Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity

A simple flow system employing a reversible-flow syringe pump was employed to synthesize uniform micron-size particles of chitosan-Cu(II) (CS-Cu(II)) catalyst. A solution of chitosan and Cu(II) salt was drawn into a holding coil via a 3-way switching valve and then slowly pumped to drip into an alka...

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Main Authors: Apichai Intanin, Prawpan Inpota, Threeraphat Chutimasakul, Jonggol Tantirungrotechai, Prapin Wilairat, Rattikan Chantiwas
Format: Article
Language:English
Published: MDPI AG 2020-04-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/25/8/1798
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author Apichai Intanin
Prawpan Inpota
Threeraphat Chutimasakul
Jonggol Tantirungrotechai
Prapin Wilairat
Rattikan Chantiwas
author_facet Apichai Intanin
Prawpan Inpota
Threeraphat Chutimasakul
Jonggol Tantirungrotechai
Prapin Wilairat
Rattikan Chantiwas
author_sort Apichai Intanin
collection DOAJ
description A simple flow system employing a reversible-flow syringe pump was employed to synthesize uniform micron-size particles of chitosan-Cu(II) (CS-Cu(II)) catalyst. A solution of chitosan and Cu(II) salt was drawn into a holding coil via a 3-way switching valve and then slowly pumped to drip into an alkaline solution to form of hydrogel droplets. The droplets were washed and dried to obtain the catalyst particles. Manual addition into the alkaline solution or employment of flow system with a vibrating rod, through which the end of the flow line is inserted, was investigated for comparison. A sampling method was selected to obtain representative samples of the population of the synthesized particles for size measurement using optical microscopy. The mean sizes of the particles were 880 ± 70 µm, 780 ± 20 µm, and 180 ± 30 µm for the manual and flow methods, without and with the vibrating rod, respectively. Performance of the flow methods, in terms of rate of droplet production and particle size distribution, are discussed. Samples of 180 µm size CS-Cu(II) particles were tested for catalytic reduction of 0.5 mM <i>p</i>-nitrophenol to <i>p</i>-aminophenol by 100-fold excess borohydride. The conversion was 98% after 20 min, whereas without the catalyst there was only 14% conversion.
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spelling doaj.art-c64e88b47a8a442ab0bb501d4ce9fac72023-11-19T21:37:11ZengMDPI AGMolecules1420-30492020-04-01258179810.3390/molecules25081798Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of ActivityApichai Intanin0Prawpan Inpota1Threeraphat Chutimasakul2Jonggol Tantirungrotechai3Prapin Wilairat4Rattikan Chantiwas5Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahidol University, Rama VI Rd., Bangkok 10400, ThailandDepartment of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahidol University, Rama VI Rd., Bangkok 10400, ThailandDepartment of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahidol University, Rama VI Rd., Bangkok 10400, ThailandDepartment of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahidol University, Rama VI Rd., Bangkok 10400, ThailandNational Doping Control Centre, Mahidol University, Rama VI Rd., Bangkok 10400, ThailandDepartment of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahidol University, Rama VI Rd., Bangkok 10400, ThailandA simple flow system employing a reversible-flow syringe pump was employed to synthesize uniform micron-size particles of chitosan-Cu(II) (CS-Cu(II)) catalyst. A solution of chitosan and Cu(II) salt was drawn into a holding coil via a 3-way switching valve and then slowly pumped to drip into an alkaline solution to form of hydrogel droplets. The droplets were washed and dried to obtain the catalyst particles. Manual addition into the alkaline solution or employment of flow system with a vibrating rod, through which the end of the flow line is inserted, was investigated for comparison. A sampling method was selected to obtain representative samples of the population of the synthesized particles for size measurement using optical microscopy. The mean sizes of the particles were 880 ± 70 µm, 780 ± 20 µm, and 180 ± 30 µm for the manual and flow methods, without and with the vibrating rod, respectively. Performance of the flow methods, in terms of rate of droplet production and particle size distribution, are discussed. Samples of 180 µm size CS-Cu(II) particles were tested for catalytic reduction of 0.5 mM <i>p</i>-nitrophenol to <i>p</i>-aminophenol by 100-fold excess borohydride. The conversion was 98% after 20 min, whereas without the catalyst there was only 14% conversion.https://www.mdpi.com/1420-3049/25/8/1798flow methodchitosancatalyst particlesmicron-sizesampling study<i>p</i>-nitrophenol reduction
spellingShingle Apichai Intanin
Prawpan Inpota
Threeraphat Chutimasakul
Jonggol Tantirungrotechai
Prapin Wilairat
Rattikan Chantiwas
Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity
Molecules
flow method
chitosan
catalyst particles
micron-size
sampling study
<i>p</i>-nitrophenol reduction
title Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity
title_full Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity
title_fullStr Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity
title_full_unstemmed Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity
title_short Development of a Simple Reversible-Flow Method for Preparation of Micron-Size Chitosan-Cu(II) Catalyst Particles and Their Testing of Activity
title_sort development of a simple reversible flow method for preparation of micron size chitosan cu ii catalyst particles and their testing of activity
topic flow method
chitosan
catalyst particles
micron-size
sampling study
<i>p</i>-nitrophenol reduction
url https://www.mdpi.com/1420-3049/25/8/1798
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