MILESTONE. RotoSYNTH. Rotative Solid-Phase Microwave Reactor

Rotative Solid-Phase Microwave Reactor

RotoSYNTH

MILESTONE

H E L P I N G

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.

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.

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.

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.

Limitations of the

‘conventional’ laboratory microwave reactors

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. 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

Product yield (%)

» 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

Typical applications

Formation of crystalline nanoparticles

Microwave promoted synthesis of LaPO4: Ce; IL: [N(t-Bu)3(Me)][N(SO2CF3)2]

G. Buhler, M. Stay. C. Feldmann, Green Chemistry, 9, 2007, 924.

LaCl₃ dissolved in IL / EtOH Precipitation of nanoparticles Barely crystalline nanoparticles in pure IL Crystalline nanoscale LAPO₄ : Ce H₃PO₄ dissolved in IL/EtOH Added at 70°C 1 - MW, 10-30 s, 300 °C 2 - Washing Centrifugation Evaporation of EtOH

K.M. Amore, N.E. Leadbeater, Macromolecular Rapid Communication, 28, 2007, 473.

» 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

Microwave hardware

• Single magnetron system with rotating diffuser for homogeneous microwave distribution in the cavity.

• Magnetron protected from reflected microwave power. • 1200 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.

Specifications are subject to change without notice.

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.

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 65.000 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.

CAT302EN-002

MILESTONE Srl - Via Fatebenefratelli, 1/5 - 24010 Sorisole (BG) - Italy

Tel: +39 035 573857 - Fax: +39 035 575498

www.milestonesrl.com - email: [email protected]

MILESTONE INC. - 25 Controls Drive - Shelton, CT 06484 - USA

Tel: (203) 925-4240 - Toll-free: (866) 995-5100 - Fax: (203) 925-4241 www.milestonesci.com - email: [email protected]

MILESTONE GENERAL K.K. - KSP, 3-2-1, Sakado - Takatsu-Ku,

Kawasaki 213-0012 - Japan - Tel: +81 (0)44 850 3811 - Fax: +81 (0)44 819 3036 www.milestone-general.com - email: [email protected]

MLS GmbH - Auenweg 37 D-88299 Leutkirch im Allgau - Germany

Tel: +49 (0)7561 9818-0 - Fax: +49 (0)7561 9818-12 www.mls-mikrowellen.de - email: [email protected]

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