Continuous Flow Reactions. From idea to production size scale up in 3 steps
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1 Continuous Flow Reactions From idea to production size scale up in 3 steps PIN NL Spring Session PIN NL Spring Session 1
2 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 PIN NL Spring Session 2
3 Introduction Flowlink PIN NL Spring Session 3
4 Introduction Flowlink Engineered Micro Gear Pumps PIN NL Spring Session 4
5 Introduction Flowlink : Engineered Gear Pumps PIN NL Spring Session 5
6 Introduction Flowlink Mixers / Heat Exchangers & Systems PIN NL Spring Session 6
7 Introduction Flowlink Engineering & Systems PIN NL Spring Session 7
8 Continuous Flow Reactions What is required for continuous flow reactions? PIN NL Spring Session 8
9 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 PIN-NL Spring Session 9
10 Dosing Mixing Heat Transfer Plug Flow Scale-up Accurate Dosing PIN NL Spring Session Page 10
11 Dosing Mixing Heat Transfer Plug Flow Scale-up Mixing Turbulent flow Laminar flow PIN NL Spring Session Page 11
12 Dosing Mixing Heat Transfer Plug Flow Scale-up PIN NL Spring Session Page 12
13 Dosing Mixing Heat Transfer Plug Flow Scale-up PIN NL Spring Session Page 13
14 Dosing Mixing Heat Transfer Plug Flow Scale-up Plug Flow PIN NL Spring Session Page 14
15 Dosing Mixing Heat Transfer Plug Flow Scale-up Scale-up is carried out by increasing the number of tubes PIN NL Spring Session Page 15
16 Dosing Mixing Heat Transfer Plug Flow Scale-up PIN NL Spring Session Page 16
17 Dosing Mixing Heat Transfer Plug Flow Scale-up PIN NL Spring Session 17
18 Dosing Mixing Heat Transfer Plug Flow Scale-up Scale up of a Plug Flow Recycle Reactor PFRR with Residence Time Reactor PIN NL Spring Session 18
19 Continuous Flow Reactions Fluitec Contiplant Modular Reaction System Reaction Concepts Available Components Examples PIN NL Spring Session 19
20 Reaction Concepts Components Examples Fluitec Moduclar Reaction System PIN NL Spring Session 20
21 Reaction Concepts Components Examples Modular reactor system 6 points per reactor for connecting accessories Diameters vary form ø4,7 36 mm PIN NL Spring Session 21
22 Reaction Concepts Components Examples Redundant System CSTR + PFR PIN NL Spring Session 22
23 Reaction Concepts Components Examples High Viscous Loop Reactor with Distillation PIN NL Spring Session 23
24 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 PIN NL Spring Session 24
25 Reaction Concepts Components Examples A B1 B2 B3 B..n. V C Overall Individual Bo = 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 PIN NL Spring Session 25
26 Reaction Concepts Components Examples Plug Flow Reactor PFR or Continuous Cascade Reactor CCR PIN NL Spring Session 26
27 Reaction Concepts Components Examples Bo = 0 Mixer / heat exchanger V Static mixer 1 Bo = B A. VL. V C 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 tm CA Reactor arrangement Reaction course t tl PIN NL Spring Session 27
28 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 PIN NL Spring Session 28
29 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) PIN NL Spring Session 29
30 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 tm CA Reactor arrangement Reaction course t tl PIN NL Spring Session 30
31 Reaction Concepts Components Examples Plug Flow Recycle Reactor PFRR With additional residence time reactor PIN NL Spring Session 31
32 Reaction Concepts Components Examples Pressure Measurement Temperature Measurement PIN NL Spring Session 32
33 Reaction Concepts Components Examples Sampling Injection Valve PIN NL Spring Session 33
34 Reaction Concepts Components Examples Rupture Discs Proportional Relief Valve PIN NL Spring Session 34
35 Reaction Concepts Components Examples Cooler with Proportional Relief Valve Numerous Accessories PIN NL Spring Session 35
36 Reaction Concepts Components Examples Sight Glass for NIR-,MIR-,RPB- probes PIN NL Spring Session 36
37 Reaction Concepts Components Examples Numerous Standard Dosing Systems PIN NL Spring Session 37
38 Reaction Concepts Components Examples Comprehensive Heating Cooling Equipment PIN NL Spring Session 38
39 Reaction Concepts Components Examples Distillation-, Degassing-, Stripping Devices PIN NL Spring Session 39
40 Reaction Concepts Components Examples Plug Flow Reactor PFR PIN NL Spring Session 40
41 Reaction Concepts Components Examples Residence Time Reactor PIN NL Spring Session 41
42 Reaction Concepts Components Examples Cooler PFR PIN NL Spring Session 42
43 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 PIN NL Spring Session 43
44 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 PIN NL Spring Session 44
45 In 3 steps from Batch to Continuous Flow Production Step 1: Fundamental Research System Pressure: 100 bar (a) Design Temperature: C Differential pressure: 5 10 bar Recirculation: Max 2,2/sec. Reactor volume: 11 ml Viscosity: < mpas Also available as gas liquid reactor Materials: SS316, Hastelloy C 22/C 276 Plug Flow Recycle Reactor PFRR PIN NL Spring Session 45
46 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 PIN NL Spring Session 46
47 In 3 steps from Batch to Continuous Flow Production Step 2: Pilot Plant Design Pressure: 100 bar (a) Design Temperature: C Materials: SS316, Hastelloy C 22/C 276 Contiplant Reactor System PIN NL Spring Session 47
48 In 3 steps from Batch to Continuous Flow Production Step 3: Production Plant Actual production unit High investment costs Large Scale, upto kg/hr Dedicated system Accurate process control Including process automation Production Plant PIN NL Spring Session 48
49 Thank you very much for your attention Questions? PIN NL Spring Session 49
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