Combined in-situ small and wide-angle synchrotron x-ray scattering (SAXS-WAXS) applied to a solid-state polymerization reaction

Herzberg, Oliver; Gehrke, Rainer; Epple, Matthias

doi:10.1016/s0032-3861(98)00328-0

Cited by 16 publications

(10 citation statements)

References 24 publications

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“…[76] ) Small-and wide-angle yes structural order on sodium chloroacetate no detectable intermediates on all length scales; X-ray scattering different length scales formation of short-range order in polyglycolide precedes (SAXS-WAXS) formation of long-range order (long period of amorphous and crystalline domains) (see ref. [80] ) Solid-state NMR ( 13 C) yes chemical environment of carbon sodium bromoacetate no detectable intermediates containing carbon (see ref. [58] ) Solid-state NMR ( 23 Na) yes chemical environment of sodium sodium chloroacetate; no detectable intermediates containing sodium (see ref.…”

Section: Poly(hydroxypropionates) By Solid-state Reactionmentioning

confidence: 99%

Formation of Polyesters by Thermally Induced Polymerization Reactions of Molecular Solids

Herzberg

Epple

2001

Eur. J. Inorg. Chem.

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The development of solid‐state polycondensation reactions, starting in 1857, is reviewed. In many cases, the elimination of metal halides from halogenated carboxylates leads to the formation of polyesters, among them polyglycolide, polylactides, polybutyrates, polymandelide, and poly(hydroxymethyl benzoates). In some cases, a reaction in the solid state is observed, whereas in other cases temporary liquefaction occurs. The resulting polymers usually have a lower degree of polymerization than the products from solution‐ or melt‐polymerization. In some cases, polymers with a distinct micromorphology (high porosity with pores in the sub‐µm range) are obtained and may be of interest for special applications, e.g. in medical technology.

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Section: Poly(hydroxypropionates) By Solid-state Reactionmentioning

confidence: 99%

Formation of Polyesters by Thermally Induced Polymerization Reactions of Molecular Solids

Herzberg

Epple

2001

Eur. J. Inorg. Chem.

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“…[20,74] ) X-ray diffraction (XRD) yes crystalline phases sodium chloroacetate no detectable crystalline intermediates (see ref. [80] ) Solid-state NMR ( 13 C) yes chemical environment of carbon sodium bromoacetate no detectable intermediates containing carbon (see ref. [74] ) EXAFS yes short-range order (Br, Rb rubidium bromoacetate/ desolvation is followed by polymerization in all phases bromoacetic acid (see ref.…”

Section: Poly(hydroxypropionates) By Solid-state Reactionmentioning

confidence: 99%

Formation of Polyesters by Thermally Induced Polymerization Reactions of Molecular Solids

Herzberg

Epple

2001

Eur. J. Inorg. Chem.

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“…In situ experiments allowed verification of the phase at which the reaction proceeds. Techniques like X‐ray spectroscopy (EXAFS),2 X‐ray diffraction,2, 3 infrared (IR) spectroscopy,4 and small‐angle X‐ray scattering5 were applied. In this way, a reaction of sodium chloroacetate was postulated to occur in the solid state with no detectable intermediate phases involved when the temperature was maintained between 120 and 140°C 6.…”

Section: Introductionmentioning

confidence: 99%

Copolymerization of potassium chloroacetate and potassium N‐chloroacetyl‐6‐aminohexanoate

Murase

Franco

Rodríguez‐Galán

et al. 2012

J of Applied Polymer Sci

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The polymerization kinetics of potassium chloroacetate (MGL), potassium N‐chloroacetyl‐6‐aminohexanoate (MEA), and their mixtures was studied by Fourier transform infrared spectroscopy. The bulk polycondensation reaction was faster for MEA than for MGL but kinetic differences in the selected temperature range (110–130°C) were not large enough to make unfeasible copolymerization of both monomers. A decrease in the activation energy was deduced for the polycondensation of monomer mixtures with respect to that determined for the homopolymerization reaction of the predominant neat monomer. differential scanning calorimetry data also showed significant differences in the exothermic polycondensation peaks that suggested an effective copolymerization reaction and favored the kinetic process over the corresponding homopolymerization. The resulting new poly(ester amide)s were characterized by spectroscopy and thermal analysis. 1H NMR spectra of samples with high MEA content revealed the existence of hetero‐sequences whose ratio was slightly lower than that expected for a random polymerization of the two monomers. Samples with high molecular weights were only attained when the MGL molar ratio in the monomer mixture was lower than 65%. Calorimetric data showed that all samples were thermally stable and became amorphous for intermediate compositions. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012

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Combined in-situ small and wide-angle synchrotron x-ray scattering (SAXS-WAXS) applied to a solid-state polymerization reaction

Cited by 16 publications

References 24 publications

Formation of Polyesters by Thermally Induced Polymerization Reactions of Molecular Solids

Formation of Polyesters by Thermally Induced Polymerization Reactions of Molecular Solids

Formation of Polyesters by Thermally Induced Polymerization Reactions of Molecular Solids

Copolymerization of potassium chloroacetate and potassium N‐chloroacetyl‐6‐aminohexanoate

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