corning ® advanced-flow™ reactors: engineered for...
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Corning ® Advanced-Flow™ Reactors:
engineered for seamless scale-up Alessandra Vizza
Corning Reactor Technologies Corning European Technology Center Avon, France
CPAC/Atochemis Rome Workshop
2013, 25-27 March
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Corning ® Advanced-Flow™ Reactors
A business based on 160 years of worldwide innovation
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Corning Incorporated Founded:
1851
Headquarters:
Corning, New York
Employees:
~ 29,000 worldwide
2011 Sales:
$7.9 Billion
Fortune 500 Rank (2012):
328
• Corning is the world leader in specialty glass
and ceramics.
• We create and make keystone components
that enable high-technology systems for
consumer electronics, mobile emissions
control, telecommunications, and life sciences.
• We succeed through sustained investment
in R&D, 160 years of materials science and
process engineering knowledge, and a
distinctive collaborative culture.
4 Reactor Technologies © Corning Incorporated 2013
Corning’s continuous flow reactors build on the
company’s 160 years of innovation
1947 TV tube
mass production
1879
Glass for
Edison’s
light bulb
1915
Heat-resistant
Pyrex®
glass
1970 Low-loss
optical fiber
1982 LCD glass
1934
Dow
Corning
silicones
1952
Glass ceramics
2010 Thin-film
photovoltaic glass
1972 Substrates for
catalytic converters
Ultra bendable fiber
2007 Thin,
lightweight, cover glass
Pre-1900 1910 1920 1930 1940 1950 1960 1970 1980 1990 2010 2000
2002 Fluidic
module AFR*
160 years of Corning innovation
* Advanced-Flow™ Reactors
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Corning ® Advanced-Flow™ Reactors
Offers broad capability from feasibility to production and enables the transition from batch to continuous processes
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quench
Corning® Advanced-Flow™ Reactors product design
• Engineered fluidic modules:
– glass or ceramic plates with integrated
mass and heat transfer
• Reactor design: a modular assembly
• Reactor:
Reactants End Product
Heat exchange
A
B
D
Corning® Advanced-Flow™ Reactor - Glass Corning® Advanced-Flow™ Reactor - SiC
A+B C C+D E
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Fluidic modules
Increase throughput with similar:
- Pressure drop
- Residence time
LF G1 G2 G3
5-9 ml 0.5 ml 20-25 ml
50-70 ml
- Heat exchange
- Mixing & Mass transfer
2-10 g/min
G4
250 ml
30-150 g/min 150-600 g/min 1000-3000 g/min 1000-4500 g/min D. Lavric and P. Woehl, Advanced-FlowTM glass reactors for seamless scale-up, Chemistry Today 27, 45-48 (2009)
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Large product portfolio enables seamless
scalability from lab to production
Low Flow G1 G2 G3 G4
Single Plate
volume (ml) 0.45 8 – 11 21 – 25 55 – 65 200 – 260
T -60 to 200 °C
P up to 18 bar
High flexibility, metal-free reaction path
From laboratory to production: a seamless scale-up
• Low internal volume
• Use minimal number
of reactants
• Small volume
• Scalability from test
to production
• Process dev. and
optimization tool
• Continuous production of large
amount of chemicals
• Several tons annually
• Large volume
• small footprint
• Processing > 300 kg/hr
• Superior corrosion
resistance of SiC
G4
G3
G2
G1
25 50 75 100 125 150 175 200 225 250 275 300 325 350
Kg / h
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For production: scale-up combined with internal
and external numbering-up
Lab scale
Pilot scale
Production
Source: Chemistry Today, vol. 27 (3), 45-48, 2009
Chemistry Today, 26 (5), 1-4, Sept~Oct (2008)
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Increasing versatility of multi-purpose plants
• Continuous flow reactors
– Displace equipment => CAPEX savings
– Small footprint => debottlenecking
– Improve yield & throughputs => OPEX savings
Batch reactor
• Agitator
• Heat Exchange
• Cooling
Reactor
• Vessel for
end-product
storage
• Cooling
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Corning Advanced-Flow™ Reactors
Benefits sources
Chemistry • New synthesis routes
• Improved yield (conv. & sel.) • Increased product quality • Increased reaction rate
• Simplified downstream process
Safety • Small reaction volume
• Enable “high-energy” chemistry • No unstable intermediate accumulation
Manufacturing • Shorter time to market
• Adjustable & flexible equipment • Lower CAPEX (e.g. foot print)
• Lower OPEX (e.g. solvent, energy) • Reduced investment risk ( at scale-up)
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Corning ® Advanced-Flow™ Reactors
Ensures superior mass & heat transfer, enabling excellent processes intensification
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Glass & ceramic materials
Superior corrosion resistance
Flow reactor
characteristics
Transfer
• Superior mixing & mass-transfer
• Excellent HE with reaction
integration
• Short residence time
• Narrow RTD
Controls
• Reduced process fluid hold-up
• Accurate T,P, & RT control
Production
• Numbering-up to meet capacity
• Flexible to fit chemistry & market
needs
Weight loss
(mg/cm².year)* Glass 316L SS S-SiC
H2SO4-96% good Destroyed good
HNO3-65% good Destroyed good
NaOH-10% low T° good good good
NaOH30% High T° Destroyed good good
HCl-32% good Destroyed good
Glass transparency for photochemistry
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Volumetric mass transfer coefficient:
A seamless scale-up
• Patented heart-shape design: – Superior mixing performance in multiphase systems2
– higher performances in L/L mass transfer coefficient (kla)1
• Up to 103 compared to packed column
• 2x-4x better than other “micro-channel” devices
2María Jose Nieves-Remacha, Amol A.
Kulkarni, and Klavs F. Jensen: Ind, & Eng.
Chem. Res. (2012) vol. 51 ( 50 ) pp. 16251 -
16262)
1Saien, J. et al., Investigation of a two impinging-jets contacting device for liquid–liquid extraction processes, Chem. Eng. Sci. 2006, 61, 3942-3950
Similar mixing performances from lab to
production
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• Seamless scale-up: similar heat transfer coefficient from G1 to G4
Heat transfer coefficient
~100x-1000x higher than batch
Method
Volumetric heat
transfer coefficient
(MW/m3K)
Ceramic SiC fluidic modules 1.5
*Corning glass fluidic modules
(water/water, ~ 0.7 m/s) 1.7
*Plate (metallic, 4 mm spaced;
water/water, 1 m/s) 1.25
*Shell and tubes (metallic; water/water;
1 m/s) 0.2
*Batch with external heat exchanger 10-2
*Jacketed batch 10-3
*D. Lavric, Thermal performance of Corning glass microstructures, Proceedings of the Heat Transfer and Fluid Flow in Microscale III Conference, Hilton Whistler, BC, Canada, ECI international, 2008
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Corning ® Advanced-Flow™ Reactors
Minimizes scale-up failures and drastically reduces the time from laboratory to production
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Case Study: customer experienced seamless
scale-up from G1 to G4
Lab G1
3,7 t/y Production, G4
110 t/y
Multiphase application: L/L/G
G1 G4
Yie
ld
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Courtesy of DSM
EXPERIMENTAL RESULT
0,5
0,6
0,7
0,8
0,9
1
1,1
1,2
1,3
1,4
1,5
0 1 2 3 4 5 6 7 8
REACTOR
un
co
nvere
td p
rod
uct
(rati
o t
o t
he
avera
ge)
0,5
0,6
0,7
0,8
0,9
1
1,1
1,2
1,3
1,4
1,5
Flo
w v
ari
ati
on
unconverted product (ratio to the average)
total flow(ratio to the average)
AFR Nitration Goes to Production Feasibility->pilot->successful production (c-GMP)
P. Poechlauer; S. Brune (DSM), 2nd symposium on Continuous Flow Reactor Technology for Industrial Applications, Oct 4, 2010,Paris
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Corning® Advanced-Flow™ Reactors
Development time reduced by ~50% vs. batch
• Faster knowledge generation => kilo-lab tests phase shortened
• Seamless scale-up => process development phase avoided
Minimum
Maximum
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Corning ® Advanced-Flow™ Reactors
Case studies have demonstrated the benefits of using AFR in pharma and fine chemical applications for safer, greener, cheaper and effectively more sustainable processes.
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What we can do better comparing to batch
• Reactions with non-stable products
– (peracid, azide, chloramines, boran,…)
• Rapid and exothermal reactions
– (oxidation, nitration, acid-base,…)
• Reactions with toxic products
– (cyanides, phosgene,…)
• Reactions with runaway hazards
– (cycloaddition, transposition, …)
• More generally, reactions impossible to be batch-operated, or difficult in batch-operation due to…
– (pressure, temperature, concentration, catalysts, partial conversion, …)
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Examples of AFR Reaction Applications (1)
• Chloroformate Chemistry
– Better yield easily followed by on-line Raman PAT
• Diasteroselective Ritter Reaction
– Increased productivity with safe & controllable operation
• Nitration Reactions in AFR
– Reduced solvent usage, higher yield of safer operation
• AFR Nitration Goes to Production
– Feasibility->Pilot->Successful Production (c-GMP)
• More Nitration Reactions in AFR
– Mixing quality vs. conversion, and selectivity
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Examples of AFR Reaction Applications (2)
• Selective Hydrogenation with Slurry Catalyst
98%+ conversion & selectivity (impurity profiles within spec)
• Low Temperature Applications
– Energy Saving and/or Better Yield (DCM-B-Pin)
• Green Process: Glycerol to Fuel Additives
– Significantly Reduce Usage of Organics
• Sulphonation Reaction Application
– Full conversion achieved with high purity
• Beckmann Rearrangement Application
– Stable and better results meeting performance targets
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Examples of AFR Reaction Applications (3)
• Photochemical Reaction Application
– High efficiency with easy controls
• Accelerating Reactions in AFR
– An alternative to microwave reactors
• Schotten-Baumann Amidation
– Improved yield via superior mixing
• Dipeptides Synthesis Application
No precipitates in biphasic solvent for amine bonding
• Grignard Reagent (RMgX) Preparation
– Precise controls lead to better purity of final products
• Continuous production of Alkyl nitrite
– For 10 T/y production capacity
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Corning ® Advanced-Flow™ Reactors
Now it is easy to FLOW with Corning ® Advanced-Flow™ Reactors
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Thank you!
Questions ?
www.corning.com/reactors