scholarly journals Synthesis and Characterization of N-Substituted Polyether-Block-Amide Copolymers

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 773
Author(s):  
Jyun-Yan Ye ◽  
Kuo-Fu Peng ◽  
Yu-Ning Zhang ◽  
Szu-Yuan Huang ◽  
Mong Liang

A series of N-substituted polyether-block-amide (PEBA-X%) copolymers were prepared by melt polycondensation of nylon-6 prepolymer and polytetramethylene ether glycol at an elevated temperature using titanium isopropoxide as a catalyst. The structure, thermal properties, and crystallinity of PEBA-X% were investigated using nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectroscopy, differential scanning calorimetry, wide angle X-ray diffraction, and thermogravimetric analysis. In general, the crystallinity, melting point, and thermal degradation temperature of PEBA-X% decreased as the incorporation of N-methyl functionalized groups increased, owing to the disruption caused to the structural regularity of the copolymer. However, in N-acetyl functionalized analogues, the crystallinity first dropped and then increased because of a new γ form arrangement that developed in the microstructure. After the cross-linking reaction of the N-methyl-substituted derivative, which has electron-donating characteristics, with poly(4,4′-methylenebis(phenyl isocyanate), the decomposition temperature of the resulting polymer significantly increased, whereas no such improvements could be observed in the case of the electro-withdrawing N-acetyl-substituted derivative, because of the incompleteness of its cross-linking reaction.

2012 ◽  
Vol 554-556 ◽  
pp. 126-129 ◽  
Author(s):  
Shun Yin ◽  
Ning Sun ◽  
Chun Yun Feng ◽  
Zhi Mou Wu ◽  
Zhao Hua Xu ◽  
...  

A series of different generation hyperbranched polyurethane(HBPU) was synthesized based on the raw materials of isophorone diisocyanate(IPDI) and diethanolamine(DEOA). Their structure, thermal degradation mechanism and glass transition temperature(Tg) were characterized by fourier transform infrared spectroscopy(FTIR), nuclear magnetic resonance spectroscopy(NMR), thermal gravimetric analysis(TGA) and differential scanning calorimetry(DSC). The results showed that: the yield of each generation HBPU was up to 90%, different generation HBPU had almost the same initial degradation temperature(about at 200°C) and they all had two decomposition platforms; with the increase of generation, Tg increased from 107.2°C to 132.1°C. The gloss and hardness of the HBPU coatings were significantly improved.


Polymers ◽  
2019 ◽  
Vol 11 (6) ◽  
pp. 937 ◽  
Author(s):  
Niki Poulopoulou ◽  
George Kantoutsis ◽  
Dimitrios N. Bikiaris ◽  
Dimitris S. Achilias ◽  
Maria Kapnisti ◽  
...  

Poly(butylene 2,5-furandicarboxylate) (PBF) constitutes a new engineering polyester produced from renewable resources, as it is synthesized from 2,5-furandicarboxylic acid (2,5-FDCA) and 1,4-butanediol (1,4-BD), both formed from sugars coming from biomass. In this research, initially high-molecular-weight PBF was synthesized by applying the melt polycondensation method and using the dimethylester of FDCA as the monomer. Furthermore, five different series of PBF blends were prepared, namely poly(l-lactic acid)–poly(butylene 2,5-furandicarboxylate) (PLA–PBF), poly(ethylene terephthalate)–poly(butylene 2,5-furandicarboxylate) (PET–PBF), poly(propylene terephthalate)–poly(butylene 2,5-furandicarboxylate) (PPT–PBF), poly(butylene 2,6-naphthalenedicarboxylate)-poly(butylene 2,5-furandicarboxylate) (PBN–PBF), and polycarbonate–poly(butylene 2,5-furandicarboxylate) (PC–PBF), by dissolving the polyesters in a trifluoroacetic acid/chloroform mixture (1/4 v/v) followed by coprecipitation as a result of adding the solutions into excess of cold methanol. The wide-angle X-ray diffraction (WAXD) patterns of the as-prepared blends showed that mixtures of crystals of the blend components were formed, except for PC which did not crystallize. In general, a lower degree of crystallinity was observed at intermediate compositions. The differential scanning calorimetry (DSC) heating scans for the melt-quenched samples proved homogeneity in the case of PET–PBF blends. In the remaining cases, the blend components showed distinct Tgs. In PPT–PBF blends, there was a shift of the Tgs to intermediate values, showing some partial miscibility. Reactive blending proved to improve compatibility of the PBN–PBF blends.


2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.


2013 ◽  
Vol 858 ◽  
pp. 13-18
Author(s):  
Abu Hannifa Abdullah ◽  
Kamal Yusoh ◽  
Mohamad Faiz Mohamed Yatim ◽  
Siti Amirah Nor Effendi ◽  
Wan Siti Noorhashimah W. Kamaruzaman

The thermal behaviour of polymer layered silicate nanocomposite were characterised to compare the improvement of the nanocomposite with the pristine polymer. It is known that pristine polymers have some weakness in its thermal properties especially biodegradable polymers. The approach of making the nanocomposite out of modified layered silicate and biodegradable polymer is to enhance the thermal behaviour of the biodegradable polymer. The nanocomposites were produced by solution method technique using dichloromethane as a solvent and the two types of nanoclay were used. One was modified with transition metal ion and another type of nanoclay is pristine nanoclay. Wide angle X-ray diffraction (XRD) was used to characterise the structure of the nanoclay after the modification and the type of nanocomposite obtained. Melting temperature and degradation temperature of the nanocomposite were obtained by using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) respectively. Decrease in both thermal degradation temperature and melting temperature of the nanocomposites were observed.


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
J. Gowsika ◽  
R. Nanthini

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.


2018 ◽  
Vol 26 (3(129)) ◽  
pp. 17-22 ◽  
Author(s):  
Xichao Sun ◽  
Yeqian Ge

In order to provide a theoretical basis for the preparation and spinnability of two-component materials, poly(3-hydroxybutyrate-co-3-hydroxyvalerate)(PHBV) and polypropylene grafting maleic anhydride (PP-g-MAH) blends were prepared by melt mixing with different ratios (100/0, 75/25, 50/50, 25/75, 0/100). Properties of the blends system were investigated by means of a mixed rheometer, scanning electron microscope, simultaneous thermal analyser, differential scanning calorimetry and X-ray diffraction. The results demonstrate that PHBV/PP-g-MAH blends exhibit different morphology of the sea-island with a change in the mix ratio. The initial thermal decomposition temperature of PHBV in the blending system is over 250 °C, which means the thermal stability of PHBV is markedly improved. The crystallisation of PHBV varied according to the blending process parameter. When the cooling velocity increases, the crystallisation peak becomes wide, the temperature of crystallisation decreases, and the crystallisation temperature of PHBV increases significantly. PHBV has a high sensitivity to variation in the shear rate, and PHBV/PP-g-MAH blends have the mixing characteristic of shear thinned liquid. There is no diffraction peak at 2θ = 22.8°, and this result certifies that PP-g-MAH changes the crystal form of PHBV. and that PP-g-MAH addition is beneficial to the spinnability of PHBV. Results show that the interplay between PHBV and PP-g-MAH is of great significance and universal for both plastics and fibres.


2020 ◽  
pp. 095400832096053
Author(s):  
Diana Serbezeanu ◽  
Ana-Maria Macsim ◽  
Ionela-Daniela Carja ◽  
Corneliu Hamciuc ◽  
Marius Pislaru ◽  
...  

Liquid crystalline hyperbranched poly(aryl ester)s (A2B3) were prepared by polycondensation reaction of 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)1,4-naphthalene diol with 1,3,5-benzenetricarbonyl trichloride, taken in two different molar ratios. The chemical structure of the newly synthesized hyperbranched polymers was confirmed by FTIR, 1H NMR, 13C NMR spectroscopy. The polymers exhibited high thermal stability with initial decomposition temperature above 410–435°C and char yield at 700°C higher than 40%. Combined differential scanning calorimetry, polarized optical microscopy and wide-angle X-ray diffraction measurements were carried out to closely examine their thermal behavior and phase transitions.


2004 ◽  
Vol 19 (5) ◽  
pp. 1492-1498 ◽  
Author(s):  
Stacey W. Boland ◽  
Suresh C. Pillai ◽  
Wein-Duo Yang ◽  
Sossina M. Haile

Solid solution Pb1-xBaxTiO3, with particular emphasis on Pb0.5Ba0.5TiO3, was prepared using a sol-gel process incorporating lead acetate trihydrate, barium acetate, and titanium isopropoxide as precursors, acetylacetone (2,4 pentanedione) as a chelating agent, and ethylene glycol as a solvent. The synthesis procedure was optimized by systematically varying acetylacetone: Ti and H2O:Ti molar ratios and calcination temperature. The resulting effects on sol and powder properties were studied using thermogravimetric analysis/differential scanning calorimetry, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller analysis, and x-ray diffraction (XRD). Crystallization of the perovskite structure occurred at a temperature as low as 450 °C. Thin films were prepared by spin coating on (100) MgO. Pyrolysis temperature and heating rate were varied, and the resultant film properties investigated using field-emission scanning electron microscopy, atomic force microscopy, and XRD. Under optimized conditions, highly oriented films were obtained at a crystallization temperature of 600 °C.


2012 ◽  
Vol 535-537 ◽  
pp. 103-109 ◽  
Author(s):  
Xiang Min Xu ◽  
Li Ping Guo ◽  
Yu Dong Zhang ◽  
Zhi Jun Zhang

The polyoxymethylene-based composites containing reactable nano-SiO2were prepared in a twin-screw extruder by melt compounding, and mechanical and thermal properties of pure polyoxymethylene (POM) and composites were investigated. The results showed that reactable nano-SiO2could reinforce the tensile strength and Young’s modulus of composites. To the impact strength of composites, there was obvious improvement when a small amount of silica was added into POM. With the increase of silica content, the impact strength of composites showed a gradually decrease trend. It was worthy to note that reactable nano-SiO2could significantly increase the decomposition temperature of POM. When the content of reactaSubscript textble nano-SiO2was up to 5 wt%, the degradation temperature of composites could increase about 38.3°C under nSubscript textitrogen atmosphere and 43.8°C under air atmosphere, respectively, compared with pure POM. Furthermore, the differential scanning calorimetry (DSC) analysis showed that reactable nano-SiO2had a good heterogeneous nucleation capability in POM, and could increase crystallization temperature of POM, but surface structure of reactable nano-SiO2was not propitious to the growth of POM crystals, accordingly leading to the decreasing crystallinity of composites.


2002 ◽  
Vol 17 (12) ◽  
pp. 3230-3236 ◽  
Author(s):  
F. Zhou ◽  
Y. T. Chou ◽  
E. J. Lavernia

Thermal decomposition of supersaturated single-phase body-centered cubic (bcc) Fe100−xZnx (5≤ x ≤65 at.%) solid solutions, processed via mechanical alloying of high-purity metal powders, was investigated using x-ray diffraction and differential scanning calorimetry (DSC). At elevated temperatures the metastable solid solution decomposed into a stable equilibrium aggregate consisting of the pure bcc Fe phase and an intermetallic compound Fe4Zn9. The decomposition temperature decreased with increasing Zn concentration. The enthalpy of decomposition for various Fe–Zn solid solutions measured by the DSC was in the range of 1.2–3.5 kJ/mol. The enthalpy of mixing of the as-milled solid solutions from elemental Fe and Zn powders was estimated to be 0.5–1.7 kJ/mol. In addition, the activation energies of decomposition for these solid solutions were determined on the basis of the Kissinger analysis, and their values appeared to be independent of the Zn concentration in the alloy, with an average of 147 ± 17 kJ/mol.


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