of reinforcing resin is key. A transparent polyurethane, based on epoxycyclohexane (CHO)-tetrahydrofuran (THF) copolyether, was adopted in this study. The ring-opening polymerization for generating the CHO-THF copolyether took place by the reactants CHO and THF, in the catalysis of boron trifluoride diethyl etherate, initiation of glycerol. Characterizations of the synthetic copolyether were conducted by infrared (IR) spectroscopy and proton nuclear magnetic resonance (1HNMR) spectroscopy. The transparent polyurethane was then produced by the CHO-THF copolyether and hexamethylene diisocyanate (HDI) trimer. The influences of different concentrations of polyurethane solution upon the paper tensile strength, elongation, folding endurance, tearing strength, gloss, and brightness were studied. These findings suggest that 10% polyurethane solution is optimal, not only for greatly improving the paper performance, but also for keeping with the principle of “repair as old”. The applied results demonstrate that the polyurethane based on the CHO-THF copolyether has the characteristics of copolyether along with polyurethane, displaying good mechanical properties in paper reinforcement.

Grafting Polymerization of D,L-Lactide on the Surface of Halloysite Nanotubes

2013 ◽  
Vol 275-277 ◽  
pp. 1742-1745 ◽  
Author(s):  
Jing Jing Li ◽  
Bing Hong Luo ◽  
Jin Xi Zhang ◽  
Ru Qiu Huo ◽  
Chang Ren Zhou
Keyword(s):  
Ring Opening ◽  
Halloysite Nanotubes ◽  
Ring Opening Polymerization ◽  
Gravimetric Analysis ◽  
Structure And Properties ◽  
Thermal Gravimetric ◽  
X Ray Diffraction ◽  
Potential Measurement ◽  
X Ray ◽  
Before And After

Halloysite nanotubes (HNTs) surface-grafting poly(D,L-lactide) (g-HNTs) were synthesized by bulk ring-opening polymerization of D,L-lactide using stannous octoate as catalyst and HNTs as co-initiator. Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and zeta potential measurement were employed to elucidate the structure and properties of HNTs before and after grafting with D,L-lactide. FTIR spectrum certified the existence of poly(D,L-lactide) chains on the surface of g-HNTs. The amount of surface-grafted poly(D,L-lactide) measured by TGA was 4.6% in weight. The grafted poly(D,L-lactide) chains on the surfaces of HNTs can relieve the clustering effect of HNTs to some extents.

Investigation of α-amino acid N-carboxyanhydrides by X-ray diffraction for controlled ring-opening polymerization

2019 ◽  
Vol 60 (3) ◽  
pp. 272-275 ◽  
Author(s):  
Olga Schäfer ◽  
Dieter Schollmeyer ◽  
Alexander Birke ◽  
Regina Holm ◽  
Kerstin Johann ◽  
...  
Keyword(s):  
Amino Acid ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
X Ray Diffraction ◽  
X Ray
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