A new pilot flow reactor for high-intensity ultrasound irradiation. Application to the synthesis of biodiesel.

In recent years, chemistry in flowing systems has become more prominent as a method of carrying out chemical transformations, ranging in scale from microchemistry up to kilogram-scale processes. Compared to classic batch ultrasound reactors, flow reactors stand out for their greater efficiency and flexibility as well as lower energy consumption. This paper presents a new ultrasonic flow reactor developed in our laboratory, a pilot system well suited for reaction scale up. This was applied to the transesterification of soybean oil with methanol for biodiesel production. This reaction is mass-transfer-limited initially because the two reactants are immiscible with each other, then because the glycerol phase separates together with most of the catalyst (Na or K methoxide). In our reactor a mixture of oil (1.6 L), methanol and sodium methoxide 30% in methanol (wt/wt ratio 80:19.5:0.5, respectively) was fully transesterified at about 45 degrees C in 1h (21.5 kHz, 600 W, flow rate 55 mL/min). The same result could be achieved together with a considerable reduction in energy consumption, by a two-step procedure: first a conventional heating under mechanical stirring (30 min at 45 degrees C), followed by ultrasound irradiation at the same temperature (35 min, 600 W, flow rate 55 mL/min). Our studies confirmed that high-throughput ultrasound applications definitively require flow reactors.

[1]  Ernesto E. Borrero,et al.  Biodiesel from an alkaline transesterification reaction of soybean oil using ultrasonic mixing , 2005 .

[2]  Aniruddha B. Pandit,et al.  Mapping the cavitation intensity in an ultrasonic bath using the acoustic emission , 2000 .

[3]  Fabiano A.N. Fernandes,et al.  Optimization of the production of biodiesel from soybean oil by ultrasound assisted methanolysis , 2009 .

[4]  B. Ondruschka,et al.  Influence of Mass Transfer on the Production of Biodiesel , 2004 .

[5]  Y. Gonthier,et al.  Method for determining the chemically active zones in a high-frequency ultrasonic reactor , 1994 .

[6]  A. Wilhelm,et al.  Comparison of ultrasound effects in different reactors at 20 kHz. , 1998, Ultrasonics sonochemistry.

[7]  Ulrich Kunz,et al.  Design, modeling and performance of a novel sonochemical reactor for heterogeneous reactions , 1996 .

[8]  Stefano Mantegna,et al.  A new approach to the decontamination of asbestos-polluted waters by treatment with oxalic acid under power ultrasound. , 2008, Ultrasonics sonochemistry.

[9]  Stefano Mantegna,et al.  The combination of oxalic acid with power ultrasound fully degrades chrysotile asbestos fibres. , 2007, Journal of environmental monitoring : JEM.

[10]  Stefano Mantegna,et al.  Improved extraction of vegetable oils under high-intensity ultrasound and/or microwaves. , 2008, Ultrasonics sonochemistry.

[11]  N. Gondrexon,et al.  Degradation of pentachlorophenol aqueous solutions using a continuous flow ultrasonic reactor: experimental performance and modelling. , 1999, Ultrasonics sonochemistry.

[12]  Parag R Gogate,et al.  Mapping the efficacy of new designs for large scale sonochemical reactors. , 2007, Ultrasonics sonochemistry.

[13]  Shriniwas D. Samant,et al.  Semiquantitative characterization of ultrasonic cleaner using a novel piezoelectric pressure intensity measurement probe , 1995 .

[14]  T J Mason,et al.  Large scale sonochemical processing: aspiration and actuality. , 2000, Ultrasonics sonochemistry.

[15]  G. Cravotto,et al.  An improved sonochemical reactor. , 2005, Ultrasonics sonochemistry.

[16]  R. Hernandez,et al.  Base-Catalyzed Fast Transesterification of Soybean Oil Using Ultrasonication , 2007 .

[17]  Gilbert Casamatta,et al.  Local investigation of some ultrasonic devices by means of a thermal sensor , 1995 .

[18]  G. Cravotto,et al.  A new flow reactor for the treatment of polluted water with microwave and ultrasound , 2007 .

[19]  C. Stavarache,et al.  Fatty acids methyl esters from vegetable oil by means of ultrasonic energy. , 2005, Ultrasonics sonochemistry.

[20]  Steven V Ley,et al.  Microwave reactions under continuous flow conditions. , 2007, Combinatorial chemistry & high throughput screening.

[21]  Vijayanand S. Moholkar,et al.  Physical Mechanism of Ultrasound-Assisted Synthesis of Biodiesel , 2009 .

[22]  L. H. Thompson,et al.  Sonochemistry: Science and Engineering , 1999 .

[23]  Steven V. Ley,et al.  New tools and concepts for modern organic synthesis , 2002, Nature Reviews Drug Discovery.

[24]  Yasuaki Maeda,et al.  Biodiesel production by esterification of oleic acid with short-chain alcohols under ultrasonic irradiation condition , 2009 .

[25]  Parag R Gogate,et al.  Sonochemical reactors: scale up aspects. , 2004, Ultrasonics sonochemistry.

[26]  S. Umemura,et al.  Effect of second-harmonic superimposition on efficient induction of sonochemical effect , 1996 .

[27]  C. Gourdon,et al.  A comparative study of local sensors of power ultrasound effects: electrochemical, thermoelectrical and chemical probes. , 1998, Ultrasonics sonochemistry.

[28]  Y. Adewuyi,et al.  Optimization of the Synthesis of Biodiesel via Ultrasound-Enhanced Base-Catalyzed Transesterification of Soybean Oil Using a Multifrequency Ultrasonic Reactor , 2009 .

[29]  Philip Hodge,et al.  Synthesis of Organic Compounds Using Polymer-Supported Reagents, Catalysts, and/or Scavengers in Benchtop Flow Systems† , 2005 .

[30]  Colin J. Barrow,et al.  Transesterification of Fish Oil to Produce Fatty Acid Ethyl Esters Using Ultrasonic Energy , 2007 .