WP 1 : Ultrasound

1. Tom Van Gerven WP 1 : Ultrasound 1st progress meeting Amersfoort, 08.07.2013

2. Objectives last 6 months • Overall objective: development of tailored equipment for ultrasound-assisted multiphase processes (reactive synthesis and cooling crystallisation, reactive L/L extraction, VLE) • Objective 1st year: data generation for enabling local positioning of the ultrasound energy at the interfaces, and experimental determination of flow and temperature profiles

3. Progress & status quo • Task 1.1.1 Reactive extraction • Start up of Jinu John (KUL, April 1st, 2013) • Selection of solvents • Design of set-up

4. Progress & status quo • Task 1.1.2 Reactive synthesis and cooling crystallisation • Start up of Jeroen Jordens (KUL, January 1st), Bjorn Gielen (KUL, April 1st) and Rohit Kacker (TUD, April 1st) • First version flow and batch reactor operational and characterised • MSZW for paracetamol recorded at different frequencies, degradation of paracetamol being studied, PSD and crystal morphology preliminary data • Seeding crystals synthesized; primary nucleation time studied • US field characterisation in preparation

5. Progress & status quo • Task 1.1.3 VLE • Matthias Wierschem started PhD at TUDO in June • Dr. Gunjan Agrahari (PhD IIT Kanpur, India) starts at KUL on July 15 • Kolja Neuman starts PhD at TUDO in August

6. Main achievements • Extraction: selection of solvents • Variation of • Viscosity • Surface Tension • Vapour Pressure

7. Main achievements Extraction: design of set-up

8. Main achievements • Crystallisation: set-ups US generator and amplifier Cooling bath Batch reactor First-version flow reactor Saturated solution Use of water bath for sonication

9. Main achievements • Crystallisation: MSZW • Exchangeable bottom (transducer) • 8 W calorimetric power • Frequencies 40-1140 kHz • 20 g/L paracetamol in water • Start at 40°C • Cooling rate: 0.7°C/min

10. Main achievements • Crystallisation: MSZW • Decrease in effect of ultrasound on MSZW with increasing frequencies • Fastest nucleation at lowest frequency

11. Main achievements • Crystallisation: PSD

12. Main achievements • Crystallisation: seeding crystals With US: lots of crystals after 30 seconds Without US: few crystals after 15 minutes

13. Main achievements • Characterizationofthe US field in presentset-up • Effect of US on control of nucleation • High intensity focused at a point/region • Process Design: Use of water (waterbath) for impedance matching.

14. Main achievements • Second-version flow reactors Measurement acoustic properties Lambda/2 matching layer Lambda/4 reactor prototype PFA tube PP tube

15. Problems & deviations • Delayed start up of VLE work Three researchers have started and should deliver results in due time

16. Plan forthenext 6 months • Continue with data generation for crystallization (batch and continuous) at KUL and TUD • Pilot experiments with OBFC: in cooperation with JP • Set-up ready for extraction and generation of data • Dedicated flow reactor by SM ready for nucleation • Characterization methods for US field ready (PIV/PIT, T, chemiluminescence, etc.) and generation of data • Start up of VLE task; interaction foreseen between KUL and TUDO in august/september

17. Deliverables & milestones Deliverables for Year 1 • Set of experimental data available for comparison between US and non-US and for input to modelling • Start with modelling for process design and control Milestones • Month 12:set of experimental data available • Month 18: models for process design ready

18. Interactions withother WPs • Interaction with WP2 on: • Microwave evaporative crystallisation • Microwave VLE • Spill-overs to WP4&5 • Interaction between WP1 members: • Meeting in Leuven, April 8th, 2013 (KUL, TUD, SM, JP) • Meeting in Dresden, May 22nd, 2013 (KUL, TUD, SM) • Meeting Amersfoort, July 8th, 2013 (KUL, TUD, SM, JP) • Material and mails going back & forth frequently

19. Additional slides

20. MSZW