Syntheses of Poly(butylene succinate) by Means of Non-Toxic Catalysts

Lahcini, Mohammed; Qayouh, Hicham; Yashiro, Takao; Simon, Peter F. W.; Kricheldorf, Hans R.

doi:10.1080/10601321003741875

Cited by 15 publications

(14 citation statements)

References 29 publications

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“…As reported in the literature, the synthesis of PBS may produce a non negligible amount of oligomers, especially cyclic species [18,19]. Most of the time, in scientific studies, PBS is purified to get rid of these species but commercial PBS clearly contains oligomers since dissolution/precipitation steps are not performed.…”

Section: End-groups Analysis Taking Into Account Cyclic Oligomersmentioning

confidence: 99%

“…They proposed a correction factor ranging from 0.54 to 0.58 depending on the polymer. For PBS, Lahcini et al [19] found that measurements by SEC in chloroform calibrated with polystyrene standards caused an overestimation of the molar mass by 80-100% compared to universal calibration. Actually, the values determined by SEC can vary significantly depending on the detector and/or on the calibration for PBS samples.…”

Section: Comparison Of Molar Mass Data Obtained By 1 H-nmr and Secmentioning

confidence: 99%

“…The above comment illustrates one of the reasons why the determination of molar mass by SEC with a refractive index or light scattering detector for polyesters is controversial in chloroform. Several authors have recently highlighted that polystyrene-calibrated SEC measurements in chloroform overestimate the real M n -by at least 50% in the range above 10 4 g·mol -1 for poly("-caprolactone), polylactide and related copolyesters [18][19][20][21][22][23][24]. For these reasons, researchers have used complementary techniques such as MALDI-TOF mass spectrometry [19,25].…”

Section: Introductionmentioning

confidence: 99%

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Solution viscosity – molar mass relationships for poly(butylene succinate) and discussion on molar mass analysis

Charlier¹,

Girard²,

Freyermouth³

et al. 2015

Express Polym. Lett.

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Abstract. Poly(butylene succinate) (PBS) is currently developing due to its biodegradability and the similarity of its mechanical properties to those of polyolefins. Relationships between the number average molar mass, M n -, and solution viscosity such as [!] and ! red were derived for this aliphatic polyester. M n -values were determined by end-group analysis and size exclusion chromatography (SEC). Mark-Houwink-Sakurada (MHS) parameters were proposed in two solvents and for the different molar masses and viscosity measurement methods. As an example, the MHS equations were respectively, [!] = 6.4·10 -4 ·M n 0.67 in chloroform and [!] = 7.1·10 -4 ·M n -0.69 in 50/50 wt% 1,2-dichlorobenzene/phenol at 25°C for molar masses measured by SEC in hexafluoro isopropanol (HFIP) with poly(methyl methacrylate) (PMMA) standards. Empirical relationships were also suggested to derive M n -directly from reduced viscosity, ! red , which is much easier to determine than intrinsic viscosity. With these data, the number average molar mass of PBS can be conveniently estimated from a single viscosity measurement. In addition, it was shown that PBS contains 1-2 wt% of cyclic oligomers produced during esterification and that molar masses determined by taking this fraction into account or not were significantly different, especially for long chains.

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Section: End-groups Analysis Taking Into Account Cyclic Oligomersmentioning

confidence: 99%

Section: Comparison Of Molar Mass Data Obtained By 1 H-nmr and Secmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Solution viscosity – molar mass relationships for poly(butylene succinate) and discussion on molar mass analysis

Charlier¹,

Girard²,

Freyermouth³

et al. 2015

Express Polym. Lett.

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show abstract

“…When at identical molar mass the hydrodynamic volume of a polyester is greater than that of polystyrene, the polyester pretends to have a higher molar mass. It is well known from the work of several research groups that calibration with polystyrene overestimates the molecular weights of aliphatic or semi‐aliphatic polyesters by 50–80% . This effect is usually more pronounced in chloroform than in THF.…”

Section: How To Evaluate Sec Measurements?mentioning

confidence: 99%

Cyclization and Dispersity of Polyesters

Kricheldorf

Weidner

Scheliga

2017

Macromolecular Symposia

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Two classes of polyesters were prepared by irreversible polycondensations. The dependence of the dispersities on the experimental parameters such as synthetic method, chemical structure, molecular weight and initial monomer concentration was determined. At first it was demonstrated that it is essential for a correct calculation of Mn and Mw to include all oligomers down to the dimers in the evaluation of SEC curves. Furthermore, it was demonstrated for poly(ϵ‐caprolactone)s and polylactides that reversible polycondensations and ring‐opening polymerizations with equilibration yield identical products. Finally, the dependence of the dispersity on various experimental parameters was determined for equilibrated poly(ϵ‐caprolactone)s and polylactides.

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“…Studies on aliphatic polyesters is dated back to 1930s . According to their chemical structure, aliphatic polyesters may be subdivided into two classes: one is prepared from hydroxyl acids by ring‐opening polymerization and another is based on alkanedios and aliphatic dicarboxylic acids by ploycondensation processes . In general, the synthesis is commercially produced by the melt polycondensation of aliphatic dicarboxylic acid and diol compounds at 200 to 250 °C under highly reduced pressure…”

Section: Introductionmentioning

confidence: 99%

Heterogeneous catalytic synthesis of poly(butylene succinate) by attapulgite‐supported Sn catalyst

Hin

Gao

2014

J of Applied Polymer Sci

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An attapulgite-supported Sn catalyst (Sn-palgorskite) was successfully prepared by ion-exchange co-impregnation method. The catalytic effect of Sn-attapulgite on the melt polycondensation reaction of poly(butylene succinate) (PBS) was examined by comparing with that of anhydrous SnCl 2 and a blank experiment. The structures and properties of the PBS products synthesized with the three catalytic systems were characterized by means of Fourier transform-infrared spectra (FT-IR), viscosity measurements, wide angle X-ray diffraction (WARD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Meanwhile, the acidolysis degradation behaviors of the PBS samples were also studied. It was found that the intrinsic viscosities and the number-average molecular weights of the PBS were remarkably increased under the catalysis of Sn-attapulgite, further leading to an increase in the decomposition temperature, the crystallization temperature, and the viscous flow activation energy, while a decrease in the melting temperature, the relative degree of crystallinity, and the rate of degradation. Additionally, no significant differences were observed in the crystal structures of all the samples, regardless of the reaction system with or without catalyst. The experiment results confirmed that Sn-attapulgite was an effective heterogeneous catalyst for the synthesis of PBS, and the recycled Sn-attapulgite still exhibited higher activity than anhydrous SnCl 2 under identical reaction conditions.

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Syntheses of Poly(butylene succinate) by Means of Non-Toxic Catalysts

Cited by 15 publications

References 29 publications

Solution viscosity – molar mass relationships for poly(butylene succinate) and discussion on molar mass analysis

Solution viscosity – molar mass relationships for poly(butylene succinate) and discussion on molar mass analysis

Cyclization and Dispersity of Polyesters

Heterogeneous catalytic synthesis of poly(butylene succinate) by attapulgite‐supported Sn catalyst

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