WP 1 : Ultrasound
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Transcript of WP 1 : Ultrasound
WP 1 : ULTRASOUNDTom Van Gerven
1st progress meetingAmersfoort, 08.07.2013
Objectives last 6 months
30.01.2013
• 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
Progress & status quo
30.01.2013
• Task 1.1.1 Reactive extraction– Start up of Jinu John (KUL, April 1st, 2013)– Selection of solvents– Design of set-up
Progress & status quo
30.01.2013
• 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
Progress & status quo
30.01.2013
• 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
Main achievements
30.01.2013
• Extraction: selection of solvents
Sl No Chemical NameViscosity
(25°C)Surface Tension (25°C)
VolatilitySp.
GravitySpeed of
sound (at 25°C)
Specific Acoustic ImpedanceVapour pr.
(21°C) Boiling point
cP N/m mm Hg °C at 20°C m/s Mrayl1 Toluene 0.59 0.0279 23.2 110.5 0.86 1330 1.144
2 Methyl Isobutyl Ketone 0.61 0.024 16.5 116 0.801 1222 0.979
3 2-methyl tetrahydrofuran 0.47 0.0246 155 79 0.86 1202 1.034
4 Chloroform 0.57 0.0267 169 61 1.48 979 1.449
5 Dichloromethane 0.44 0.0272 376 40 1.33 1070 1.423
6 2-Butanol 3.7 0.0225 13.2 99.5 0.807 1240 1.001
7 Cyclohexane 0.98 0.0246 78.8 81 0.778 1454 1.131
8 Carbon tertrachloride 0.97 0.0264 99.6 76 1.58 926 1.463
9 Cyclohexanone 2.2 0.0345 3.1 156 0.948 1423 1.349
10 Acetophenone 1.74 0.039 0.35 82 1.024 1492 1.528
11 Chlorobenzene 0.8 0.0323 9.5 132 1.106 1273 1.408
12 Hexane 0.31 0.0178 128 69 0.659 1112 0.733
13 Diisopropyl ether 0.33 0.018 123 68 0.724 976 0.707
14 Tributyl phosphate 3.88 0.0278 27 180 0.979 1272 1.245
Variation ofViscosity
Surface Tension
Vapour Pressure
Main achievements
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Extraction: design of set-up
Main achievements
30.01.2013
• Crystallisation: set-ups
Saturated solution
Use of water bath for sonication
US generator and amplifier
Cooling bath
First-version flow reactor
Batch reactor
Main achievements
30.01.2013
• 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
Main achievements
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• Crystallisation: MSZW
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SZW
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Frequency (kHz)
• Decrease in effect of ultrasound on MSZW with increasing frequencies• Fastest nucleation at lowest frequency
Main achievements
30.01.2013
• Crystallisation: PSD
Silent conditions SonicationMean diameter (µm) Span Mean diameter (µm) Span
Batch 447,63 0,9902 65,56 1,097
Milliflow 303,38 0,6888 25,96 1,365
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1090
DDDSpan
Main achievements
30.01.2013
• Crystallisation: seeding crystals
With US:lots of crystals after 30 seconds
Without US: few crystals after 15 minutes
Main achievements
30.01.2013
• Characterization of the US field in present set-up
o Effect of US on control of nucleationo High intensity focused at a point/region
o Process Design: Use of water (waterbath) for impedance matching.
Main achievements
30.01.2013
• Second-version flow reactorsMeasurement acoustic properties
Lambda/2matching layer
Lambda/4reactor prototype
PFA tube PP tube
Problems & deviations
30.01.2013
• Delayed start up of VLE workThree researchers have started and should deliver results in due time
Plan for the next 6 months
30.01.2013
• 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
Deliverables & milestones
30.01.2013
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
Interactions with other WPs
30.01.2013
• 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
Additional slides
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MSZW
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40-90 kHz transducer
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165kHz transducer
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Meinhardt transducer
silent
40.7 97.7 165 570 850 1140
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MSZ
W (°
C)Frequency (kHz)
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MSZ
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