corning ® advanced-flow™ reactors: engineered for...

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

2 Reactor Technologies © Corning Incorporated 2013

Corning ® Advanced-Flow™ Reactors

A business based on 160 years of worldwide innovation


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.


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



Offers broad capability from feasibility to production and enables the transition from batch to continuous processes


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


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)


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


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)


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


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)



Ensures superior mass & heat transfer, enabling excellent processes intensification


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


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


• 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



Minimizes scale-up failures and drastically reduces the time from laboratory to production


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


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


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



Case studies have demonstrated the benefits of using AFR in pharma and fine chemical applications for safer, greener, cheaper and effectively more sustainable processes.


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, …)


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



• 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

http://www.uk-cpi.com/index.html



• 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



Now it is easy to FLOW with Corning ® Advanced-Flow™ Reactors


Thank you!

Questions ?

www.corning.com/reactors

[email protected]

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