scholarly journals Environmental Profile and Technological Validation of New High-Tg Unsaturated Polyesters from Fully Bio-Based Monomers and Reactive Diluents

2020 ◽  
Author(s):  
Raffaella Suriano ◽  
Maria Nelly Garcia Gonzalez ◽  
Stefano Turri
Keyword(s):  
Unsaturated Polyester ◽  
Gel Permeation Chromatography ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Positive Effects ◽  
Reactive Diluents ◽  
Composite Polymers ◽  
Category Indicator ◽  
Monomer Feed

Abstract This study was focused on the synthesis and characterization of a fully bio-based unsaturated polyester resin (UPR) with good thermal properties suitable for the commercial production of composite polymers. UPRs based on different ratios of bio-based furan dicarboxylic acid (FDCA), itaconic acid, and diols were synthesized. The unsaturated polymers prepared were evaluated by differential scanning calorimetry, gel permeation chromatography, FTIR and 1H-NMR spectroscopy. The results showed positive effects of FDCA on the glass transition temperature (Tg) of these fully bio-based polyesters, especially when FDCA was combined with 1,2-propanediol. Optimal values of Tg were obtained in the range of 30–32 °C for UPRs synthesized starting with a higher concentration of FDCA in the monomer feed. The possibility of substituting styrene, which usually acts as a reactive diluent, with a greener and safer alternative during the crosslinking of UPRs, was also explored. Two bio-based reactive diluents were considered: dimethyl itaconate (DMI) and butanediol dimethacrylate. After crosslinking, an average Tg of 75 °C and a good crosslinking efficiency indicated by a gel content of 90% were achieved for the fully bio-based polyester obtained under milder reaction conditions and dilution with DMI. Life cycle assessment was performed on selected UPRs, and comparison with a reference fossil-based resin in terms of the calculated category indicator results confirmed the lower environmental impact of the newly prepared bio-based polyesters.

Characterization of bi-layered magnetic nanoparticles synthesized via two-step surface-initiated ring-opening polymerization

2015 ◽  
Vol 87 (11-12) ◽  
pp. 1085-1097 ◽  
Author(s):  
Li Wang ◽  
Stefan Baudis ◽  
Karl Kratz ◽  
Andreas Lendlein
Keyword(s):  
Magnetic Nanoparticles ◽  
Ring Opening ◽  
Average Molecular Weight ◽  
Polymer Networks ◽  
Gel Permeation Chromatography ◽  
Degree Of Crystallinity ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Transmission Electron

AbstractA versatile strategy to integrate multiple functions in a polymer based material is the formation of polymer networks with defined nanostructures. Here, we present synthesis and comprehensive characterization of covalently surface functionalized magnetic nanoparticles (MNPs) comprising a bi-layer oligomeric shell, using Sn(Oct)2 as catalyst for a two-step functionalization. These hydroxy-terminated precursors for degradable magneto- and thermo-sensitive polymer networks were prepared via two subsequent surface-initiated ring-opening polymerizations (ROPs) with ω-pentadecalactone and ε-caprolactone. A two-step mass loss obtained in thermogravimetric analysis and two distinct melting transitions around 50 and 85°C observed in differential scanning calorimetry experiments, which are attributed to the melting of OPDL and OCL crystallites, confirmed a successful preparation of the modified MNPs. The oligomeric coating of the nanoparticles could be visualized by transmission electron microscopy. The investigation of degrafted oligomeric coatings by gel permeation chromatography and 1H-NMR spectroscopy showed an increase in number average molecular weight as well as the presence of signals related to both of oligo(ω-pentadecalactone) (OPDL) and oligo(ε-caprolactone) (OCL) after the second ROP. A more detailed analysis of the NMR results revealed that only a few ω-pentadecalactone repeating units are present in the degrafted oligomeric bi-layers, whereby a considerable degree of transesterification could be observed when OPDL was polymerized in the 2nd ROP step. These findings are supported by a low degree of crystallinity for OPDL in the degrafted oligomeric bi-layers obtained in wide angle X-ray scattering experiments. Based on these findings it can be concluded that Sn(Oct)2 was suitable as catalyst for the preparation of nanosized bi-layered coated MNP precursors by a two-step ROP.

Synthesis and Characterization of Poly (L-Lactic acid) Containing the Azobenzene Mesogens

2011 ◽  
Vol 181-182 ◽  
pp. 185-188
Author(s):  
Run Tao Dong ◽  
Qing Bin Xue ◽  
Ling Min Sun ◽  
Quan Xuan Zhang
Keyword(s):  
Lactic Acid ◽  
Optical Rotation ◽  
Gel Permeation Chromatography ◽  
Helical Structure ◽  
Feed Ratio ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
H Nmr ◽  
Azobenzene Mesogens

A series of azobenzene containing group Poly (L-lactic acid) (PLLA) were synthesized by Ring-Opening Polymerization of L-lactide (L-LA) catalysted by Sn (Oct)2initiated by alcohol-OH containing the azobenzene chromophores. Their molecular weights were well controlled by the feed ratio as characterized by Gel Permeation Chromatography (GPC) and1H NMR Spectrometry and agreed well with theoretical values. The thermal properties and liquid crystal phases were investigated by Differential Scanning Calorimetry (DSC), polarized optical microscopy (POM) and X-ray Diffraction (XRS) measurements. Cis-trans photoisomerization behavior of the polymers in the solutions and the films were studied with UV irradiation. By the Circular Dichroism Spectroscopy (CD) characterization of the solutions and films of the polymer, the PLLA segments show huge optical rotation power in helical structure.

Synthesis and Characterization of Polyacrylates Side-Chain Liquid Crystalline Polymer via Atom Transfer Radical Polymerization

2012 ◽  
Vol 535-537 ◽  
pp. 1516-1519
Author(s):  
Ying Gang Jia ◽  
Peng Tian ◽  
Kun Ming Song ◽  
Bao Yan Zhang
Keyword(s):  
Atom Transfer Radical Polymerization ◽  
Radical Polymerization ◽  
Liquid Crystalline ◽  
Gel Permeation Chromatography ◽  
Crystalline Polymer ◽  
Atom Transfer ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
H Nmr

Atom transfer radical polymerization (ATRP) of methacrylate liquid crystal monomer M (4-((4-(2-(acryloyloxy)ethoxy)benzoyl)oxy)phenyl 4-propylbenzoate) was carried out using CuBr/PMDETA complex as catalyst and 2-bromo-2-methyl-propionic acid ester as initiator. The obtained monomer M and polymer P was characterized via infrared spectroscopy and1H NMR. The phase behavior and mesomorphism were investigated by differential scanning calorimetry (DSC), polarizing optical microscopy (POM), and x-ray diffraction (XRD). The molecular weight and the structure of the polymers were identified with gel permeation chromatography and nuclear magnetic resonance.

Synthesis and characterization of 4-chloromethylstyrene polymers containing bulky organosilicon groups

e-Polymers ◽  
2004 ◽  
Vol 4 (1) ◽  
Author(s):  
Kazem Dindar Safa ◽  
Mirzaagha Babazadeh
Keyword(s):  
Differential Scanning Calorimetry ◽  
Glass Transition ◽  
Gel Permeation Chromatography ◽  
Synthesis And Characterization ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Gel Permeation ◽  
Covalently Linked ◽  
C Nmr

Abstract The homopolymer of 4-chloromethylstyrene and its copolymers with styrene (in 1:3 and 1:1 mole ratio) were synthesized by bulk and solution freeradical polymerisations, respectively, at 70±1°C using α,α'-azoisobutyronitrile as an initiator. Highly sterically hindered tris(trimethylsilyl)methyl (Tsi) substituents were then covalently linked to the obtained homopolymer and copolymers. The polymers were characterized by IR, 1H NMR and 13C NMR, differential scanning calorimetry (DSC) and gel permeation chromatography. DSC showed that incorporation of Tsi substituents in the side chains of homopolymer and copolymers increases the rigidity of the polymers and, subsequently, their glass transition temperature.

scholarly journals Synthesis and Characterization of a Multifunctional Conjugated Polymer

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
Emerson C. G. Campos ◽  
Cristiano Zanlorenzi ◽  
Bruno F. Nowacki ◽  
Gabriela M. Miranda ◽  
Denis A. Turchetti ◽  
...  
Keyword(s):  
Conjugated Polymer ◽  
Molar Mass ◽  
Photophysical Properties ◽  
Gel Permeation Chromatography ◽  
Thermal Characterization ◽  
Polymer Structure ◽  
Synthesis And Characterization ◽  
Metallic Ions ◽  
Scanning Calorimetry

This work reports the synthesis and characterization of a conjugated polymer based on fluorene and terpyridine, namely, poly[(9,9-bis(3-((S)-2-methylbutylpropanoate))fluorene-alt-6,6′-(2,2′:6′,2′′-terpyridin-6-yl)] (LaPPS71). The structure was characterized by 1H and 13C nuclear magnetic resonance (NMR) and Fourier-transform infrared (FTIR) spectroscopy. The molar mass was measured by gel permeation chromatography (GPC). As thermal characterization, the glass transition temperature (Tg) was measured by differential scanning calorimetry (DSC). The polymer structure contains two sites capable of complexation with metallic ions, affording the possibility of obtainment of independent or electronically coupled properties, depending on the complexation site. The photophysical properties were fully explored in solution and solid state, presenting ideal results for the preparation of various metallopolymers, in addition to potential application as a metamaterial, due to the presence of the chiral center in the side chains of the polymer.

Study on Synthesis and Characterization of Unsaturated Polyester by Enzyme-Catalyzed

2013 ◽  
Vol 575-576 ◽  
pp. 67-70
Author(s):  
Fen Juan Shao ◽  
Qun Yang ◽  
Lan Ying Li ◽  
Da Nian Lu
Keyword(s):  
High Temperature ◽  
Unsaturated Polyester ◽  
Soxhlet Extraction ◽  
Side Chain ◽  
Synthesis And Characterization ◽  
Cross Linking ◽  
Cross Link ◽  
H Nmr ◽  
Ft Ir

Unsaturated polyester was prepared with adipic acid (AA), fumaric acid (FA), itaconic acid (IA) and 1, 6-hexanediol (HD) by enzyme-catalyzed polmerization. The insoluble gel fraction (Qs), as the cross-linking degree of cured unsaturated polyesters which could be self-cross-linked at high temperature through C=C in it, was got by Soxhlet Extraction. The properties were investigated by FT-IR, 1H NMR, DSC, XRD and so on. The results indicated that the C=C in unsaturated diacids reduced the acitvity of N435, which affected the polmerization. With the introduction of C=C of IA or FA, the Mn of polyester reduced. The C=C could self-cross-link under high temperature for lengthy time. The higher the temperature and the longer the time, the Qs increased. As the C=C of IA was in the side chain, it could move easily. Then Qs of poly (AA-co-IA-co-HD) was higher than ploy (AA-co-FA-co-HD). With the increased content of unsaturated diacid, Qs increased. And the biodegradation of cross-linked polyesters became worse.

Cationic copolymerization of 1,3-pentadiene with α-pinene

2014 ◽  
Vol 34 (7) ◽  
pp. 583-589 ◽  
Author(s):  
Ai-Yuan Li ◽  
Xiang-Dong Sun ◽  
Hui-Bo Zhang ◽  
Yong-Chun Zhang ◽  
Bin Wang ◽  
...  
Keyword(s):  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Polymerization Temperature ◽  
Scanning Calorimetry ◽  
Gardner Color ◽  
H Nmr ◽  
Cationic Copolymerization ◽  
Ft Ir ◽  
Better Than ◽  
C Nmr

Abstract The cationic copolymerization of 1,3-pentadiene (PD) with α-pinene (AP) initiated by aluminum trichloride (AlCl3) was carried out in N-pentane solvent. The effects of the polymerization temperature and the comonomer composition on the yield of the copolymer, softening point, Gardner color scale and number-average molecular weight (Mn) are discussed. The performance of the copolymer was better than that of AP homopolymer (PAP) and PD homopolymer (PPD). The structure of the copolymer was characterized by Fourier transform infrared spectroscopy (FT-IR), 1H-nuclear magnetic resonance (1H-NMR), 13C-NMR, differential scanning calorimetry (DSC) and gel permeation chromatography (GPC). In addition, the reactivity ratios for AP (M1) and PD (M2) determined by the Kelen-Tudos method from low-conversion data are r1=0.58 and r2=5.92, respectively.

Preparation and characterization of post-derivatives from functional polystyrene (ATRP) with p-nitroanilineazomethine phenol and their thermal and optical study

e-Polymers ◽  
2006 ◽  
Vol 6 (1) ◽  
Author(s):  
Xifei Yu ◽  
Guo Zhang ◽  
Tongfei Shi ◽  
P.K. Dutta ◽  
Lijia An
Keyword(s):  
Glass Transition ◽  
Transition Temperature ◽  
Glass Transition Temperature ◽  
Liquid Crystalline ◽  
Gel Permeation Chromatography ◽  
Side Chain ◽  
Scanning Calorimetry ◽  
Xrd Study ◽  
Covalently Linked

AbstractThe functional polystyrene, (Cl-PS)2-CHCOOCH2CH2OH (designated as XPSt and coded P2) was prepared by ATRP at 1300C using CuCl and bipyridine as catalysts, 2,2-dichloro acetate-ethylene glycol (DCAG) as multifunctional initiator and THF as solvent. 4-Nitoroaniline azomethine-4’ phenol (P1) as chromophores were covalently linked to the functional end groups of the polymer by using simple displacement reaction. The functional polystyrenes, namely XPSt (P2) and (PS)2-CHCOOCH2CH2OH, designated as X-PSt and coded P3 and their post-derivatives, namely, DXPSt (P4) and DX-PSt (P5) respectively were characterized by IR, NMR and UV spectroscopies, gel permeation chromatography (GPC) and thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), polarising optical microscopy (POM) and XRD studies. DSC showed that incorporation of chromophores in the side chains of polymers towards the polystyrene moiety increases the rigidity of the polymer and subsequently, its glass transition temperature; however the incorporation of side chain towards the alcoholic functional group decreases the glass transition temperature. The post derivatives do not play any significant role to increase the thermal stability (TGA). There was evidence for liquid crystalline properties in the resulting polymer derivative DXPSt (P4) as observed from POM study, which defines the alignment of chromophores into the polymers. The XRD study shows crystalline behaviour of the polymer derivative, P4. The polymer derivative, DXPSt (P5) does not show such behaviour and this may be due to the bonding of azomethine towards the short chain alcoholic telechelic alcoholic sides of the copolymer.

Purification and characterization of kraft lignin

Holzforschung ◽  
2015 ◽  
Vol 69 (8) ◽  
pp. 943-950 ◽  
Author(s):  
Wenwen Fang ◽  
Marina Alekhina ◽  
Olga Ershova ◽  
Sami Heikkinen ◽  
Herbert Sixta
Keyword(s):  
Thermal Properties ◽  
High Performance ◽  
Inorganic Compounds ◽  
Gel Permeation Chromatography ◽  
Kraft Lignin ◽  
Hot Water ◽  
Scanning Calorimetry ◽  
Target Values ◽  
Lower Glass Transition Temperature

Abstract To upgrade the utilization of kraft lignin (KL) for high-performance lignin-based materials (e.g., carbon fiber), the purity, molecular mass distribution (MMD), and thermal properties need to be improved and adjusted to target values. Therefore, different methods, such as ultrasonic extraction (UE), solvent extraction, dialysis, and hot water treatment (HWT), were applied for the purification of KL. The chemical and thermal properties of purified lignin have been characterized by nuclear magnetic resonance, Fourier transform infrared, gel permeation chromatography, elemental analysis, differential scanning calorimetry, and thermogravimetric analysis. The lignin fractions obtained by UE with ethanol/acetone (E/A) mixture (9:1) revealed a very narrow MMD and were nearly free of inorganic compounds and carbohydrates. Further, the E/A-extracted lignin showed a lower glass transition temperature (Tg) and a clearly detectable melting temperature (Tm). Dialysis followed by HWT at 220°C is an efficient method for the removal of inorganics and carbohydrates; however, lignin was partly forming condensed structures during the treatment.

scholarly journals Synthesis, Characterization andIn VitroAnticancer Evaluation of Itaconic Acid Based Random Copolyester

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
J. Gowsika ◽  
R. Nanthini
Keyword(s):  
Itaconic Acid ◽  
Hydrolytic Degradation ◽  
Gel Permeation Chromatography ◽  
Xrd Analysis ◽  
Titanium Tetraisopropoxide ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Melt Polycondensation

The present study deals with the synthesis and characterization of an aliphatic copolyester, poly [butylene fumarate-co-butylene itaconate] (PIFB) copolymer was obtained from itaconic acid, fumaric acid, and 1,4-butanediol using titanium tetraisopropoxide (TTiPO) through a two step process of transesterification and melt polycondensation. The synthesized aliphatic random copolyester was characterized with the help of FT-IR,1H-NMR,13C-NMR, viscosity measurements, Gel Permeation Chromatography (GPC) and X-ray diffraction (XRD) analysis. Thermal properties have been analyzed using thermogravimetric analysis (TGA) and Differential Scanning Calorimetry (DSC). Hydrolytic degradation studies were carried out in acid and alkaline regions of various pH values. The synthesized copolymer was subjected toin vitroanticancer activity studies against human breast cancer (MCF-7) cell line.

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