scholarly journals Preparation and Characterization of Biobased Lignin-Co-Polyester/Amide Thermoplastics

Molecules ◽  
2021 ◽  
Vol 26 (9) ◽  
pp. 2437
Author(s):  
Eric L. Young ◽  
Armando G. McDonald
Keyword(s):  
Ftir Spectroscopy ◽  
Chain Length ◽  
Lignin Content ◽  
Condensation Reaction ◽  
Building Blocks ◽  
Polymerization Reaction ◽  
Synthesis Methods ◽  
Ionization Mass ◽  
Molar Content ◽  
Scanning Calorimetry

More than 23 million tonnes of lignin are produced annually in the US from wood pulping and 98% of this lignin is burnt. Therefore, creating products from lignin, such as plastics, offers an approach for obtaining sustainable materials in a circular economy. Lignin-based copolymers were synthesized using a single pot, solvent free, melt condensation reaction. The synthesis occurred in two stages. In the first stage, a biobased prepolymer consisting of butanediol (BD, 0.8–1 molar content) and a diacid (succinic (SA), adipic (AA) and suberic acids (SuA), with varying amounts of diaminobutane (DAB, 0–0.2 molar content) was heated under vacuum and monitored by Fourier transform infra-red (FTIR) spectroscopy and electrospray ionization-mass spectrometry (ESI-MS). In the second stage, prepolymer was mixed with a softwood kraft lignin (0–50 wt.%) and further reacted under vacuum at elevated temperature. Progression of the polymerization reaction was monitored using FTIR spectroscopy. The lignin-copolyester/amide properties were characterized using tensile testing, X-ray diffraction (XRD), dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) techniques. Lignin co-polymer tensile (strength 0.1–2.1 MPa and modulus 2 to 338 MPa) properties were found to be influenced by the diacid chain length, lignin, and DAB contents. The lignin-copolymers were shown to be semi-crystalline polymer and have thermoplastic behavior. The SA based copolyesters/amides were relatively stiff and brittle materials while the AA based copolyesters/amides were flexible and the SuA based copolyesters/amides fell in-between. Additionally, > 30 wt.% lignin the lignin- copolyesters/amides did not exhibit melt behavior. Lignin-co-polyester/amides can be generated using green synthesis methods from biobased building blocks. The lignin- copolyesters/amides properties could be tuned based on the lignin content, DAB content and diacid chain length. This approach shows that undervalued lignin can be used in as a macromonomer in producing thermoplastic materials.

Preparation and Characterization of Compounds Based on Poly(hydroxymethylacrylamide) and Post-consumer Polypropylene

2016 ◽  
Vol 10 (3) ◽  
pp. 291-298 ◽  
Author(s):  
Ilma Cirne ◽  
◽  
Maria Esperidiao ◽  
Jaime Boaventura ◽  
Elizabete Lucas ◽  
...  
Keyword(s):  
Polymer Composites ◽  
Food Packaging ◽  
Low Cost ◽  
Condensation Reaction ◽  
Polymerization Reaction ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Swelling Capacity ◽  
Ft Ir

In this work, in order to obtain materials with potential for treatment of water from oil industry, polymer composites were synthesized by polymerization reaction via free radical using n-hydroxymethyl acrylamide (HMAA) in the presence of post-consumer polypropylene (PP) with subsequent condensation reaction catalyzed by heating, which avoids the use of crosslinking agents. The products were characterized by Fourier transform infrared spectroscopy (FT-IR), optical microscopy (OM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and X-ray diffraction (XRD). Moreover, the bulk density and the degree of swelling were also determined. The synthesis was shown to be reproducible and led to achieving polymer composites with high levels of PP after usage from food packaging, which can be associated with a relatively low cost of production. The swelling capacity and the thermal stability of the composite increased with increasing PP content in the mixture.

scholarly journals Synthesis of Triphenylamine-Based Rhombimine Macrocycle by [2+2] Cyclocondensation Reaction between (1R,2R)-Diaminocyclohexane and 4,4’-Diformyl Triphenylamine

2009 ◽  
Vol 4 (1) ◽  
pp. 97-102
Author(s):  
Loredana Vacareanu (Stafie) ◽  
Virgil Barboiu ◽  
Daniel Timpu ◽  
Mircea Grigoras
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Ftir Spectroscopy ◽  
Electrospray Ionization ◽  
1H Nmr ◽  
Electrospray Ionization Mass Spectrometry ◽  
Condensation Reaction ◽  
Uv Absorption ◽  
Ionization Mass ◽  
Cyclocondensation Reaction

A Schiff base macrocycle with persistent rhomboidal shape was synthesized in excellent yield through [2+2] condensation reaction between (R,R)-1,2-diaminocyclohexane and 4,4’-diformyltriphenylamine. The dimeric macrocylic structure was proved by electrospray ionization mass spectrometry (ESI-MS), 1H-NMR, and FTIR spectroscopy. The complexation properties were evidenced by UV absorption.

scholarly journals Manipulation of the Glass Transition Properties of a High-Solid System Made of Acrylic Acid-N,N′-Methylenebisacrylamide Copolymer Grafted on Hydroxypropyl Methyl Cellulose

2021 ◽  
Vol 22 (5) ◽  
pp. 2682
Author(s):  
Nazim Nassar ◽  
Felicity Whitehead ◽  
Taghrid Istivan ◽  
Robert Shanks ◽  
Stefan Kasapis
Keyword(s):  
Glass Transition ◽  
Acrylic Acid ◽  
Methyl Cellulose ◽  
Small Deformation ◽  
Polymerization Reaction ◽  
Solid Matrix ◽  
Scanning Calorimetry ◽  
Modulated Differential Scanning Calorimetry ◽  
High Solid ◽  
Hydroxypropyl Methyl Cellulose

Crosslinking of hydroxypropyl methyl cellulose (HPMC) and acrylic acid (AAc) was carried out at various compositions to develop a high-solid matrix with variable glass transition properties. The matrix was synthesized by the copolymerisation of two monomers, AAc and N,N′-methylenebisacrylamide (MBA) and their grafting onto HMPC. Potassium persulfate (K2S2O8) was used to initiate the free radical polymerization reaction and tetramethylethylenediamine (TEMED) to accelerate radical polymerisation. Structural properties of the network were investigated with Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), modulated differential scanning calorimetry (MDSC), small-deformation dynamic oscillation in-shear, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The results show the formation of a cohesive macromolecular entity that is highly amorphous. There is a considerable manipulation of the rheological and calorimetric glass transition temperatures as a function of the amount of added acrylic acid, which is followed upon heating by an extensive rubbery plateau. Complementary TGA work demonstrates that the initial composition of all the HPMC-AAc networks is maintained up to 200 °C, an outcome that bodes well for applications of targeted bioactive compound delivery.

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.

scholarly journals Solvo-thermal Assisted-Synthesis; Experimental and Theoretical Characterization; and Biological Evaluations of Azo-Chelator-Ligand Chelates of Fe(II) and Zn(II) ions

2021 ◽  
pp. 40-56
Author(s):  
Festus Chioma
Keyword(s):  
Condensation Reaction ◽  
Test Methods ◽  
Molar Conductance ◽  
Ionization Mass ◽  
Metallic Ions ◽  
Bivalent Ions ◽  
Iron Sulphate ◽  
Methods Analytical ◽  
Micro Analysis

Background and Objectives: The resistance of microbes against anti-bacteriological drugs leading to countless deaths and terminal ailments remains a basis for concern. Hence, the main interest of this study was to design, synthesize and report unusual compounds with basic hydrophilic moieties plus hydrophobic functions for anti-bacteriological studies. Materials and Methods: Analytical (melting points, micro-analysis (C. H.N.S) magnetic susceptibility (µeff), molar conductance plus solubility test) methods; spectral (Fourier Transform Infrared(FTIR)), electrospray ionization mass spectrometry (ESI-MS), nuclear magnetic resonance (1H- plus 13C-NMR), electronic(UV-Vis)) measurements; theoretical (DFT) evaluations were utilized for the characterization of the chelator and its chelates. All synthesized compounds were examined for antimicrobial and antioxidant potentials while the chelator was singly evaluated for solvent extractive capacity. Results: A nitrogenous based chelator-ligand, (E)-1-(((4,6-dimethylpyrimidin-2-yl)imino)methyl) naphthalen-2-ol(LH) synthesized through reflux-condensation reaction of 2-amino-4,6-dimethylpyrimidine with 2-hydroxy-1-napthaldehyde was acquired. Further reflux of the chelator-ligand with bivalent ions of iron-sulphate and zinc-acetate salts plus 2,2’-bipyridine resulted into separate bivalent-heteroleptic metallic chelates. The deprotonated nitrogen of the amine moiety and carbon of the carbonyl gave rise to the chelator-ligand with N2O2 chromophore detected around the metallic atom in the chelates. The µeff data plus UV-Vis spectral values of the chelates conformed to 6-coordinate octahedral geometry. All the chelates were high spin and non-ionic in dimethylsulfoxide (DMSO). The antimicrobial and antioxidant screening of the compounds presented moderate to fantastic results, while the metallic extractive proficiency of the chelator showed outstanding extractability for Fe2+ and Zn2+ions with an efficiency of 79.34% and 51.92% correspondingly. Conclusion: All the synthesized compounds are novel and demonstrated prospective biological, plus metallic ions’ extractive potentials required for designs plus isolation of products also for such actions.

Sensitization of nitrocompounds by amines

1992 ◽  
Vol 339 (1654) ◽  
pp. 403-417 ◽  
Keyword(s):  
Thermal Decomposition ◽  
Charge Transfer ◽  
Nitro Group ◽  
Picric Acid ◽  
Isotope Analysis ◽  
Ionization Mass ◽  
Scanning Calorimetry ◽  
Absorption Bands ◽  
Rate Determining Step ◽  
The Impact

A study has been carried out of the sensitization of nitromethane, trinitrotoluene, trinitrobenzene, picric acid and tetryl by the addition of small amounts of amines. The sensitization has been confirmed using dropweight impact experiments and a new method has been found, using differential scanning calorimetry, of making reproducible and quantitative measurements of the effect. It is found that the nitrocompound-amine mixtures decompose at temperatures lower than those of either of the pure components and show a drop in the impact energy required to cause initiation of ignition. The thermal decomposition experiments also yield substantially lower activation energies and an empirical sensitization factor (defined in the text) for nitromethane mixtures that decreases as the nitromethane aci-anion concentration increases. Kinetic deuterium isotope analysis points to C-N bond scission as the rate-determining step in the thermal decomposition of nitromethane and nitromethane-amine mixtures. Laser ionization mass analyses of the solid nitrocompound-amine mixtures indicate significant changes in the fragmentation patterns, with removal of the nitro-group occurring in all cases as the first step in the breakdown of the mixtures, which is not the case for the pure materials. Absorption bands appear in the UV / visible spectra of all the sensitized materials. These bands are ascribed to an intermolecular charge transfer from the nitrogen of an amine group to the antibonding orbital of the nitro-group. It is shown that, with small amounts of amines present, each amine molecule can form a complex with as many nitrocompound molecules as there are amine groups on it. The formation of this charge transfer complex is shown to weaken the nitrocompound C-N bond involved. The weakening of the C-N bond increases directly with increasing binding energy of the complex. Combined with the knowledge that the C-N bond breakage is the rate- ­determining step in the thermal decomposition of these materials and the suggestion that the dominant mechanism in their ignition/detonation is most likely thermal in origin, the sensitization is explained. This explanation deviates from the theories which have been previously proposed.

Azomethine ether-based potential curing agent for epoxy resin (diglycidyl ether of bisphenol A): Synthesis and characterization

2020 ◽  
pp. 009524432092857
Author(s):  
Fozia Noreen ◽  
Ahtaram Bibi ◽  
Naila Khalid ◽  
Imran Ullah Khan
Keyword(s):  
Spectral Analysis ◽  
Bisphenol A ◽  
Light Emission ◽  
Condensation Reaction ◽  
Stokes Shift ◽  
Green Light ◽  
Diglycidyl Ether ◽  
Proton Nuclear Magnetic Resonance ◽  
Curing Agent ◽  
Scanning Calorimetry

Novel azomethine ether-based compounds (A: N-((4-(9-(4-(phenylimino)methyl)phenoxy)nonyloxy)benzylidene)bezenamine and B: N-((4-(9-(4-(p-hydroxyphenylimino)methyl)phenoxy)nonyloxy)benzylidene)-4-hydroxybenzenamine) were synthesized by condensation reaction of dialdehyde, 4,4-(1,9-nonandiyle)bis(oxy)dibenzaldehyde with aromatic amines. Structures of synthesized compounds were successfully characterized by Fourier transform infrared (FTIR), ultraviolet–visible, proton nuclear magnetic resonance imaging and photoluminescence (PL) spectroscopy. The PL spectral analysis revealed that emission maxima of compounds A and B are at 475 and 500 nm, respectively, indicate blue and green light emission with large Stokes shift range (Δ λ ST, 109–138 nm). Two series of polymers: one azomethine-based polymers (C1–C5) and other without azomethine (H1–H4) were prepared by curing diglycidyl ether of bisphenol A with a synthesized curing agent (B) and commercial curing agent, respectively, in various proportions. The structural characterization of the resulting polymers was carried out by FTIR spectral analysis. Thermal properties revealed that azomethine-based polymers (C1–C5) were thermally stable up to 400°C as compared to H1–H4. The glass transition temperature of the polymers, determined by differential scanning calorimetry, was in the range 121–123°C.

Effect of chain segment length on crystallization behaviors of poly(l-lactide-b-ethylene glycol-b-l-lactide) triblock copolymer

2019 ◽  
Vol 28 (2) ◽  
pp. 77-88
Author(s):  
Yongji Gong ◽  
Weihua Song ◽  
Yifan Wu ◽  
Daohai Zhang ◽  
Yufei Liu ◽  
...  
Keyword(s):  
Growth Rate ◽  
Ethylene Glycol ◽  
Chain Length ◽  
Triblock Copolymer ◽  
Triblock Copolymers ◽  
Segment Length ◽  
Resonance Spectroscopy ◽  
Chain Segment ◽  
Scanning Calorimetry ◽  
Crystallization Behaviors

The poly(l-lactide-b-ethylene glycol-b-l-lactide) (PLLA-PEG-PLLA) triblock copolymers with different chain segment length are fabricated by ring-opening polymerization. The structure, molecular weight, and crystallization behaviors of the triblock copolymers are characterized by Fourier transform infrared, nuclear magnetic resonance spectroscopy, gel permeation in chromatography, X-ray diffraction, differential scanning calorimetry, and polarizing optical microscopy (POM). The results show that the increase of block length is beneficial to improve its crystallization. In addition, the triblock copolymer exhibits a double crystallization phenomenon. The POM results indicate that PEG and PLLA chains of the copolymer crystallize in their respective crystallization temperature regions. The growth rate of the PLLA spherocrystal decreases and the dendritic spherocrystals appear with increasing the PEG chain length when the PLLA chain of the copolymer is isothermal crystallized at 80°C and PLLA chain length is constant. The growth rate of the PEG spherocrystal decreases and the spherocrystal morphology changes little with increasing PLLA chain length when the PEG chain is isothermal crystallized at 25°C and the length of PEG chain remained unchanged.

Sign in / Sign up

Export Citation Format

Share Document