ContinuousFlow Reactions From idea to production size ... · 13‐4‐2017 PIN‐NL Spring Session 29 Continuous loop reactor Mixer / heat exchanger Static mixer C. V A B. V L V Continuous

Continuous Flow Reactions‐

From idea to production size scale up in 3 steps

PIN‐NL Spring Session13‐04‐2017

13‐4‐2017 PIN‐NL Spring Session 1

• Introduction Flowlink• Continuous Flow Reactions

What is required?

• Fluitec Contiplant Modular Reaction SystemProcess Concepts and Examples

• In 3 steps from Batch to Continuous Flow Production

Topics


Introduction Flowlink



Engineered Micro Gear Pumps



Engineered Gear Pumps:



Mixers / Heat Exchangers &Systems



Engineering & Systems


What is required for continuous flow reactions?

Continuous Flow Reactions



What is required for continuous flow reactions?

Continuous addition of feed stock -> DosingInteracting molecules - > Mixing

Heating and/or Cooling-> Heat TransferSelectivity / 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

PIN‐NL Spring Session Page 10

Accurate Dosing

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Mixing

Turbulent flow

Laminar flow

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13‐4‐2017



13‐4‐2017


Plug Flow


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Page 15PIN‐NL Spring Session


Scale-upis carried out by

increasing the number of tubes

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Page 16PIN‐NL Spring Session


13‐4‐2017





Scale up of a Plug Flow Recycle Reactor PFRR with Residence Time Reactor

Fluitec Contiplant Modular Reaction System

Reaction ConceptsAvailable Components

Examples



Fluitec Moduclar Reaction System


Reaction Concepts – Components – Examples


• Modular reactor system• 6 points per reactor for connecting

accessories• Diameters vary form ø4,7 – 36 mm


Redundant System CSTR + PFR



High Viscous Loop Reactor with Distillation



Residence time distribution with impulse marking

A B

- High concentrations- Fast reaction- Immediate converstion

Mixer / heat exchangerA

B CV

.V

Reactor arrangement

cc0

ttR

CA

1st oder reaction (example)

Reaction course

x = 6

A + B > C

1

tR = half life

Continuous tube reactor (PFR)

1

Bo > 65



1

Bo = 15 ... 100

q > 6 (no. of vessel)

Individual

Overall

1st oder reaction (example)

x

A + B > C

tM1

cc0

ttR

1

CA

Reactor arrangement

Continuous cascade reactor (CCR)

A CStart with A

B

- Repeated metering of B into A (+C) - Controlled heat production

12... n

A

B1

C

.V

B2 B ..nB3

V


Reaction course



Plug Flow Reactor PFR orContinuous Cascade Reactor CCR



A + B > C

tM1

0.02CA

cc0

ttL

1

1 2 3 4

- cont. metering of A + B - receiver with C - absorbed heat production

C (A,B)

BA

Start with C

Reactor arrangement

Continuous loop reactor

Mixer / heat exchangerStatic mixer

C

.VA

B .VL

V

Continuous recycle reactor (RR) Residence time distribution with impulse marking

Reaction course

1

Bo = 0

Bo = 20 .... 100

1 2 3 4 ttL



Volume = 11 ml

Studies in a Continuous Laboratory Reactor


Loop Model Characteristics

• Plug flow in all flow regimes and viscosity ranges

• Inlet streams are immediatelymixed with the recycle stream

• Very short mixing times can beset

• Only radial mixing in the loop• Controlled recycle ratio R, due to

compact and precise flow measurement

• No volume change due to the reaction



Continuous loop reactor

Mixer / heat exchangerStatic mixer

C

.VA

B .VL

V

Continuous recycle reactor (RR)

Recirculation rate RR ‐> ∞ ‐> CSTR behaviorCalculate the reactions kinects

Reduce the recirculation rate to:• Improve selectivity / Residence

time distribution• Reduce loop volume / System size• Limited by the adiabatic

temperature rise



A + B > C

tM1

0.02CA

cc0

ttL

1

1 2 3 4

- cont. metering of A + B - receiver with C - absorbed heat production

C (A,B)

BA

Start with C

Reaction course


Reactor arrangement

Continuous loop reactorContinuous loop reactor + residence time

Mixer-heatexchanger

C

.V

AB

VM

VP

T

Q VP

V.

R=1

R=2

R=3

R=4



Plug Flow Recycle Reactor PFRRWith additional residence time reactor


Pressure Measurement Temperature Measurement



Sampling Injection Valve



Proportional Relief ValveRupture Discs



Cooler with Proportional Relief Valve Numerous Accessories



Sight Glass for NIR-,MIR-,RPB- probes



Numerous Standard Dosing Systems



Comprehensive Heating Cooling Equipment



Distillation-, Degassing-, Stripping Devices



Plug Flow Reactor PFR



Residence Time Reactor



PFR



Cooler

Continuous Flow versus BatchPossible drivers

Why should you want to change?

• 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


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



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



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

Contiplant Reactor System



Step 2: Pilot Plant

Contiplant Reactor System


• Design Pressure: 100 bar (a)• Design Temperature: ‐20 ‐ +300°C• Materials: SS316, Hastelloy C‐22/C‐276


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



Thank you very much for yourattention

Questions?


Documents

ContinuousFlow Reactions From idea to production size ... · 13‐4‐2017 PIN‐NL Spring Session 29 Continuous loop reactor Mixer / heat exchanger Static mixer C. V A B. V L V Continuous