Synthesis and characterization of novel poly(butylene succinate-co-2-methyl-1,3-propylene succinate)s

Abstract

Abstract. Poly(butylene succinate) (PBSu), poly(2-methyl-1,3-propylene succinate) (PMPSu), and PBSu-rich copolyesters were synthesized using an effective catalyst, titanium tetraisopropoxide. Measurements of intrinsic viscosity (1.20-1.28 dl/g) and gel permeation chromatography demonstrated the success of the preparation of polyesters with high molecular weights. The compositions of the copolyesters were determined in three approaches from 1 H and 13 C NMR (nuclear magnetic resonance) analyses, and good agreement between the results was obtained. The distributions of the comonomers were found to be random from the spectra of carbonyl carbon. Their thermal properties were elucidated using a differential scanning calorimeter and a thermogravimetric analyzer. No marked difference exists among the thermal stabilities of these polyesters. However, the window between the glass transition and the melting temperatures becomes narrower with the increase in the concentration of 2-methyl-1,3-propylene succinate in the copolymers. Additionally, the cold crystallization ability decreases considerably. Finally, PMPSu is an amorphous homopolymer. Wide-angle X-ray diffractograms of isothermally crystallized copolyesters also follow the same trend.

Slow relaxations in semicrystalline poly(butylene succinate) below and aboveTg

“…The component peak with higher intensity of this relaxation (PP peak obtained with a polarization temperature T P 5 242 C) has its maximum at T m 5 240 C, which is the T g value provided by the TSDC technique. Note that this value is somewhat lower than the value of the calorimetric T g reported before (234 C), but it is in good agreement with other values published in the literature [10,23,24,41]. The fitting to the Arrhenius equation of the log s (T) versus 1/T line corresponding to this higher intensity peak provides the value of the activation energy at T g , E a (T g ) 5 191 kJ mol 21 (close to the value 195 kJ mol 21 reported before and obtained from DRS data).…”

Mechanisms and kinetics of thermal degradation of poly(butylene succinate‐co‐propylene succinate)s

“…Peaks a–c are associated with the carbonyl carbons of BSB, the BSP‐B side structure and the BSP‐P side structure, respectively, (where B, S, and P represent the groups that are derived from 1,4‐butanediol, succinic acid, and 1,3‐propanediol, respectively). The normalized areas under these three peaks can be used to calculate the probabilities of three triads, composition, randomness, and the sequence distribution of BS and PS units of this copolyester 21, 30, 31. PBPSu 90/10 is characterized as having 89.5% BS units and 10.5% PS units, which finding differs slightly from that of 1 H‐NMR (see Table I).…”

A Novel Approach for the Preparation of Poly(Butylene Succinate) Microparticles

“…The obtained molar masses can be considered low for applications that require good mechanical properties, but seem adequate for manufacture of microparticles intended for cosmetic applications and are higher than molar masses reported in other studies and obtained at more severe reaction conditions . For the sake of comparison, Chen et al studied the synthesis of several biomass polymers; for the specific case of PBS, the reaction was performed with the catalyst TTP (titanium tetraisopropoxide) and led to PBS resins with Mn of 3000 Da after 20 h of reaction at 220 °C. Costa et al also synthesized a series of polycondensation polymers, using succinic acid, itaconic acid, and furanic acid as monomers, in the absence of catalyst at 205 °C for 12 h, leading to PBS resins with Mn of 3500 Da.…”