Additional file 1 of Electroreduction of divanillin to polyvanillin in an electrochemical flow reactor
Creators: name: Kunkel, Robin
name: Fath, Maximilian
name: Schmiedl, Detlef
name: Schmidt, Volkmar M.
name: Tübke, Jens
Publisher: name: figshare
Year: 2024
Subjects: subject: Biochemistry
subject: Physical Sciences not elsewhere classified
subject: Biotechnology
subject: Chemical Sciences not elsewhere classified
subject: Immunology
subject: FOS: Clinical medicine
subject: Biological Sciences not elsewhere classified
subject: Plant Biology
subject: FOS: Biological sciences

description: Additional file 1. Isolated yields of polyvanillin, additional CVs of Zn cathode after resting phase in OCP, CVs of RDE experiments, detailed calculation of the limiting current density, conversion and Faradaic efficiency plots versus charge of the impact of the current density, 2D-NMR spectra of the polyvanillin samples and results of selected peak integrations as well as additional data of the high divanillin concentration attempt. Table S1. Isolated yield of polyvanillin after acidification of the catholyte to pH = 2 electrolyte. Table S2. Methoxy group normalized 1H-peak areas of the terminal alcohol and stilbene groups of the 2D-NMR spectra. Parameters: 50 mM initial divanillin concentration, 8 F mol−1, 20 cm s−1. Figure S1. CVs of Zn-cathode in 1 M NaOH after a resting phase of 10 min each in OCP. Four consecutive rounds were conducted, which are indicated by the round number displayed in the corresponding graph. Parameters: Undivided beaker cell (50 mL of electrolyte – 1 M NaOH), RT, WE: 5 cm2 Zn-piece, CE: 1.5 cm2 Pt-piece, REF: RHE (Fa. Gaskatel), CVs are corrected by iR-drop (0.4 Ohm determined via PEIS), 3 cycles -0.45 V vs. RHE to -1.1 V vs. RHE with 20 mV s−1. Figure S2. a Exemplary CVs of divanillin in 1 M NaOH measured at the RDE on a Pb disc with a potential sweep rate of 10 mV s−1. b Levich-plot for determination of the diffusion coefficient of divanillin in 1 M NaOH. Limiting current densities were extracted at − 0.9 V vs. RHE. Figure S3. Impact of current density on concentration courses. Inlaid plot in shows concentration course of the 9 and 18 mA cm−2 experiments on a logarithmic y-axis. Parameters: 50 mM initial divanillin concentration, 20 cm s−1, 8 F mol−1. Figure S4. Impact of current density on Faradaic efficiency courses (assuming 100% pinacolization). Parameters: 50 mM initial divanillin concentration, 20 cm s−1, 8 F mol−1. Figure S5. 2D-NMR (HSQC, 13C/1H) spectra of isolated polyvanillin after an applied charge of a 2 F mol−1, which partly precipitated, and b 8 F mol−1. Parameters: 50 mM initial divanillin concentration, 9 mA cm−2, 20 cm s−1 and γ = 0.5. Solvent was pyridin-d5. Figure S6. 2D-NMR (HSQC, 13C/1H) spectra of isolated polyvanillin after an applied charge of 8 F mol−1 synthesized at a current density of a 9 mA cm−2 and b 18 mA cm−2. Parameters: 50 mM initial divanillin concentration, 20 cm s−1. Solvent was pyridin-d5. Figure S7. Molecular weight distributions of the low and high concentration experiment. Parameters: 20 cm s−1. Figure S8. Space–time-yields STY and specific energy consumption ES courses for the high concentration (300 mM) and high current density (54 mA cm−2) experiment. For comparison the low concentration (50 mM) and low current density (9 mA cm−2) experiment of the same dimensionless current density of γ = 0.5 is shown. Parameters: 20 cm s−1.