SINE 2020 – Chemical Deuteration WP FZJ Contributions

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Presentation transcript:

SINE 2020 – Chemical Deuteration WP FZJ Contributions Jürgen Allgaier Jülich Centre for Neutron Science JCNS and Institute for Complex Systems ICS Forschungszentrum Jülich GmbH

Tasks Novel route for isoprene synthesis (D5.3, month 15) Synthesis of deuterium labelled polythiophene based block copolymers (D5.5, month 20) Synthesis of deuterium labelled polylactic acid (D5.8, month 30) (Synthesis of L- and D-lactic acid, ESS deliverable D5.4) (PEG/PEGylated lipids, D5.11)

Novel route for isoprene synthesis accessibility/costs of starting compounds monomer purity deuteration degree

Synthesis of deuterium labelled polythiophene based block copolymers 1. GRIM Polymerization of P3HT

Synthesis of deuterium labelled polythiophene based block copolymers 2. Diblocks P3HT: structural quality, chemical functionalization impurities: homopolymers, salts deuteration scenarios

Synthesis of deuterium labelled polylactic acid lactic acid (h and d): ESS lactide: FZJ poly(lactic acid): RWTH (Prof. Okuda)

Synthesis of deuterium labelled polylactic acid Lactide synthesis D-lactic acid (h), 10g 52% LA, 48% open dimer 28% water LA open dimer, 1H

Synthesis of deuterium labelled polylactic acid Conversion to lactide Purification by sublimation, recrystallization: (yield: 2g, 35%) lactide open dimer, 1H open dimer, 1H LA

THF; 18 h; ambient temperature Synthesis of deuterium labelled polylactic acid Polymerization (Dr. Beckerle, RWTH) [ZnEt2]/[BnOH]/[L-Lactide] 1 / 2 / 100 Mn D GPC (RI) 10 800 1.15 Corrected 6 300 - Calculated 6 900 THF; 18 h; ambient temperature 96 % conversion (NMR) 13C{1H}NMR iii iis/ sii isi

PEG Polymerization of EO (h and d) End group functionalization

PEG Synthesis of maleimide functionalized PEGs