A New Step Forward for
Continuous Flow Processing
MUNICH 2017
CHEMICAL PLANT
CONTINUOUS FLOW REACTION
COMPETITIVE ADVANTAGES
CONTINUOUS vs BATCH
o Reduce reaction time: few seconds
o Less energy, solvent and reagents consumption
o Low waste management
o Complete control of highly exothermic reactions
o Manage very high pressure and temperature reactions in safe conditions
o Manage highly toxic and corrosive reagents in safe conditions
o Rapid reaction optimization: easy scale-up
o Miniaturization
RAPTOR TECHNOLOGY
La Mesta has developed a proprietary Plug Flow Reactor called
RAPTOR
Plug Flow Reactor has a series of thin coherent "plugs", each
with an uniform composition, travelling in the axial direction,
perfectly mixed in the radial direction but not in the axial
direction. Each plug is considered as a separate entity, without a
forward or a back mixing.
RAPTOR TECHNOLOGY
RAPTOR TECHNOLOGY
Reagents inlet
Stirring engine
Product outlet
Reaction
chamber
RAPTOR TECHNOLOGY
o Gas / Liquide / Solid phase reactions
o Handling of toxic or highly corrosive reagents
o Highly exothermic, high temperature or cryogenic processes
o Viscous reactions
o Solid suspension up to 30% (as starting materials or generate during reaction)
Temperature -100°C +300°C
Pressure 300 bar
Heat exchange (area/vol.) 150 m2/ m3
Residence Time 10 sec to few min
Flow rate 5 to 500 liters / h
Stirring 1500 rpm
RAPTOR TECHNOLOGY
5 Raptors are in place:
#1 (hastelloy) : flow rate 150 liters/h (production)
#2 (ss) : flow rate 30 liters/h (pilot)
#3 (hastelloy) : flow rate 50 liters/h (pilot)
#4 (hastelloy) : flow rate 50 liters/h (phosgene chemistry)
#5 (hastelloy) : flow rate 500 liters/h (production)
RAPTOR CHEMISTRY
Ammonolysis
Condensation
Grignard Chemistry
Isomerization
Phosgene Chemistry
MULTIPURPOSE EQUIPMENT
Carbonylation
Decarboxylation
Hydrogenation
Oxidation
Reductive amination
2004 2017
Raptor 1 2004
ISOMERIZATION
2007
PROJET at PILOT SCALE: 18
VOLUME PRODUCED AT RAPTOR 130MT
PROJECT TESTED in RAPTOR: 60
Raptor 2 2006
Raptor 3 2008
Raptor 4 2008
Raptor 5 2016
CARBONYLATION 2009
PHOSGENATION 2
2012
PHOSGENATION 1
2011
MAIN INDUSTRIAL PRODUCTIONS WITH RAPTOR
DECARBOXYLATION
2015
CONDENSATION
2017
MULTIPURPOSEWORKSHOP for CONTINUOUS
PROCESS
2017
ISOMERIZATION
Temperature 35-4’0°C
Residence Time 6 sec.
Productivity 26.5 kg/h
Conversion 100 %
Production Campaign 20 MT 9 weeks
Fine Chemical for Flavor & Fragrance
RAPTOR LAYOUT
CARBONYLATION
Temperature 45°C
Pressure CO 45 bar
Alcohol in CH2Cl2 40% w/w
Residence Time 30 sec.
Triflic acid 50% w/w
Yield 84%
Production Campaign 2MT 3 weeks
API in cGMP
PHOSGENATION 1
Temperature 35-45°C
Pressure COCl2 0 bar
Phosgene Excess 5% mole
Residence Time 12 sec.
Productivity 16 kg/h
Conversion Complete
Production Campaign 2MT 3 weeks
API in cGMP
PHOSGENATION 2
Temperature 85-90°C
Pressure COCl2 < 1.0 Bar
Phosgene Excess 5% mole
Residence Time 12 sec.
Productivity 3.1 kg/h
Conversion Complete
Production Campaign 0.2MT 1 week
Fine Chemical for Cosmetic
RAPTOR LAYOUT
Process control
Phosgene generation
Continuous reaction
DECARBOXYLATION
Starting Material for Fine Chemical
Temperature 45°C
Generation of CO2 124.8 g /min
Residence Time 8 sec.
Productivity 20 kg/h
Volume CO2 per Campaign 317 M3
Production Campaign 2MT 1.5 weeks
Hazardous Reaction: uncontrolled CO2 gas evolution
RAPTOR LAYOUT
SULFONIC ESTER CONDENSATION
Annual production: 60 MT
Exothermic Reaction
Starting Material for Fine Chemical
Washing – Separation in Continuous
Distillation in continuous (THIN FILM EVAPORATOR)
DEDICATED AREA TO THE CONTINUOUS PROCESS
CONTINUOUS LAYOUT
MULTIPURPOSE CONTINUOUS FLOW
WORKSHOP
CONTINUOUS VS BATCH
BATCH CONTINUOUS
Annual production 60 MT
Equipment used Vessel (6000liter) + tanks Raptor (0,001liter) + tanks
Duration of Production 25 weeks 10 weeks
Productivity 42 kg/h 133 kg/h
Cooling Brine Water
Reaction temperature 10 – 15°C 65°C
Toluene 3,5 vol 1,75 vol
Water (washing) 4 vol 2 vol
Excess CMS & TEA 30% 10%
Product Quality Orange
(purification step needed) Pale yellow
Waste 6,2 kg /kg 3kg / kg
RAPTOR SUMMARY
PROJECTS TESTED IN RAPTOR: 60
PROJECTS MOVED AT LEAST TO PILOT / PRODUCTION: 18
MORE THAN 130 MT PRODUCED USING RAPTOR TECHNOLOGY
MULTIPURPOSE CONTINOUS FLOW WORKSHOP
THANK YOU FOR YOUR ATTENTION