Abstract
The electrochemical conversion of a spruce lignosulfonate into vanillin, at nickel anodes, was explored in previously unobtainable detail. A flow reactor (FM01), in a rig that permitted considerable variation of electrolysis conditions, allowed up to 150 g to be electrolysed at up to12 A at a variety of electrode configurations. Samples taken during electrolysis gave detailed reaction profiles. The electrolyser operated at 145 °C/500 kPa/3 M NaOH and yields of vanillin were similar to those obtained industrially using chemical oxidants (about 5–7% w/w). Vanillin production was favoured by low current density and low initial concentration of lignosulfonate. Vanillin, alone, was consumed in a 2.7 F process under the above conditions. Historically, yields in chemical and electrochemical conversions of lignins into vanillin do not exceed 10%; the results herein explain this apparent limit as equilibrium between formation of vanillin, its concomitant oxidative destruction and further condensation of lignins.
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Acknowledgments
The flow rig was designed by Dr J.K. Hammond (ICI) and it centred on an FM01-LC filter press flow reactor (donated by ICI). Components, including Expamet and Retimet nickel electrodes, were donated by ICI and the rig was constructed in The Queen Mary Faculty of Science Mechanical Workshop under the supervision of Mr F. Hands. We are also grateful for substantial financial and material support from Borregaard Industries Ltd., PO Box 162, N-1701 Sarpsborg, Norway and for crucial help and discussions with Dr Hans Evju of that company.
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John K. Hammond—formerly of ICI Chemicals and Polymers Ltd.
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Smith, C.Z., Utley, J.H.P. & Hammond, J.K. Electro-organic reactions. Part 60[1]. The electro-oxidative conversion at laboratory scale of a lignosulfonate into vanillin in an FM01 filter press flow reactor: preparative and mechanistic aspects. J Appl Electrochem 41, 363–375 (2011). https://doi.org/10.1007/s10800-010-0245-0
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DOI: https://doi.org/10.1007/s10800-010-0245-0