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A hybrid microreactor/microwave high-pressure flow system of a novel concept design and its application to the synthesis of silver nanoparticles
Affiliation:1. Department of Materials and Life Sciences, Faculty of Science and Technology, Sophia University, 7-1 Kioicho, Chiyodaku, Tokyo 102-8554, Japan;2. Gruppo Fotochimico, Dipartimento di Chimica, Universita di Pavia, via Taramelli 10, Pavia 27100, Italy;1. National Engineering Laboratory for Textile Fiber Materials and Processing Technology (Zhejiang), School of Materials Science and Engineering, Zhejiang Sci–Tech University, Hangzhou 310018, China;2. State Key Laboratory of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China;1. Laboratory of Chemical Reactor Engineering, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven, The Netherlands;2. Unité de Catalyse et de Chimie du Solide, UMR 8181 CNRS, Bât. C3, Université Lille, ENSCL, Ecole Centrale de Lille, 59655 Villeneuve d’Ascq, France;1. Process & Energy Department, Delft University of Technology, Leeghwaterstraat 39, Delft, 2628 CB, The Netherlands;2. K.N. Toosi University of Technology, Shariati Ave., Tehran, Iran;1. School of Chemical Engineering, Sichuan University, Chengdu, Sichuan 610065, China;2. State Key Laboratory of Polymer Materials Engineering, Sichuan University, Chengdu, Sichuan 610065, China;3. State Key Laboratory of Separation Membranes and Membrane Processes, Tianjin Polytechnic University, Tianjin 300187, China;4. Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing, Jiangsu 211816, China;1. National Local Joint Laboratory of Engineering Application of Microwave Energy and Equipment Technology, Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming 650093, PR China;2. Mechanical Engineering, University of Washington, Seattle, WA 98195, USA;3. Chemical Engineering Program, The Petroleum Institute, Abu Dhabi, P.O. Box 253, United Arab Emirates
Abstract:This article reports on a microreactor/microwave high-pressure flow hybrid apparatus of a novel concept design, which includes both the microreactor and a spiral reactor, and its efficient use in the synthesis of silver nanoparticles of relatively uniform sizes (4.3 ± 0.7 nm) under microwave irradiation. By contrast, under otherwise identical experimental conditions but with conventional heating, the nanoparticle size was non-uniform (8.3 ± 2.7 nm) and the spiral reactor walls were covered with a silver mirror deposit. Formation of the nanoparticles was monitored by UV–visible spectroscopy (plasmonic absorption band; LSPR), TEM and by small-angle X-ray scattering (SAXS). Both the spiral microreactor and the spiral quartz reactor of the hybrid system played an important role in the synthesis, with the microreactor providing the environment wherein mixing of the aqueous solution of Ag(NH3)2]+ and the solution of glucose (the reducing agent) and poly(N-vinyl-2-pyrrolidone) (PVP; stabilizer/dispersing agent) occurred. The microwaves provided the thermal energy to effect a uniform growth of the silver nanoparticles at temperatures above 120 °C. Mixing the two solutions by conventional methods (no microreactor) failed to yield such nanoparticles even under microwave irradiation and no formation of a silver mirror occurred in the inner walls of the spiral reactor.
Keywords:Microreactor  Microwave  Nanoparticle  Flow chemistry  Small-angle X-ray scattering (SAXS)
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