Flowid presentation CPhI workshop 2015 Mumbai
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Chemicals Production in the Future: Energy, Raw Materials, Capital & Risk
2
Highly variable supply Distributed production Storage/transport inefficient Use for chemicals production Highly variable production rate
Wind Turbines
50 TW
5 TW
Slides by dr.ir. John van der Schaaf TU/e
Chemicals Production in the Future: Energy, Raw Materials, Capital & Risk
3
0.5 MW
Highly variable resources Biomass, recycle, waste Distributed production Safe, robust, efficient, versatile equipment + processes
Slides by dr.ir. John van der Schaaf TU/e
Chemicals Production in the Future: Energy, Raw Materials, Capital & Risk
4
Low CAPEX High ROI Multipurpose, Scalable Robust, Safe Millions vs. Billions
Slides by dr.ir. John van der Schaaf TU/e
Multiphase Systems: Bottlenecks
5
Gas Liquid Solid
agl asCg CL
Gas Liquid Solid
11A
g g gl l gl s s r t s
r H H HC k a k a k a k L aη δ
−$ %−
= + + +& '& '( )
Catalyst concentration/activity
Rea
ctio
n ra
te
mass transfer limited
kinetically limited
δ
Slides by dr.ir. John van der Schaaf TU/e
Rotor-Stator Spinning Disc Technology
6
Rotor-Stator Spinning Disc Technology
Answers demands PI of multiphase systems: • High mass transfer (GL ~10 1/s, LL ~300 1/s, LS ~ 1 1/s)
• High heat transfer (U.A ~ 40 MW/m3/K)
• Short micromixing times (tm ~ 0.1 ms)
• Countercurrent Flow (100-1000 kg/hr)
• Plug Flow (~4 tonnes/hr)
• Low volume ( VR ~ 1 L)
Applications: • Extreme fast and exothermic reactions (nitrification) • Multiphase reactions (sulfonation, halogenation) • Extraction (LL, LS) • Distillation (RPB), Absorption • Crystallization • Electrochemistry, Photochemistry
Slides by dr.ir. John van der Schaaf TU/e
Rotor-Stator Spinning Disc Technology
7
Rotor-Stator Spinning Disc Technology
Special Features: • Alternative construction materials • Specialty coatings, surface treatment • High corrosion resistivity • Membranes, Catalytically active discs • Phase separation (GL, LS) • High pressure, high temperature • High viscosity (Glycerol, 98% H2SO4)
Slides by dr.ir. John van der Schaaf TU/e
ReactorReactor
Chemical Production Process
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Extractor
Evaporation Crystallizer
A(S) + B(g) ----> C(S)
C(S) + B(g) ----> D(S)
A(S)
B(g)
A(S), C(S), D(S)
D(E)
C(E), D(E)
E
C(s)
E
Crystallizer
D(s)
C(E), D(E)
cat
catSlides by dr.ir. John van der Schaaf TU/e
Gas-Liquid Mass Transfer
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3 -3 -1L G0.5 m m sL GL
G
k aε
≈
Gas-Liquid Mass Transfer
Meeuwse et al., Gas–liquid mass transfer in a rotor–stator spinning disc reactor, CES 65 466-471(2010)
Gas flow: 400 mL/min Liquid flow: 400 mL/min
Slides by dr.ir. John van der Schaaf TU/e
Gas-Liquid Mass Transfer
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Gas-Liquid Mass Transfer
Van Eeten et al., A theoretical study on gas-liquid mass transfer in the rotor stator spinning disc reactor, CES 129 2015 Slides by dr.ir. John van der Schaaf TU/e
Reactor ExtractorExtractorReactor
Chemical Production Process
15
Evaporation Crystallizer
A(S)
B(g)
A(S), C(S), D(S)
D(E)
C(E), D(E)
E
C(s)
E
Crystallizer
D(s)
C(E), D(E)
A(S) + B(g) ----> C(S)
C(S) + B(g) ----> D(S)Slides by dr.ir. John van der Schaaf TU/e
Cocurrent Liquid-Liquid Flow Rotor-Stator
16Visscher, Ind. & Eng. Chem. Res. 2012; Visscher, Chem. Eng. J. 2012 Slides by dr.ir. John van der Schaaf TU/e
Cocurrent Liquid-Liquid Flow Rotor-Stator
17Visscher, Ind. & Eng. Chem. Res. 2012; Visscher, Chem. Eng. J. 2012 Slides by dr.ir. John van der Schaaf TU/e
Physical separation efficiency
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500 1000 1500 2000500
1000
1500
2000 Light outlet: Purity (%)
Ωinner rotor [rpm]
Ωou
ter r
otor
[rpm
]
500 1000 1500 2000500
1000
1500
2000 Heavy outlet: Purity (%)
Ωinner rotor [rpm]
Ωou
ter r
otor
[rpm
]
80
82
84
86
88
90
92
94
96
98
100
80
82
84
86
88
90
92
94
96
98
100
5 mL/s heptane, 5 mL/s water
Slides by dr.ir. John van der Schaaf TU/e
Physical separation efficiency
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5 mL/s heptane, 5 mL/s water
500 1000 1500 2000500
1000
1500
2000
PSE = Purityheavy*Puritylight (-) (Fheavy=5 ml/s and Flight=5 ml/s)
Ωinner rotor
[rpm]
Ωou
ter
roto
r [rpm
]
PSE < 0.850.85 < PSE < 0.99PSE > 0.99
Slides by dr.ir. John van der Schaaf TU/e
Physical separation efficiency
22
5 mL/s heptane, 5 mL/s water
500 1000 1500 2000500
1000
1500
2000
PSE = Purityheavy*Puritylight (-) (Fheavy=5 ml/s and Flight=5 ml/s)
Ωinner rotor
[rpm]
Ωou
ter
roto
r [rpm
]
PSE < 0.850.85 < PSE < 0.99PSE > 0.99
Slides by dr.ir. John van der Schaaf TU/e
500 1000 1500 2000500
1000
1500
2000
PSE = Purityheavy*Puritylight (-) (Fheavy=5 ml/s and Flight=5 ml/s)
Ωinner rotor
[rpm]
Ωou
ter
roto
r [rpm
]
PSE < 0.850.85 < PSE < 0.99PSE > 0.99
Physical separation efficiency
23
5 mL/s heptane, 5 mL/s water
6 mL/s, 6 mL/s
10 mL/s, 10 mL/s
Slides by dr.ir. John van der Schaaf TU/e
Extraction efficiency: kLa
24
5 mL/s heptane, 5 mL/s water, 0-50 g/L benzoic acid in heptane
500 1000 1500 2000500
1000
1500
2000
PSE = Purityheavy*Puritylight (-) (Fheavy=5 ml/s and Flight=5 ml/s)
Ωinner rotor
[rpm]
Ωou
ter
roto
r [rpm
]
PSE < 0.850.85 < PSE < 0.99PSE > 0.99
0.05 1/s
0.35 1/s 0.7 1/s
0.1 1/s
0.13 1/s
Slides by dr.ir. John van der Schaaf TU/e
Extractor
Chemical Production Process
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Reactor
Evaporation Crystallizer
A(S)
B(g)
A(S), C(S), D(S)
D(E)
C(E), D(E)
E
C(s)
E
Crystallizer
D(s)
C(E), D(E)
A(S) + B(g) ----> C(S)
C(S) + B(g) ----> D(S)Slides by dr.ir. John van der Schaaf TU/e
27
Opportunities for Spinning Disc Technology
Small, Safe, VersatileIntensification of all unit operationsLow CAPEX, High ROI Low Risk 2 Marco
Opportunities for Spinning Disc Technology
Slides by dr.ir. John van der Schaaf TU/e
Flowid Products & Services
FlowFlex
Automated modular platform SpinPro Reactor
Continuous Reactor based on patented Spinning Disc Technology
SpinPro ExtractorCounter current Extractor based on patented Spinning Disc Technology
Process Development & TestingFully to customers specs, testing in house possible on lab and pilot scale
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Spinning Disk ReactorCon2nuous Reactors
Metric tons/DayFast chemistry
Extremely inert material
High heat transferMulti-stage reactions
Metric tons/DayFast ChemistryExtreme mixing efficiencyHandles gas/liquid/solids
Multi-stage reactions
“Lab to Manufacture” Platforms
Production ScaleSpinning Disk ReactorCon2nuous Reactors
fast and predictable scale up to the most suitable platform
•Multiple modules on one platform•One user interface•Data logging•Available as a service or purchase
SpinPro R300
34
Number of stages: 3
Temperature: -20 - 160 °C
Pressure: 10 bar (g)
Flowrate: 0,1 - 600 l/hr
Reactor volume: 135/230 ml
Body material: SS316 / Hastelloy C
Seal material: PTFE
O-ring material: FFKM
Rotation: 3000 rpm
Heat transfer: up to 1 kW/stage (ΔT=40 °C)
Measurement: thermocouple at each stage
SpinPro R700
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Number of stages: 7
Temperature: -20-160 °C
Pressure: 10 bar (g) (100bar autoclave)
Flowrate: up to 3600 L/hr
Reactor volume: 430 ml
Body material: Hastelloy-C
Seal material: Teflon (PTFE)
O-ring material: Kalrez (FFKM)
Rotation: 4500 rpm
Heat transfer: tbd (ΔT=70 °C)
Measurement: thermocouple at each stage
SpinPro Reactor
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Easy to cleanEasy to assemble and inspectEasy to re-machine the surfacesEasy to scale to R700
Reaction Example: Halogen/Lithium Exchange
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Batch Continuous lab97% Yield 97% Yield
-78 C required, slow addition
Scalable, room temp 2.7 Kg/hr @ Feedrates 200+ mL/min
Feed reagent concentrations of 2.0M, lithium products were quenched with TMSCl and analyzed by GC. Tet. Lett., 2010, 51, p. 4793.
Cl
SiMe3
Cl
Br
Li
2.0M
+
Cl
Li
Flow Process:◆ 97,5% Conversion, ◆ Overall combined flow rate = 400 mL/min
Reaction Example: Halogen/Lithium Exchange
Li+
Br
LiS3T1@RT
S3T1@RT
DMF (in THF)O
Cl
Cl
Cl
Set-up production scale Component BBuLi
Quench
Reaction and quench in one system
V = 135 ml. 45 ml per disc
Flow at 100 LPH
Lab to Manufacture Scalability
Tet. Lett., 2010, 51, p. 4793.
15 mL experiments
97.5% 1.1 eq BuLi200 uM gap and 5500 rpm on a 2.5"disk
100 kg finished API/day 97% 1.1 eq BuLi1mm gap and 2500 rpm on a 6" disk
Batch reactor
The SpinPro allows for safe operation at high temperaturesArrhenius law: higher temperature equals a higher production rate
SpinPro reactor
Reaction Example: Halogen/Lithium Exchange
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Wouter StamManaging Director
wouter.stam@Flowid.nl+316 2467 9774www.Flowid.nl
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