Flowid presentation CPhI workshop 2015 Mumbai

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Chemicals Production in the Future: Energy, Raw Materials, Capital & Risk

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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


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0.5 MW

Highly variable resources Biomass, recycle, waste Distributed production Safe, robust, efficient, versatile equipment + processes



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Low CAPEX High ROI Multipurpose, Scalable Robust, Safe Millions vs. Billions


Multiphase Systems: Bottlenecks

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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


Rotor-Stator Spinning Disc Technology

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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



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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)


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

Multiple Spinning Disc Reactor

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Gas-Liquid Mass Transfer

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3 -3 -1L G0.5 m m sL GL

G

k aε

≈


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



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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

Multiple Spinning Disc Slurry Reactor


Spinning Disc Electrolysis

13 I (A) Slides by dr.ir. John van der Schaaf TU/e

Photochemical Reactor


Reactor ExtractorExtractorReactor


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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

Rotor-Rotor Spinning Disc Extractor


Multiple contacting stages


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



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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



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500 1000 1500 2000500

1000

1500

2000


Ωinner rotor

[rpm]

Ωou

ter

roto

r [rpm

]

PSE < 0.850.85 < PSE < 0.99PSE > 0.99


500 1000 1500 2000500

1000

1500

2000


Ωinner rotor

[rpm]

Ωou

ter

roto

r [rpm

]

PSE < 0.850.85 < PSE < 0.99PSE > 0.99


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6 mL/s, 6 mL/s

10 mL/s, 10 mL/s


Extraction efficiency: kLa

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5 mL/s heptane, 5 mL/s water, 0-50 g/L benzoic acid in heptane

500 1000 1500 2000500

1000

1500

2000


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


Extractor


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Reactor


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

Multifunctionality


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Opportunities for Spinning Disc Technology

Small, Safe, VersatileIntensification of all unit operationsLow CAPEX, High ROI Low Risk 2 Marco

Opportunities for Spinning Disc Technology


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

flowid®

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

FlowFlex With SpinPro R300

Control panel

Pumps

Flow controllers

SpinPro Reactor

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FlowFlex With Chemtrix MR260

Control panel

MR260

Pumps

Flow controllers

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SpinPro R300

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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

300 LPH Slurry at 135 degC

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Oil, water, gas phase and quench

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Oil and water phase reaction at 160 degC

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Pharma Pilot Production Plant

Reaction Example: Halogen/Lithium Exchange

Batch


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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


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


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Wouter StamManaging Director

[email protected]+316 2467 9774www.Flowid.nl

mailto:[email protected]?subject=

http://www.Flowid.nl

Flowid presentation CPhI workshop 2015 Mumbai

Engineering