Browsing by Author "Steinmann, Mark"

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    Dual catalysis with an N‐heterocyclic carbene and a Lewis acid : thermally latent precatalyst for the polymerization of ε‐caprolactam
    (2020) Altmann, Hagen J.; Steinmann, Mark; Elser, Iris; Benedikter, Mathis J.; Naumann, Stefan; Buchmeiser, Michael R.
    So far, the earlier reported strong correlation between basicity of an N‐heterocyclic carbene (NHC) and its reactivity in poly(ε‐caprolactam) (PA6) synthesis resulted in a substantial limitation of applicable carbenes. Here, to overcome this issue, 1,3‐dimethylimidazolium‐2‐carboxylate, an easily accessible, air and moisture‐stable NHC, was applied as thermally latent initiator. In order to compensate for its low basicity, reactivity was enhanced by the addition of both a Lewis acid and an activator to ease the initial polymerization step. The resulting mixtures of ε‐caprolactam, the CO2‐protected NHC, a Lewis acid and N‐acylazepan‐2‐one constitute homogeneous, thermally fully latent “single‐component” blends for the anionic polymerization‐based synthesis of PA6. They can be stored both in the liquid and solid state for days and months, respectively, without any loss in activity. The role of the Lewis acid as well as technical implications of the prolonged pot‐times are discussed.
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    High‐performance carbon fibers prepared by continuous stabilization and carbonization of electron beam‐irradiated textile grade polyacrylonitrile fibers
    (2021) König, Simon; Bauch, Volker; Herbert, Christian; Wego, Andreas; Steinmann, Mark; Frank, Erik; Buchmeiser, Michael R.
    The manufacturing of high‐performance carbon fibers (CFs) from low‐cost textile grade poly(acrylonitrile) (PAN) homo‐ and copolymers using continuous electron beam (EB) irradiation, stabilization, and carbonization on a kilogram scale is reported. The resulting CFs have tensile strengths of up to 3.1 ± 0.6 GPa and Young's moduli of up to 212 ± 9 GPa, exceeding standard grade CFs such as Toray T300. Additionally, the Weibull strength and modulus, the microstructure, and the morphology of these CFs are determined.
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    Melt spinning of propylene carbonate‐plasticized poly(acrylonitrile)‐co‐poly(methyl acrylate)
    (2020) König, Simon; Kreis, Philipp; Reinders, Leonie; Beyer, Ronald; Wego, Andreas; Herbert, Christian; Steinmann, Mark; Frank, Erik; Buchmeiser, Michael R.
    The primary use of poly(acrylonitrile) (PAN) fibers, commonly referred to as acrylic fibers, is in textile applications like clothing, furniture, carpets, and awnings. All commercially available PAN fibers are processed by solution spinning; however, alternative, more cost‐effective processes like melt spinning are still highly desired. Here, the melt spinning of PAN‐co‐poly(methyl acrylate) (PMA) plasticized with propylene carbonate (PC) at 175°C is reported. The use of methyl acrylate (MA) as comonomer and PC as an external plasticizer renders the approach a combination of internal and external plasticization. Various mixtures of PAN and PC used in this work were examined by rheology, subjected to melt spinning, followed by discontinuous and continuous washing, respectively. The best fibers were derived from a PAN‐co‐PMA copolymer containing 8.1 mol‐% of MA having a number‐average molecular weight Mn of 34 000 g/mol, spun in the presence of 22.5 wt.‐% of PC. The resulting fibers were analyzed by scanning electron microscopy and wide‐angle X‐ray scattering (WAXS), and were subjected to mechanical testing.
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    Melt-spinning of an intrinsically flame-retardant polyacrylonitrile copolymer
    (2020) König, Simon; Kreis, Philipp; Herbert, Christian; Wego, Andreas; Steinmann, Mark; Wang, Dongren; Frank, Erik; Buchmeiser, Michael R.
    Poly(acrylonitrile) (PAN) fibers have two essential drawbacks: they are usually processed by solution-spinning, which is inferior to melt spinning in terms of productivity and costs, and they are flammable in air. Here, we report on the synthesis and melt-spinning of an intrinsically flame-retardant PAN-copolymer with phosphorus-containing dimethylphosphonomethyl acrylate (DPA) as primary comonomer. Furthermore, the copolymerization parameters of the aqueous suspension polymerization of acrylonitrile (AN) and DPA were determined applying both the Fineman and Ross and Kelen and Tüdõs methods. For flame retardancy and melt-spinning tests, multiple PAN copolymers with different amounts of DPA and, in some cases, methyl acrylate (MA) have been synthesized. One of the synthesized PAN-copolymers has been melt-spun with propylene carbonate (PC) as plasticizer; the resulting PAN-fibers had a tenacity of 195 ± 40 MPa and a Young’s modulus of 5.2 ± 0.7 GPa. The flame-retardant properties have been determined by Limiting Oxygen Index (LOI) flame tests. The LOI value of the melt-spinnable PAN was 25.1; it therefore meets the flame retardancy criteria for many applications. In short, the reported method shows that the disadvantage of high comonomer content necessary for flame retardation can be turned into an advantage by enabling melt spinning.