scholarly journals Novel Poly(Methylenelactide-g-L-Lactide) Graft Copolymers Synthesized by a Combination of Vinyl Addition and Ring-Opening Polymerizations

Polymers ◽  
2021 ◽  
Vol 13 (19) ◽  
pp. 3374
Author(s):  
Tanyaluck Mekpothi ◽  
Puttinan Meepowpan ◽  
Montira Sriyai ◽  
Robert Molloy ◽  
Winita Punyodom
Keyword(s):  
Ring Opening ◽  
Graft Copolymers ◽  
Decomposition Temperature ◽  
Melt Processing ◽  
Resonance Spectroscopy ◽  
Molecular Weights ◽  
Melting Temperatures ◽  
Grafting Reaction ◽  
Ft Ir ◽  
Liquid Tin

In this work, a novel poly (methylenelactide-g-L-lactide), P(MLA-g-LLA) graft copolymer was synthesized from poly(methylenelactide) (PMLA) and L-lactide (LLA) using 0.03 mol% liquid tin(II) n-butoxide (Sn(OnBu)2) as an initiator by a combination of vinyl addition and ring-opening polymerization (ROP) at 120 °C for 72 h. Proton and carbon-13 nuclear magnetic resonance spectroscopy (1H- and 13C-NMR) and Fourier-transform infrared spectroscopy (FT-IR) confirmed the grafted structure of P(MLA-g-LLA). The P(MLA-g-LLA) melting temperatures (Tm) range of 144–164 °C, which was lower than that of PLA (170–180 °C), while the thermal decomposition temperature (Td) of around 314–335 °C was higher than that of PLA (approx. 300 °C). These results indicated that the grafting reaction could widen the melt processing range of PLA and in doing so increase PLA’s thermal stability during melt processing. The graft copolymers were obtained with weight-average molecular weights (M¯w) = 4200–11,000 g mol−1 and a narrow dispersity (Đ = 1.1–1.4).

Synthesis and characterization of amphiphilic graft copolymers with hydrophobic poly(α-methylstyrene) backbone and hydrophilic poly(n-vinylpyrrolidone) side chains

e-Polymers ◽  
2012 ◽  
Vol 12 (1) ◽  
Author(s):  
Fatima Zohra Sebba ◽  
Seghier Ould Kada ◽  
Mohamed Benaicha ◽  
Nerjesse Nemiche
Keyword(s):  
Graft Copolymer ◽  
Graft Copolymers ◽  
Radical Copolymerization ◽  
Side Chains ◽  
Free Radical Copolymerization ◽  
Good Efficiency ◽  
Molecular Weights ◽  
Grafting Reaction ◽  
Viscosity Variation ◽  
End Capping

AbstractIn this study, 2-oxopropylmethacrylate-terminated poly(N-vinyl-2- pyrrolidone) is produced by cationic polymerization using HClO4 as an initiator. Termination (end capping) step is accomplished using 2- hydroxypropylmethacrylate (2HPMA) and the polymer product has different chain lengths of molecular weight averages ranging from 672 to 3049 g/mol. The study also synthesised amphipathic graft copolymers having hydrophobic poly(α- methylstyrene) as a backbone chain and hydrophilic poly(N-vinyl-2-pyrrolidone) (PVP) as side chains of various lengths. The copolymer synthesis was accomplished by free radical copolymerization of ω-oxopropylmethacrylate PVP in the presence of α-methyl styrene initiated with benzoyl peroxide. Measurements of the dynamic viscosity of the polymer solution (20% weight of macromonomers in ethanol) show that the viscosity is proportional to the average molecular weights M̅n . However, a reverse behaviour of the viscosity variation with regard to M̅n is observed for graft copolymer samples. The viscosity variation with respect to the graft copolymer mass must be due to steric effects, which are strongly pronounced in grafted copolymer chains. Appearance of the number of side chains attached to poly(α-methylstyrene) backbone reveals that the grafting reaction has occurred with good efficiency.

scholarly journals Polyols Prepared from Ring-Opening Epoxidized Soybean Oil by a Castor Oil-Based Fatty Diol

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Jing Zhang ◽  
Ji Jun Tang ◽  
Jiao Xia Zhang
Keyword(s):  
Soybean Oil ◽  
Castor Oil ◽  
Ring Opening ◽  
Epoxidized Soybean Oil ◽  
Epoxy Ring ◽  
Molecular Weights ◽  
Molar Ratios ◽  
Epoxy Ring Opening ◽  
Ft Ir

Several biorenewable vegetable oil-based polyols with different molecular weights and various hydroxyl functionalities were successfully prepared by ring-opening epoxidized soybean oil with a castor oil-based fatty diol. It was found that several factors, including reaction time, reaction temperature, and molar ratios between epoxidized soybean oil and castor oil diol, affect structures and rheology behaviors of the final polyols. Proton NMR, FT-IR, GPC, and rheometry results revealed that the hydroxyl functionalities, molecular weight, and viscosity of the polyols could be tailored by controlling the above-mentioned factors. Besides, the role of solvents in the epoxy ring-opening process was investigated as well.

scholarly journals Synthesis of poly(γ-tert-butyl L-glutamate): influence of polymerization conditions

2019 ◽  
Vol 16 (3) ◽  
pp. 25
Author(s):  
Phung Thi Thuy Dung ◽  
Nguyen Thi Le Thu
Keyword(s):  
Ring Opening ◽  
Gel Permeation Chromatography ◽  
Attenuated Total Reflection ◽  
Resonance Spectroscopy ◽  
Reaction Conditions ◽  
Tert Butyl ◽  
Ft Ir ◽  
Hydrolysis Of ◽  
Polymerization Conditions

This work presents the synthesis and characterization of poly(γ-tert-butyl L-glutamate) (PtBuLG) via a living ring-opening polymerization procedure of γ-tert-butyl L-glutamate N-carboxyanhydride (tBuLG-NCA). The reaction conditions were investigated to optimize the polymerization yield and molecular weight polydispersity. The synthesized PtBuLG was characterized using nuclear magnetic resonance spectroscopy (NMR), gel permeation chromatography (GPC) and attenuated total reflection-Fourier transform infrared (ATR FT-IR. Finally, hydrolysis of PtBuLG resulted in poly(L-glutamic acid) (PLGA).

scholarly journals Poly(delta-gluconolactone) and Poly(delta-gluconolactone-ε-caprolactone) from delta-Gluconolactone and ε-Caprolactone by Ring-Opening Polymerization

2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Ruijiang Li ◽  
Peng Wang ◽  
Haohao Ren ◽  
Hong Li ◽  
Zhengwen Ding ◽  
...  
Keyword(s):  
Melting Temperature ◽  
Intrinsic Viscosity ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
Decomposition Temperature ◽  
Degradation Rates ◽  
Ft Ir

Poly(delta-gluconolactone) (PGL) and poly(delta-gluconolactone-ε-caprolactone) (P(GL-CL)) were synthesized through ring-opening polymerization (ROP) and characterized by FT-IR, NMR, XRD, intrinsic viscosity, GPC, DSC, and TGA. The crystallinity of P(GL-CL) with various d-GL/CL ratios (d-GL/CL = 5 : 5, 4 : 6, 3 : 7, 2 : 8, and 1 : 9) was 12.09 to 59.78% while PGL was amorphous. Melting temperature (Tm) of these polymers was 49.8 to 62.0°C and decomposition temperature was 282 to 489°C depending on the d-GL/CL ratios. In addition, all these polymers were degradable and the degradation rates could be controlled by adjusting d-GL/CL ratios. These results indicated that PGL and P(GL-CL) might be promising novel absorbable materials.

Synthesis and Characterisation of PLA-CO-PEG Copolymers

2012 ◽  
Vol 506 ◽  
pp. 178-181 ◽  
Author(s):  
C. Thanomsilp ◽  
U. Phetthianchai
Keyword(s):  
Molecular Weight ◽  
Tensile Strength ◽  
Thermal Degradation ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
Molecular Weights ◽  
Copolymer Films ◽  
Melting Temperatures ◽  
Monomer Feed ◽  
Solution Cast

PLA-co-PEG copolymers synthesized through ring opening polymerization between a lactide monomer and PEG were solution-cast into films. The effect of the molecular weight of PEG and also the percentage of added PEG on the properties of the copolymers were studied. The molecular weight of PEG was 4000, 8000, and 20000 while the percentage of added PEG was varied from 10 to 50 mol%. The NMR spectrums confirmed that the ratio of PLA:PEG in the copolymers are close to the monomer feed of the respective monomers. DSC and TGA results showed that, compared to PLA, the PLA-co-PEG copolymers have slightly lower melting temperatures but similar thermal degradation temperatures. Both molecular weights and the percentage added of PEG influenced the properties of the films. As expected, the tensile strength and Youngs modulus of the PLA-co-PEG copolymer films were lower than that of neat PLA. Conversely, theelongation at break of the copolymer film was higher than that of the PLA when the molecular weight of PEG was 20000. This study suggests that high molecular weight PEG could be used to improve the flexibility of the polymer films.

scholarly journals Synthesis of Highly Thermally Stable Daidzein-Based Main-Chain-Type Benzoxazine Resins

Polymers ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1341 ◽  
Author(s):  
Mengchao Han ◽  
Sijia You ◽  
Yuting Wang ◽  
Kan Zhang ◽  
Shengfu Yang
Keyword(s):  
Thermal Stability ◽  
Main Chain ◽  
Gel Permeation Chromatography ◽  
Polymerization Process ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
Potential Applications ◽  
Ft Ir ◽  
Chain Type

In recent years, main-chain-type benzoxazine resins have been extensively investigated due to their excellent comprehensive properties for many potential applications. In this work, two new types of main-chain benzoxazine polymers were synthesized from daidzein, aromatic/aliphatic diamine, and paraformaldehyde. Unlike the approaches used synthesizing traditional main-chain-type benzoxazine polymers, the precursors derived from daidzein can undergo a further cross-linking polymerization in addition to the ring-opening polymerization of the oxazine ring. The structures of the new polymers were then studied by 1H nuclear magnetic resonance spectroscopy (NMR) and Fourier-transform infrared spectroscopy (FT-IR), and the molecular weights were determined by using gel permeation chromatography (GPC). We also monitored the polymerization process by differential scanning calorimetry (DSC) and in situ FT-IR. In addition, the thermal stability and flame-retardant properties of the resulting polybenzoxazines were investigated using TGA and microscale combustion calorimeter (MCC). The polybenzoxazines obtained in this study exhibited a very high thermal stability and low flammability, with a Tg value greater than 400 °C, and a heat release capacity (HRC) value lower than 30 J/(g K).

Biodegradable Poly(lactic Acid)/TDI-Montmorillonite Nanocomposites: Preparation and Characterization

2011 ◽  
Vol 221 ◽  
pp. 211-215 ◽  
Author(s):  
Na Li Chen ◽  
Hui Xia Feng ◽  
Jing Wei Guo ◽  
He Ming Luo ◽  
Jian Hui Qiu
Keyword(s):  
Thermal Stability ◽  
Molecular Weight ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
Decomposition Temperature ◽  
Toluene Diisocyanate ◽  
Poly Lactic Acid ◽  
Infrared Spectrometry ◽  
Ft Ir ◽  
Thermal Stability Of

Activated montmorillonite(MMT) was modified by toluene diisocyanate(TDI) and TDI-montmorillonite(TDI-MMT) was prepared. The characterization of TDI-MMT was carried out by X-ray diffraction(XRD) and fourier transform infrared spectrometry (FT-IR). The results showed that TDI had been inserted to the interlayer of MMT and the interlayer spacing of MMT increased by 0.26nm. With stannous chloride as catalyst, the biodegradable polylactide acid/TDI-montmorillonite(PLA/TDI-MMT) nanocomposites were synthesized through ring-opening polymerization of lactide in the layer of TDI-MMT by in-situ polymerization. The structure and thermal stability of nanocomposites were investigated by XRD, FT-IR and thermogravimetry (TG). Exfoliated nanocomposites were obtained as shown by XRD results. FT-IR spectra confirmed that TDI-MMT participated in the ring-opening polymerization of lactide. TG analysis indicated the decomposition temperature of nanocomposites rose and the thermal stability was improved contrast to the neat PLA. The effect of the content of TDI-MMT on the molecular weight and thermal stability of nanocomposites was studied. With the increase of the proportion of TDI-MMT, the molecular weight of resultant nanocomposites decreased and the decomposition temperature rose at the range of experiment research.

Synthesis of α,ω-bis(3-aminopropyldiethoxylsilane) Poly(tri fluoropropylmethyl)siloxanes

e-Polymers ◽  
2007 ◽  
Vol 7 (1) ◽  
Author(s):  
Zhendong Shi ◽  
Xinling Wang
Keyword(s):  
Molecular Weight ◽  
Ring Opening ◽  
Reaction Rate ◽  
Ring Opening Polymerization ◽  
Step Process ◽  
Molecular Weights ◽  
H Nmr ◽  
One Step ◽  
Ft Ir ◽  
High Yields

AbstractHigh molecular weight α,ω-bis(3-aminopropyldiethoxylsilane) poly(tri fluoropropylmethyl)siloxanes (APTFPMS) were prepared via a “one-step” process, based on the ring-opening polymerization of 1,3,5-tris(trifluoropropylmethyl) cyclotrisiloxane (F3) in the presence of water and 3-aminopropyltriethoxysilane (APTES). GPC, FT-IR and 1H NMR confirmed the structure of the polymers. It was found that the amount of APTES had significant influence on the reaction rate and the molecular weights of polymers decreased with the increasing amount of water. It was probably because both water and the amino group of APTES favoured generation of hydroxyl ions, which efficiently initiate the polymerization of F3 to achieve APTFPMS. In order to verify this mechanism, another “two-step” process was also performed: Firstly the α,ω-dihydroxylated poly(trifluoropropylmethyl) siloxanes were synthesized from F3 catalyzed by both diaminoethane and water, then reacted with APTES to achieve APTFPMS. All the syntheses had high yields and the molecular weight of the polymers ranged from 2000 to 25000.

Preparation, Cross-Linking and Characterization of Novel Benzocyclobutene-Siloxane Polymers with Polysiloxane Mainchain and Silylbenzocyclobutene Pendant Groups

2012 ◽  
Vol 534 ◽  
pp. 178-183 ◽  
Author(s):  
Hui Ling Li ◽  
Ya Wen Hang ◽  
Ke Cao ◽  
Fang Hua Zhu ◽  
Jun Xiao Yang
Keyword(s):  
Ring Opening ◽  
Decomposition Temperature ◽  
Cross Linking ◽  
Initial Decomposition Temperature ◽  
Hydrosilylation Reaction ◽  
On Line ◽  
Ft Ir ◽  
Siloxane Polymers ◽  
Incorporation Ratio

A series of BCB-siloxane polymers with benzocyclobutene (BCB) pendant groups and polysiloxane mainchain was prepared by the hydrosilylation reaction between 4-(1,1-di-methyl-1-vinyl) silylbenzocyclobutene (4-DMVSBCB) and poly (methylhydrosiloxane) (PHMS) employing Pt/C as catalyst. Upon heating the BCB-siloxane polymers, the cross-linking occurred via ring-opening of benzocyclobutene as evidenced by on-line FT-IR, 1H NMR and 13C NMR. TGA examination indicates that the thermal stability was enhanced with increasing the incorporation ratio of BCB. Most importantly, the initial decomposition temperature of crosslinked BCB-siloxane resins is as high as 429 oC, showing a superior thermal resistance over most other BCB resins.

Preparation of graft copolymers by the reaction of polymeric acyl chlorides with monohydroxy-terminated polymers: An introductory study

1988 ◽  
Vol 53 (8) ◽  
pp. 1735-1744 ◽  
Author(s):  
Jitka Horská ◽  
Jaroslav Stejskal ◽  
Pavel Kratochvíl ◽  
Aubrey D. Jenkins ◽  
Eugenia Tsartolia ◽  
...  
Keyword(s):  
Light Scattering ◽  
Chemical Composition ◽  
Statistical Model ◽  
Graft Copolymers ◽  
Coupling Reaction ◽  
Molecular Characteristics ◽  
Gel Formation ◽  
Acyl Chlorides ◽  
Molecular Weights

An attempt was made to prepare well-defined graft copolymers by the coupling reaction between acyl chloride groups located along the backbone chain and monohydroxy-terminated grafts prepared separately. The molecular weights and the parameters of heterogeneity in chemical composition of the products were determined by light scattering and osmometry. The determination of molecular characteristics revealed that the degree of grafting was low. The results therefore could not be confronted with a statistical model at this stage. The problems encountered in the synthesis, e.g., gel formation, and the data relating to the soluble products are discussed.

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