an invenios company mikroglas technology and products mikroglas chemtech gmbh galileo-galilei-str....
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an Invenios company
mikroglasTechnology and Products
mikroglas chemtech GmbHGalileo-Galilei-Str. 28, 55129 Mainz
Tel.: 06131/55550-0Fax: 06131/[email protected]
www.mikroglas.com
an Invenios company
Available Micro Fluidic Modules
Micro reactors are commercially available for different applications, e.g.:
micro mixer
micro heat exchanger
micro reactor
micro emulsifier
micro falling film reactor
micro photo reactor
Different materials are available: glass, metal, ceramics, silicon, etc.Different designs for different applications are available.Handling of gases, liquids and particles are possible.
an Invenios company
Example for reactions in mikroglas mixer
Synthesis of Benzaldehyd from Sulfuric acid and Benzal Chloride
Properties of the reaction
liquidphase reaction: 2 phases, highly viscous, difficult to mixexothermic reaction: cooling to 0°C necessary
temperatur: 0°C temperature: +70°C
difficult mixing fast diffusion controlled mixing
conventional technology microreaction technology
yield: 65% yield 69%
CHCl2 CHO
H2SO4
reaction time: several hours reaction time: 6 min
an Invenios company
Interdigital Micromixer for liquid mixing
- mixing of two liquid or gaseous media
channels:width 65 µmdepth 150 µm
walls:width down to 30 µmdepth 150 µm
- 30 channels run parallel in a mixing chamber
SEM of themixing chamber
Developed in co-operation withInstitut für Mikrotechnik Mainz GmbH
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Direct Nitration of Toluene
Properties of the reaction- two-phase reaction- very exothermic (explosive !)
In usual interdigital micromixers:Within seconds the droplets agglomerate to large plugs !
50 µm channels
Example out of EC funded project NEPUMUC
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Column micromixer
plug flow coming from interdigital micromixer
emulsion after column micromixer
free space between columns: 50 µmbubble size: < 40 µm stable emulsion
Column height: 100 µm20,000 columns !
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Cyclone Mixer for gas - liquid mixing
Mixing of O2 and water (isopropanol)
dimension of the 16 nozzles:width 50 µm / height 150 µm
mixing chamber:diameter 10 mmheight 2,15 mm
Developed in cooperation with IMM
RESULTS:- homogeneous bubble size (~ 150µm)- dissolution: 35g/l (equilibrium: 45 g/l)
homogeneous mixing within 2 s
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Fluidic Chip for Electrochemistry
Geometry:
dimension of the feeding channelswidth 400 µm / height 400 µm
Developed in cooperation with the University of Hull
dimension of the connecting channelswidth 150 µm / height 150 µm
Liquid Flow
Voltage Platinum electrodes:diameter 250 µm
Applying voltage
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Equipment for Electro Chemistry
in co-operation with University of Stuttgart (Prof. Klemm)
membrane reactor for electro chemistry- with electrodes out of Au, Pt, or Cu- integrated electrical heater
plant- with syrringe pumps- mfc for gas feed (e.g. O2, CO2, N2)
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Micro Reactor for PhotochemistryThe synthesis of bioactive compounds by photodecarboxylative addition of carboxylates to phthalimides
S. Gallagher, F. Hatoum, M. Oelgemöller and A. G. Griesbeck, Book of Abstracts, Central Europ. Conf. on
Photochemistry (CECP 2008), Bad Hofgastein,Austria, February 2008, p. 69.
results:- significant reduction of the reaction time- yield 97%- channel length: 1.4 m- flow: 0,08 ml/min- residence 21 min- exposure at 300 nm (Luzchem UB Panel)
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mikroglas photo reactor
mikroglas photo reactor withXeCl excimer lamp (308 nm 10 W)(Heraeus Noblelight GmbH)
GEOMETRY:Reaction channel: 1.4 ml internal Volumeouter dimensions: 118 mm x 73 mm x 6.0 mmchannel dimensions: 1.15 m x 2.0 mm x 0.5 mmexposure area: 2300 mm²
integrated heat exchangermaterial: Foturan-Glassfluidic connection with teflon tubesTemperature range: -20°C up to 120°C flow: up to 30 ml/min.
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Local Plasma Deposition of Channels
separation of:Toluol – red coloured water
Y-mixer und Y-separator
hydrophilic
hydrophobic
Test setup flows: 0,1 - 2 mL/min per liquid
Channel geometry: separation: 150x200 µm² reaction: 300x200 µm²
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Gas - Liquid Separation
triangular or arrow shaped separation modules chamber depth: 500 µm
with surface modification
hydrophilic
hydrophobic
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Modification of Micro Settler
"nose"
Separation has been optimized by:- A "nose" breaks adhesion of liquid bubbles at upper wall.- Active pumping keeps liquid level in settler constant.- Surface modification holds liquid in lower half of settler.
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Upscaling
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New mikroglas reactor for high troughput
Mixer/Reactor5 parallel mixers:• á 96 mm x 0.5 mm x 0.5 mm• flowrate 9 l/h at 1.5 bar
Inlet Feed 1 1/8“Inlet Feed 2 1/8“
Product Outlet 1/8“
Heat exchangerInlet/Outlet ¼”
Heat exchangerInlet/Outlet ¼”
Heat exchanger2 x 17 parallel channels:• á 75 mm x 2.0 mm x 0.5mm• flowrate 150 l/h at 0.3 bar
mikroglas microreactor withredesigned heat exchangerfor low pressure dropand integrated preheaterfor feed streams.
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New mikroglas reactor for high troughput
Pressure loss depending on volume flow [Reactor]
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
1,60
1,80
0,00 20,00 40,00 60,00 80,00 100,00 120,00 140,00 160,00
Volume flow [ml/min]
Pres
sure
loss
[bar
]
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New mikroglas reactor for high troughput
Pressure loss depending on volume flow [Heat exchanger]
0,00
0,05
0,10
0,15
0,20
0,25
0,30
0,00 500,00 1000,00 1500,00 2000,00 2500,00 3000,00
Volume flow [ml/min]
Pres
sure
loss
[bar
]
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Production scale
ProductNumber of reactors at 10 kg/h throughput per reactor
Feed concentration in wt%
3 5 20 50 100
10 kg/day 2 1 1 1 1
100 kg/week 3 2 1 1 1
5 T/month 25 15 4 2 1
10 T/month 50 30 8 3 2
50 T/year 21 13 4 2 1
100 T/year 50 25 7 3 2
1000 T/year 50 14 6 4
Day: 24h Week: 120 h Month: 667h Year 8000h
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Numbering up of Reactors
Stack out of 4 mikroglas microreactors which can run in series or parallel.E.g. with this setup one can reach a production capacity of 50 T/yeardown to a feed concentration of 20 wt%!
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mikroSyn in Vitamin A production
8 heat parallel exchanger moduls
Source: Roche AG
Cooling water:• inlet temperature 25°C• outlet temperature < 40°C• inlet pressure 3 bar• outlet pressure 1 bar• flowrate 200 l/h
• inlet temperature 70°C• outlet temperature < 60°C• inlet pressure from 2 up to 3 bar• outlet pressure 1 bar• flowrate 200 l/h
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Equipment
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Chemical Plant
fluidic connection
equipmentwith pumps, heater/cooler, automation, analytics
microreactors
Inlet
Outlet
Set screw
Outlet pressure relief valve
Sensor block
sensors
control software
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Connecting microreactors
• teflon tubing • standard HPLC-Fittings• thermal insulation• maximum pressure: 20 bar
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Sensors for process control
ATR-IR-sensor
sensorblock for press. & temp.with pressure reliefvalve
viscosity sensor
pH-sensor
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Photo Cycloaddition
Photo Cycloaddition of Benzaldehyde to 2,3-Dihydrofuran(one-step, liquid/liquid reaction, no catalyst)
temperature -20°C – 120°C
pressure 10 bar
solvent ethanol
residence time minutes to hours (conv: 14 hrs.)
volume flow 0.1 ml/min - 10 ml/min
production volume approx. 1 kg/day
inlets for 2 reagents, 1 inert gas, 1 cleaning
sensors pressure, temperature, IR (product analysis)
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Flow diagram for photo reaction plant
reaction loop
P1
P2
E1
E2
V3 V4
P3sensors
sensors
sensors
cooling
mixer
exposure: XeCl lamp(Heraeus Noblelight)
process control by IR-measurement
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IR- measurement: flow cell
transmission measurement
flow cell dimensions:length: 8.5 mmdepth: 20/30/40 µm
Bruker Optics:• FT-IR Spectrometer• 375 cm-1 bis 7500 cm-1
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Photo reaction loop
E1
E2
V3V4
P3
- reagents E1 and E2 are mixed - mixture enters photo reaction loop- pump P3 pumpes through loop- IR sensors measures conversion- at maximum conversion valve V4 opens- rinsing of loop with sovent- start again
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Electronic Control Unit
SIMATIC S7 for microreaction systems(in co-operation with SIEMENS)
• recording pressure temperature flow reaction data
• controlling pumps valves heater/chiller
• runs with operatoras well as fully automated(receipt control)
• safety featurespressure limitleak detectioncontrolled stop function
user defined receipt automatic modus
mixing of 2 components ....with cooling circuit
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mikroglas Tool Box
micromixer
microreactors
interfaces
process control
sensors
mikroSyn IIFor 2-step-reactions
mikroSyn EDUfor liquid-liquid reactions
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One Platform – Different Applications
Different modules can be fixed easily and connected on top of a platform with the "MicroChemTec" standard pitch.
mikroSyn for gas/liquid reactionwith back pressure valve
mikroSyn forheterogeneous catalysis
mikroSyn forhomogeneous catalysis
mikroSyn EDU with data collection
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New Concept for Multiple Purpose Use
mikroSyn for gas/liquid reactionwith back pressure valve
mikroSyn (modular) for:- gas/liquid, liquid/liquid reactions- up to 3 reaction steps- up to 5 reactants
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Microreaction System "mikroSyn µflow"
- mikroglas reactor
- Siemens SIMATIC S7
- mixing of up to 5 components
- syringe pumps for 1µl – 1 ml / min
- temperatur control (-20 to 120°C)
- two step reaction
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Entwicklung und Test einer mikro-verfahrenstechnischen Anlage mit Steuerung und On-Line-Analytik zur Durchführung Übergangsmetall-katalysierter C-C-Kupplungen (Suzukikupplung) am Beispiel der Polykondensation zu polymeren, lichtemittierenden Halbleitern in kontinuierlicher Produktion
POlyKOndensation im MIkroreaktor
Pd(II)
Br
Br
Pd(0)
Pd(II)
OH
B (OH)2
OH
Pd(II)
B
OH
(OH)3
OHB (OH)2
Beispiel einer gelungenen KMU-Entwicklung zur "nachhaltigen Chemie"
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Microreaction plants for different applications
ozonation reduction / hydrogenation
polymerization nitration
reaction type gas/liquidhomogeneous
liquid/liquidcatalytic
liquid/liquid/solidtwo phase liquid/liquid
reactor falling film reactorinterdigital mixer
with long residence time
capillary,
packed bed reactor,
mixing of up to 5 components
multiple feed mixer with emulsification
pumps/tubingpiston pumps
mass flow controler (gas)
rotary pumps
teflon tubing
gear pumps
stainless steel capillaries
rotary pumps
teflon tubings
detection online MIR sensor online MIR sensor pH sensor
viscosity sensorfor molecular weight
pH sensor
NIR sensor
temperature sensor
flowliquid: 5 – 10 ml/min
gas: 100 ml/min5 – 20 ml / min 0.1 – 1 ml / min 0.1 – 10 ml / min
temperature 0 to -60°C 0 to –15°C 80 – 120°C 10 – 40 °C
pressure 1 bar 1 bar 1 – 3 bar 3 – 6 bar
residence time 5 – 60 s 1 - 120 min 30 – 120 min 15 – 60 s
otherspecial safety
issuesspecial safety
issues
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Multi-Purpose-Equipment
Basis Ozonisation Hydro-bromation
Fluorination
Reactants 3 x liquids
1 x gas
1 x solvent
Pumps 3 Rotary Pumps 1 syrringe pump2 gear pumps1 MFC
µ-fluidic Modules
Falling film reactor
interdigital-mixer
residence mod.
Superfokus-M.
interdigital-mixer
residence mod.
catapillar-mixer
capillary reactor
Sensors 7 sensor blocks
3 T-sensors
1 IR-sensor
3 T-sensors 2 T-sensors 2 T-sensors
Valves 4x 2/2-valves
4x 2/3-valves
Base Plate Reaction Plates
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F1, F2, F3: liquid reactants V1 – V4: 3-way valvesSB1 – SB3: sensor blocks in reactant stream SBff, SBT: sensor blocks for falling film / temp.IR, T: IR- und temperaturesensors
Multi-Purpose-EquipmentBaseplate
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Multi-Purpose-Equipment for Ozonization
pump modules
sensor blocks
valves
massflow controller
reactors
electronic control module
exchangablereaction plate
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Modular Equipment
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mikroSyn Equipment
flexible laboratory equipment for research and development
multi-purpose equipment for development and small scale production
automated plants for production in chemical facilities