Continuous Flow Reactions From idea to production size scale up in 3 steps PIN NL Spring Session 13 04 2017 13 4 2017 PIN NL Spring Session 1
Topics Introduction Flowlink Continuous Flow Reactions What is required? Fluitec Contiplant Modular Reaction System Process Concepts and Examples In 3 steps from Batch to Continuous Flow Production 13 4 2017 PIN NL Spring Session 2
Introduction Flowlink 13 4 2017 PIN NL Spring Session 3
Introduction Flowlink Engineered Micro Gear Pumps 13 4 2017 PIN NL Spring Session 4
Introduction Flowlink : Engineered Gear Pumps 13 4 2017 PIN NL Spring Session 5
Introduction Flowlink Mixers / Heat Exchangers & Systems 13 4 2017 PIN NL Spring Session 6
Introduction Flowlink Engineering & Systems 13 4 2017 PIN NL Spring Session 7
Continuous Flow Reactions What is required for continuous flow reactions? 13 4 2017 PIN NL Spring Session 8
Continuous Flow Reactions What is required for continuous flow reactions? Continuous addition of feed stock -> Dosing Interacting molecules - > Mixing Heating and/or Cooling-> Heat Transfer Selectivity / Residence Time Distribution -> Plug Flow Small scale testing / large scale production -> Scale-up 13-4-2017 PIN-NL Spring Session 9
Dosing Mixing Heat Transfer Plug Flow Scale-up Accurate Dosing 13 4 2017 PIN NL Spring Session Page 10
Dosing Mixing Heat Transfer Plug Flow Scale-up Mixing Turbulent flow Laminar flow 13 4 2017 PIN NL Spring Session Page 11
Dosing Mixing Heat Transfer Plug Flow Scale-up 13 4 2017 PIN NL Spring Session Page 12
Dosing Mixing Heat Transfer Plug Flow Scale-up 13 4 2017 PIN NL Spring Session Page 13
Dosing Mixing Heat Transfer Plug Flow Scale-up Plug Flow 13 4 2017 PIN NL Spring Session Page 14
Dosing Mixing Heat Transfer Plug Flow Scale-up Scale-up is carried out by increasing the number of tubes 13 4 2017 PIN NL Spring Session Page 15
Dosing Mixing Heat Transfer Plug Flow Scale-up 13 4 2017 PIN NL Spring Session Page 16
Dosing Mixing Heat Transfer Plug Flow Scale-up 13 4 2017 PIN NL Spring Session 17
Dosing Mixing Heat Transfer Plug Flow Scale-up Scale up of a Plug Flow Recycle Reactor PFRR with Residence Time Reactor 13 4 2017 PIN NL Spring Session 18
Continuous Flow Reactions Fluitec Contiplant Modular Reaction System Reaction Concepts Available Components Examples 13 4 2017 PIN NL Spring Session 19
Reaction Concepts Components Examples Fluitec Moduclar Reaction System 13 4 2017 PIN NL Spring Session 20
Reaction Concepts Components Examples Modular reactor system 6 points per reactor for connecting accessories Diameters vary form ø4,7 36 mm 13 4 2017 PIN NL Spring Session 21
Reaction Concepts Components Examples Redundant System CSTR + PFR 13 4 2017 PIN NL Spring Session 22
Reaction Concepts Components Examples High Viscous Loop Reactor with Distillation 13 4 2017 PIN NL Spring Session 23
Reaction Concepts Components Examples Bo > 65 A B Mixer / heat exchanger V. V C 1 Continuous tube reactor (PFR) Residence time distribution with impulse marking A B c A + B > C c0 - High concentrations - Fast reaction - Immediate converstion 1 1st oder reaction (example) CA x = 6 t Reactor arrangement tr = half life Reaction course tr 13 4 2017 PIN NL Spring Session 24
Reaction Concepts Components Examples A B1 B2 B3 B..n. V C Overall Individual Bo = 15... 100 q > 6 (no. of vessel) V 1 Continuous cascade reactor (CCR) Residence time distribution with impulse marking B... n 2 1 c A + B > C c0 Start with A A C - Repeated metering of B into A (+C) - Controlled heat production 1 tm1 1st oder reaction (example) CA Reactor arrangement Reaction course x t tr 13 4 2017 PIN NL Spring Session 25
Reaction Concepts Components Examples Plug Flow Reactor PFR or Continuous Cascade Reactor CCR 13 4 2017 PIN NL Spring Session 26
Reaction Concepts Components Examples Bo = 0 Mixer / heat exchanger V Static mixer 1 Bo = 20... 100 B A. VL. V C 1 2 3 4 t tl Continuous recycle loop reactor (RR) Residence time distribution with impulse marking A B c c0 A + B > C Start with C C (A,B) - cont. metering of A + B - receiver with C - absorbed heat production 1 tm1 0.02 CA Reactor arrangement 1 2 3 4 Reaction course t tl 13 4 2017 PIN NL Spring Session 27
Reaction Concepts Components Examples Loop Model Characteristics Plug flow in all flow regimes and viscosity ranges Inlet streams are immediately mixed with the recycle stream Very short mixing times can be set Only radial mixing in the loop Controlled recycle ratio R, due to compact and precise flow measurement No volume change due to the reaction Volume = 11 ml Studies in a Continuous Laboratory Reactor 13 4 2017 PIN NL Spring Session 28
Reaction Concepts Components Examples Recirculation rate R R > > CSTR behavior Calculate the reactions kinects Reduce the recirculation rate to: Improve selectivity / Residence time distribution Reduce loop volume / System size Limited by the adiabatic temperature rise Mixer / heat exchanger B A. V VL Static mixer. V C Continuous recycle loop reactor (RR) 13 4 2017 PIN NL Spring Session 29
Reaction Concepts Components Examples Mixer-heatexchanger VP R=1 R=2 R=3 VM R=4 T B A. V Q C Continuous loop reactor Continuous loop reactor + residence time VP V. Residence time distribution with impulse marking A B c c0 A + B > C Start with C C (A,B) - cont. metering of A + B - receiver with C - absorbed heat production 1 tm1 0.02 CA Reactor arrangement 1 2 3 4 Reaction course t tl 13 4 2017 PIN NL Spring Session 30
Reaction Concepts Components Examples Plug Flow Recycle Reactor PFRR With additional residence time reactor 13 4 2017 PIN NL Spring Session 31
Reaction Concepts Components Examples Pressure Measurement Temperature Measurement 13 4 2017 PIN NL Spring Session 32
Reaction Concepts Components Examples Sampling Injection Valve 13 4 2017 PIN NL Spring Session 33
Reaction Concepts Components Examples Rupture Discs Proportional Relief Valve 13 4 2017 PIN NL Spring Session 34
Reaction Concepts Components Examples Cooler with Proportional Relief Valve Numerous Accessories 13 4 2017 PIN NL Spring Session 35
Reaction Concepts Components Examples Sight Glass for NIR-,MIR-,RPB- probes 13 4 2017 PIN NL Spring Session 36
Reaction Concepts Components Examples Numerous Standard Dosing Systems 13 4 2017 PIN NL Spring Session 37
Reaction Concepts Components Examples Comprehensive Heating Cooling Equipment 13 4 2017 PIN NL Spring Session 38
Reaction Concepts Components Examples Distillation-, Degassing-, Stripping Devices 13 4 2017 PIN NL Spring Session 39
Reaction Concepts Components Examples Plug Flow Reactor PFR 13 4 2017 PIN NL Spring Session 40
Reaction Concepts Components Examples Residence Time Reactor 13 4 2017 PIN NL Spring Session 41
Reaction Concepts Components Examples Cooler PFR 13 4 2017 PIN NL Spring Session 42
In 3 steps from Batch to Continuous Flow Production Why should you want to change? Continuous Flow versus Batch Possible drivers Less energy consumption Less process steps Less personnel impact / handling Less floor space Smaller reaction volume Higher yield Higher selectivity Higher safety Higher space time yield Better reaction/system control 13 4 2017 PIN NL Spring Session 43
In 3 steps from Batch to Continuous Flow Production Step 1: Fundamental Research Low investment costs Determine reaction kinetics Determine principle reaction characteristics Feasibility and Safety Studies Small Scale (<1kg/hr) Fume Hood size Suitable for various reactions Suitable for liquid liquid / liquid gas reactions Accurate process control Plug Flow Recycle Reactor PFRR 13 4 2017 PIN NL Spring Session 44
In 3 steps from Batch to Continuous Flow Production Step 1: Fundamental Research System Pressure: 100 bar (a) Design Temperature: 20 +250 C Differential pressure: 5 10 bar Recirculation: Max 2,2/sec. Reactor volume: 11 ml Viscosity: <1 2.000 mpas Also available as gas liquid reactor Materials: SS316, Hastelloy C 22/C 276 Plug Flow Recycle Reactor PFRR 13 4 2017 PIN NL Spring Session 45
In 3 steps from Batch to Continuous Flow Production Contiplant Reactor System Step 2: Pilot Plant Medium investment costs Actual process research Process Window Studies Medium Scale (0,5 50kg/hr) 1:1 scalable to production size Dedicated system Accurate process control Including process automation 13 4 2017 PIN NL Spring Session 46
In 3 steps from Batch to Continuous Flow Production Step 2: Pilot Plant Design Pressure: 100 bar (a) Design Temperature: 20 +300 C Materials: SS316, Hastelloy C 22/C 276 Contiplant Reactor System 13 4 2017 PIN NL Spring Session 47
In 3 steps from Batch to Continuous Flow Production Step 3: Production Plant Actual production unit High investment costs Large Scale, upto 10.000 kg/hr Dedicated system Accurate process control Including process automation Production Plant 13 4 2017 PIN NL Spring Session 48
Thank you very much for your attention Questions? 13 4 2017 PIN NL Spring Session 49