Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization

The selective separation of ions is a major technological challenge having far-ranging impacts from product separation in electrochemical production of base chemicals from CO2 to water purification. In recent years, ion-selective electrochemical systems leveraging redox-materials emerged as an attra...

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Main Authors: Sevgi Polat, Ruud Kortlever, Huseyin Burak Eral
Format: Article
Language:English
Published: Elsevier 2022-09-01
Series:Ultrasonics Sonochemistry
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S1350417722002425
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author Sevgi Polat
Ruud Kortlever
Huseyin Burak Eral
author_facet Sevgi Polat
Ruud Kortlever
Huseyin Burak Eral
author_sort Sevgi Polat
collection DOAJ
description The selective separation of ions is a major technological challenge having far-ranging impacts from product separation in electrochemical production of base chemicals from CO2 to water purification. In recent years, ion-selective electrochemical systems leveraging redox-materials emerged as an attractive platform based on their reversibility and remarkable ion selectivity. In the present study, we present an ultrasound-intensified fabrication process for polyvinyl ferrocene (PVF)–functionalized electrodes in a carbon nanotube (CNT) matrix for selective electro-adsorption of formate ions. To this end, a response surface methodology involving the Box–Behnken design with three effective independent variables, namely, PVF to CNT ratio, sonication duration, and ultrasonic amplitude was applied to reach the maximum formate adsorption efficiency. The fabricated electrodes were characterized using cyclic voltammetry, X-ray diffraction, Raman spectroscopy, and scanning electron microscopy (SEM). SEM images revealed that an optimized ultrasonic amplitude and sonication time provided remarkable improvements in electrode morphology. Through a sedimentation study, we qualitatively demonstrate that the main optimized conditions improved PVF/CNT dispersion stability, consequently providing the highest number of active surface sites for adsorption and the highest adsorption efficiency. The highest percentage of active electrode surface sites and the maximum adsorption efficiency were 97.8 and 90.7% respectively at a PVF/CNT ratio of 3, ultrasonication time of one hour, and 50% ultrasonic amplitude.
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spelling doaj.art-94530c96011f4e548ec61632650559ac2022-12-22T04:30:55ZengElsevierUltrasonics Sonochemistry1350-41772022-09-0189106146Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimizationSevgi Polat0Ruud Kortlever1Huseyin Burak Eral2Complex Fluid Processing Section, Process & Energy Department, Faculty of Mechanical, Maritime and Materials Engineering, Delft University of Technology, 2628 CB Delft, The Netherlands; Chemical Engineering Department, Faculty of Engineering, Marmara University, 34854 İstanbul, Turkey; Corresponding authors at: Complex Fluid Processing Section, Process & Energy Department, Faculty of Mechanical, Maritime and Materials Engineering, Delft University of Technology, 2628 CB Delft, The Netherlands.Large-Scale Energy Storage Section, Process & Energy Department, Faculty of Mechanical, Maritime and Materials Engineering, Delft University of Technology, 2628 CB Delft, The NetherlandsComplex Fluid Processing Section, Process & Energy Department, Faculty of Mechanical, Maritime and Materials Engineering, Delft University of Technology, 2628 CB Delft, The Netherlands; Corresponding authors at: Complex Fluid Processing Section, Process & Energy Department, Faculty of Mechanical, Maritime and Materials Engineering, Delft University of Technology, 2628 CB Delft, The Netherlands.The selective separation of ions is a major technological challenge having far-ranging impacts from product separation in electrochemical production of base chemicals from CO2 to water purification. In recent years, ion-selective electrochemical systems leveraging redox-materials emerged as an attractive platform based on their reversibility and remarkable ion selectivity. In the present study, we present an ultrasound-intensified fabrication process for polyvinyl ferrocene (PVF)–functionalized electrodes in a carbon nanotube (CNT) matrix for selective electro-adsorption of formate ions. To this end, a response surface methodology involving the Box–Behnken design with three effective independent variables, namely, PVF to CNT ratio, sonication duration, and ultrasonic amplitude was applied to reach the maximum formate adsorption efficiency. The fabricated electrodes were characterized using cyclic voltammetry, X-ray diffraction, Raman spectroscopy, and scanning electron microscopy (SEM). SEM images revealed that an optimized ultrasonic amplitude and sonication time provided remarkable improvements in electrode morphology. Through a sedimentation study, we qualitatively demonstrate that the main optimized conditions improved PVF/CNT dispersion stability, consequently providing the highest number of active surface sites for adsorption and the highest adsorption efficiency. The highest percentage of active electrode surface sites and the maximum adsorption efficiency were 97.8 and 90.7% respectively at a PVF/CNT ratio of 3, ultrasonication time of one hour, and 50% ultrasonic amplitude.http://www.sciencedirect.com/science/article/pii/S1350417722002425Electrochemical separationsUltrasoundRedox electrodeOptimizationExperimental design
spellingShingle Sevgi Polat
Ruud Kortlever
Huseyin Burak Eral
Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization
Ultrasonics Sonochemistry
Electrochemical separations
Ultrasound
Redox electrode
Optimization
Experimental design
title Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization
title_full Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization
title_fullStr Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization
title_full_unstemmed Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization
title_short Ultrasound-promoted preparation of polyvinyl ferrocene-based electrodes for selective formate separation: Experimental design and optimization
title_sort ultrasound promoted preparation of polyvinyl ferrocene based electrodes for selective formate separation experimental design and optimization
topic Electrochemical separations
Ultrasound
Redox electrode
Optimization
Experimental design
url http://www.sciencedirect.com/science/article/pii/S1350417722002425
work_keys_str_mv AT sevgipolat ultrasoundpromotedpreparationofpolyvinylferrocenebasedelectrodesforselectiveformateseparationexperimentaldesignandoptimization
AT ruudkortlever ultrasoundpromotedpreparationofpolyvinylferrocenebasedelectrodesforselectiveformateseparationexperimentaldesignandoptimization
AT huseyinburakeral ultrasoundpromotedpreparationofpolyvinylferrocenebasedelectrodesforselectiveformateseparationexperimentaldesignandoptimization