MILESTONE. RotoSYNTH. Rotative Solid-Phase Microwave Reactor

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1 MILESTONE H E L P I N G C H E M I S T S RotoSYNTH Rotative Solid-Phase Microwave Reactor

2 RotoSYNTH benefits The benefits of microwave-enhanced synthesis Microwave enhanced chemistry represents a fundamental step forward in the capabilities of synthetic chemists. Since its introduction, it has allowed to run experiments faster than ever before and with higher yields, and to scale-up reactions reliably from milligrams to much larger quantities, without the need of reaction optimization. Today, microwave assisted synthesis has become a cutting-edge technology across the pharmaceutical, biotech, polymers, fine-and agro-chemical industries, with thousands of units installed worldwide.

3 RotoSYNTH features Limitations of the conventional laboratory microwave reactors Heating heterogeneous reaction mixtures, thick media or solid phase systems suffers of inhomogeneous temperature distribution and stirring difficulties using both, conventional heating systems or standard dedicated microwave instruments. The innovative Milestone RotoSYNTH, combines all the traditional advantages of microwave-enhanced synthesis, with the unique capability of physically rotate the reaction vessel, to achieve very homogenous bulk heating of slurries, viscous and solid reaction mixtures media and highly efficient mixing. Milestone unique RotoSYNTH system consists of a state-of-the-art microwave platform, with a 45 tilted rotating reaction vessel. Monitoring and controlling of the reaction temperature are assured by both, a contact-less infrared pyrometer and plus a contact optical fibre thermometer. Furthermore, the RotoSYNTH allows operations under normal atmosphere, inert gas, and under vacuum. The RotoSYNTH is fully controlled via a compact terminal, with bright, full-colour, touch-screen display. The dedicated software automatically reproduces a preset temperature/ time profile tuning the emitted microwave power. Methods and runs are saved on a flash memory card or on a USB stick and can be read on any Windows based computer. Moreover, using the Milestone EasyDOC software, all data can be graphically displayed and converted into standard formats readable by any database or spreadsheet software (Microsoft Excel, etc.). The RotoSYNTH system represents an excellent platform for both, method optimization and for scale-up, as it can host a number of accessories for sealed or reflux microwave synthesis with full control of all reaction parameters (time, microwave power, heating and cooling rate, temperature, pressure, and vacuum), in the safest working environment. The RotoSYNTH enables a continuous fast mixing of the solids, induced by the rotation of the vessel. Coupling this effect with microwave irradiation, it is possible to obtain very homogeneous temperature distribution.

4 RotoSYNTH applications Typical applications Solid phase synthesis, with or without solvent (dry media) Synthesis of inorganic materials Surface functionalization of glass and polymer beads Polymerization reactions under vacuum (Polycondensations) Dehydration of natural oils Coating of polymeric membranes Impregnation and functionalization of drug carriers Synthesis, Functionalization and Surface Treatment of Nanoparticles Large scale homogeneous phase reactions without hot spots Reactions under vacuum and protective or reactive atmosphere Drying of raw organic, inorganic and polymeric materials Synthesis, Functionalization and Surface Treatment of Nanoparticles Synthesis of biofuels Extraction of volatile active compounds Esterification reaction Using the Milestone RotoSYNTH, water is continuously removed from the reaction mixture, shifting the equilibrium toward the ester formation and improving the reaction yield. Alcohol 1-Octanol 1-Butanol 1-Propanol 2-Octanol Product yield (%) K.M. Amore, N.E. Leadbeater, Macromolecular Rapid Communication, 28, 2007, 473. Formation of crystalline nanoparticles Due to the unique rotative stirring and to the highly homogeneous and fast heating, the nanoparticles crystallization is almost instantaneous, resulting in anhydrous oxide materials with low defect concentration. LaCl 3 dissolved in IL / EtOH H 3 PO 4 dissolved in IL/EtOH Added at 70 C Precipitation of nanoparticles Evaporation of EtOH Barely crystalline nanoparticles in pure IL 1 - MW, s, 300 C 2 - Washing Centrifugation Crystalline nanoscale LAPO 4 : Ce Microwave promoted synthesis of LaPO 4 : Ce; IL: [N(t-Bu) 3 (Me)][N(SO 2 CF 3 ) 2 ] G. Buhler, M. Stay. C. Feldmann, Green Chemistry, 9, 2007, 924.

5 The RotoSYNTH benefits Homogeneous heating of solid material Efficient processing of slurries and thick reaction media Fast removal of volatile side-products Full control of all reaction parameters High flexibility of operation

6 RotoSYNTH technical specifications Microwave hardware Single magnetron system with rotating diffuser for homogeneous microwave distribution in the cavity. Magnetron protected from reflected microwave power Watt installed power. Up to 1200 Watt output power, controlled via microprocessor. Large microwave cavity of 37 x 34,5 x 33,5(h)cm. Cavity illumination. Microwave cavity entirely made of 18/8 stainless steel housing, with PTFE coating. All hardware protected against acids/organic solvents with polymer coating both on inside and outside surfaces. 7 micro-switches of which 4 safety interlocks to prevent microwave emission with door open. Exhaust located in the side of the cavity, separate from electronics to prevent corrosion. Reaction sensors Built-incontact-less infrared temperature sensor. Built-indirect fiber optic temperature sensor (opt.). Control terminal 6,5 industrial grade touch screen controller with colours. VGA resolution 640 x 480 dots for sharp process graphic. 1 USB port for printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices. Methods and reporting data saved on removable flashcard and USB pendrive. Reaction system 50 ml, 300 ml, 2000 ml glass vessels complete with cover, flange, mixing device, and support. NP Normal pressure glassware setup (opt.). SV and BSV quartz and PTFE vessels setup (opt.). Weight 75kg. External dimensions 57 x 51 x 61(h) cm. Power 220V/50-60Hz, 2,4kW. Specifications are subject to change without notice. MILESTONE MILESTONE Srl - Via Fatebenefratelli, 1/ Sorisole (BG) - Italy Tel: Fax: analytical@milestonesrl.com UNI EN ISO 9001: 2008 CERTIFIED In your country: H E L P I N G C H E M I S T S MILESTONE INC Controls Drive - Shelton, CT USA Tel: (203) Toll-free: (866) Fax: (203) mwave@milestonesci.com MILESTONE GENERAL K.K. - KSP, 3-2-1, Sakado - Takatsu-Ku, Kawasaki Japan - Tel: +81 (0) Fax: +81 (0) info@milestone-general.com CAT302EN-002 MLS GmbH - Auenweg 37 D Leutkirch im Allgau - Germany Tel: +49 (0) Fax: +49 (0) mws@mls-mikrowellen.de