efficient processing with corning® advanced-flow...
TRANSCRIPT
Efficient Processing with Corning® Advanced-FlowTM Glass Technology
Jay SutherlandJune 24, 2009
2Advanced-Flow Reactor Technology
Corning Incorporated
Founded:1851
Headquarters:Corning, New York
Employees:Approximately 25,000 worldwide
2008 Sales:$5.9 Billion
Fortune 500 Rank (2008): 417
• 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, more than 150 years of materials science and process engineering knowledge, and a distinctive collaborative culture.
3Advanced-Flow Reactor Technology
A Culture of Innovation
Processes for mass producing the television bulb
19471879
Glass envelope for Thomas Edison’s light bulb
1915
Heat-resistant Pyrex® glass
First low-loss optical fiber
1970 1984
AMLCD glass for TVs, notebook computers & monitors
1972
Ceramic substrates for automotive catalytic converters
Dow Corning silicones
1934
Glass ceramics
1952 2006
High-throughput label-free screening platform for drug discovery
Fusion drawprocess
1960
4Advanced-Flow Reactor Technology
Doing chemical reactions in big tanks is like trying to bake big cakes…hard
-Ovens work well for these-Better heat transfer means perfectly baked cake-Predictable scale-up by simply adding more pans-Easy to make ovens and pans for any kind of cupcake!
-Oven hard to build an oven for this!-Heat transfer poor…cake will burnon outside and be raw inside-Must fit cake recipe to equipment(in fact, they had to make an ice cream cake!)
5Advanced-Flow Reactor Technology
Conventional batch chemical reactors
-Mixing is poor-Hard to get heat in and out-Scale-up is hard-Must fit chemistry to equipment
-Easier and safer to operate-Better heat & mixing control-Predictable scale-up by adding modules-Equipment adapts to chemistry
continuous reactors
Solution: Don’t do batch reactions!
6Advanced-FlowReactor Technology
Edge Brownie PanA baker’s dream: deliciously chewy edges for every piece!
If you love the crunchy, caramelized, toasty edges of a brownie, this pan is for you. No more gooey centers—every serving has two edges, thanks to the patented interior sidewalls on this pan.
This is an even better analogy!
7Advanced-FlowReactor Technology
Today’s IndustrialManufacturing
Glass FluidicModules
Evolution in processingRevolution
Corning® Advanced-FlowTM
Glass Reactor
Alchemy
8Advanced-Flow Reactor Technology
Fluidic ModulesAdd-on (insulation…)Labelling
Sensing
Instrumentation (Pressure relief valve…)
Connectors
Interfaces
Tubing
Standard Fittings
Frames
O-ring seals
Reactor components
9Advanced-Flow Reactor Technology
Assembly of fluidic modules for production
FLUIDIC MODULES
REACTORS
PRODUCTION BANKS(Reactors in Parallel)
10Advanced-Flow Reactor Technology
Fluidic modules for many applications
Organicphase
Gas phase
Aqueousphase
Solid phasesuspensions
11Advanced-Flow Reactor Technology
Multiple ports add even more flexibility
12Advanced-Flow Reactor Technology
Heat exchange & mixing are integrated in the fluidic module
Reaction layerHeat exchange layer
Heat exchange layer
Reactants Product
13Advanced-Flow Reactor Technology
Designs optimize heat and mass transfer
Mixing 300 microns
Pressure drop1 millimeter
Reactants
700 microns
4 mm
Heat transfer
Reactants
Heat exchange fluid
700 microns
14Advanced-Flow Reactor Technology
Benefits of process intensificationReactor Characteristics-Continuous processing-Reduced process hold up-Residence time control-Efficient mixing-High surface-to-volume ratio-Improved process control-Worry-free scale-up by “numbering-up”-Work above solvent boiling point-Easy to clean-Equipment fits the chemistry
Economic-Less capital risk-Lower manufacturing and operating cost-Less raw material, solvent, waste, energy-Less work-up-Constant quality-Shorter time to market-Improved production management (on demand)
Safety-Enhanced safety; new reactions possible-No scale-up issues-No unstable intermediate accumulation-Elimination of batch critical operations
Chemistry Benefits-Improved yield, selectivity& product purity-Increased reaction rates-Expanded temperature range-New process windows
15Advanced-FlowReactor Technology
Multi-phase chemistry: Liquid/LiquidMiscible liquids
Non-miscible liquids
Biphasic bubble system
Biphasic bubble system
Biphasic bubble system
Corning (NIM)One phase system
Source of the data PhD from F. SarrazinMicroréacteurs diphasiques pour le
développement rapide des procédés, INPG(2), 2006
Measurement at LGC(1)
(mixing time)Modelling (shear rates)
Critical size (µm) 50 500 1000 700-4000
Flow rates mL/h 0.1 2 6 4000-8000
Mixing time (ms) 10 - 60 400-1500 3000-10000 10 - 20
Shear rate (s-1) 4000 80 15 30000-65000
(1)Laboratoire de Génie Chimique – Toulouse – France(2)Institut National Polytechnique de Toulouse – France
16Advanced-FlowReactor Technology
Multi-phase: Gas/Liquid
Gas / liquid
17Advanced-FlowReactor Technology
Multi-Phase: Liquid/Solid
Many solid types are compatible with our reactors:
• Slurries• Particles in feed• Fine precipitates
SiC nominal size (µm)
Concentration (g/L)
13 >30037 >300
105 >25 g/LHigh mixing capabilityfluidic module
18Advanced-FlowReactor Technology
Processing of high viscosity fluids
1
10
100
1000
0 50 100 150 200
TEMPERATURE (°C)
VISC
OSI
TY (c
P) Pressure drop <10 bars (6 kg/h)
0
50
100
150
200
Tem
pera
ture
(°C
)
•Fluid with viscosities up to ~500 cP• Viscosities at operating temperature up to ~100 cP
19Advanced-FlowReactor Technology
( ) ( )cp TTVSUHkA
ddTC −⋅⋅−∆−= )(τ
ρ
Multi-port injection: Provides better temperature management along the flow path
Heat generation
Heat removal
0
0,2
0,4
0,6
0,8
1
0 2 4 6 8 10 12 14 16 18
NUMBER OF INJECTION POINTS
RED
UC
TIO
N O
F TE
MP
ERA
TUR
E
Single -injection
Multi -injection
20Advanced-Flow Reactor Technology
Specific examples• Increase product quality
– Esterification from RCOCl– Nitration (HNO3 / H2SO4)– Hydrosilation
• Increase yield and/or consume less solvent, energy etc.– Nitration (HNO3)– Condensation– Metalorganic reactions
• Remove or reduce time consumingoperations
– Oxidation (NaClO)– Condensation– Metalorganic reactions
• Improve safety– Oxidation (NaClO)– Coupling (H2SO4)– Nitration (HNO3)
Outputs : Process Results Yield Selectivity Cost Safety…
Inpu
ts :
Pro
cess
Par
amet
ers
Pre
ssur
e Te
mpe
ratu
re C
once
ntra
tion
Process optimization depends on the
output target
X
X
X
XX
21Advanced-Flow Reactor Technology
Broad range of applications• Reactions which have already benefited from Corning reactors
– Nitration– Metal Organic – Oxidation – Reduction– Coupling, substitutions– Rearrangements – Amidation– Bromination– Alkylation– Hydrogenation etc.
• Mono- or multi-step processes including pre-mixing, quenching etc.
• In mono- or multi-phase reactions– Miscible liquid feeds– Non miscible feeds – emulsions– Liquid and gas feeds– Precipitation of sub-product or products
Under Development– Fluoride-containing systems– Hot alkaline conditions– Solid starting materials– Immobilized heterogeneous catalysts– Microwaves, Ultrasound, UV light
22Advanced-Flow Reactor Technology
1 10 100 1000 10000
Nitration (sulfonitric)Oxidation (bleach)HydrosilationMetal Organic
Batch vs. Corning Reactors (CR) – Reaction time
Batch
CR
Reaction time (s)
1 10 100 1000
Batch
CR
2,5min 14h
Reaction time (min)
Application 1First trials
23Advanced-Flow Reactor Technology
Batch vs. Corning Reactors – Yield and Purity
50 60 70 80 90 100
Nitration (nitric)
Metal OrganicBatch
CR
Yield (%)
50 60 70 80 90 100
Nitration (nitric)
Nitration (sulfonitric)Hydrosilation
Batch
CR
Purity (%)
24Advanced-Flow Reactor Technology
Batch vs. Corning Reactors – Temperature and Solvent
-100 -50 0 50 100
Metal Organic 1
Metal Organic 2
Coupling
Rearrangement 1Rearrangement 2Batch
CR
Temperature (°C)
0 20 40 60 80 100
Nitration (nitric)
Solvent ratio (wt %)
Batch
CR
25Advanced-Flow Reactor Technology
Batch vs. Corning Reactors – SafetyEND-USER CASE CONVENTIONAL
TECHNOLOGIESCorning Reactors
Oxidation with bleach Scale-up issuesHazardous reaction
Safe operation
Coupling in presence of sulfuric acid
First production batch at 60°C damped into a quench solution
Operation under full control at 90°C
Autocatalytic nitration Accumulation risksNo scale-up possible
Safe operation
Nitration reaction Dedicated equipment Safe operation
0,1 1 10 100 1000
Reactor Volume (L)
Batch
CR
0,1 1 10 100 1000 10000
JacketedBatch
CR
GlobalHeat TransferCoefficientkW/(m3.K)
BatchExternal
HE
26Advanced-Flow Reactor Technology
Total flow rate min-max
20 – 300 mL/min 3 – 7 L/min
Working temperature -60°C up to 230°C -60°C up to 230°C
Working pressure up to 18 bar up to 6 bar
Internal volume 20 – 50 mL 40 – 100 mL
Residence time 10 – 60 s @ 30 mL/min N/A
Mixing (Villermaux) 90% @ 30 mL/min N/A
Pressure drop (calculated)
0.4 – 3.0 bar @ 100mL/min 1 cPo
1.4 bar @ 3L/min 7cPo
Typical values for Generation 1 Fluidic Modules
Reaction channelHeat exchange
channels
27Advanced-Flow Reactor Technology
Evaluation kit
A1
A2
A3
A’2 A’3 A’4
A4
28Advanced-Flow Reactor Technology
Full Product Synthesis Unit - eg. 3-step Nitration process
1.Sulfonitric mixture production
1
2.Nitration
2
3.Quench
3Feed 1
Feed 2
DT
DT MJ
MF
DT
DT MJ
MF
Feed 3
DT SJFeed 4
DT
PRODUCT OUTPUT
29Advanced-Flow Reactor Technology
Designs for high throughput• Need for higher throughput reactors :
– Increase productivity (tons/year) for a given number of reactors
– Reduce number of reactors needed to fit production requirements
• Main challenges to higher throughput:• Residence time • Pressure drop • Heat Transfer
• Solution: larger glass fluidic modules with comparable residence time, pressure drop and heat exchange performance
1st Generation 2nd Generation
30Advanced-Flow Reactor Technology
How the technology scales for production
Typical tonnage (In isolated product)
Number of reactors at 13 kg/h processed per reactor in 1X
Feed concentration in wt%3 5 20 50 100
10 kg / day 1 1 1 1 1
100 kg / week 2 1 1 1 1
5 mT / month 19 –10-5 12-6 3 2 1
100 mT / year 16 - 8 19-10- 5 5 2 1
50 mT / 3 month 32-16 19-10 10-5-3 4 2
400 mT / year 32 19 19-10-5 8-4-2 4
1,000 mT /year 48 24-12 18-9 10-5-3
10,000 mT /year 119 48 24
# of 1X throughputreactor
# of 2X throughput reactor
# of 4X throughput reactor
31Advanced-Flow Reactor Technology
Full production banks
per Month per Quarter per YearReaction step 40 120 460Reaction + downstream 80 240 960
Processed in metric TONS
Two production banks, containing 4 reactor lines each, enable a multistep production capacity of up to 1,000 metric tons per year
32Advanced-Flow Reactor Technology
Fully engineered solution available with complete automation
•Multipurpose reactors or single chemistry reactors can be built into this turnkey system•50t/y up to 1,500t/y (depending on dilution)•ATEX EEx Zone II•3 liquid feeds•1 gas feed•Temperature from -60°C to +250°C
33Advanced-Flow Reactor Technology
Making News