Transcript Sensors - mikroglas chemtech GmbH

mikroglas
Technology and Products
mikroglas chemtech GmbH
Galileo-Galilei-Str. 28, 55129 Mainz
Tel.: 06131/55550-0
Fax: 06131/55550-52
[email protected]
www.mikroglas.com
an Invenios company
Available Micro Fluidic Modules
Micro reactors are commercially available for different applications, e.g.:
micro emulsifier
micro mixer
micro falling film reactor
micro heat exchanger
micro photo reactor
micro 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.
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Example for reactions in mikroglas mixer
Synthesis of Benzaldehyd from Sulfuric acid and Benzal Chloride
CHCl2
CHO
H2SO4
Properties of the reaction
liquidphase reaction: 2 phases, highly viscous, difficult to mix
exothermic reaction: cooling to 0°C necessary
conventional technology
microreaction technology
difficult mixing
fast diffusion controlled mixing
temperatur: 0°C
temperature: +70°C
yield: 65%
yield 69%
reaction time: several hours
reaction time: 6 min
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Interdigital Micromixer for liquid mixing
SEM of the
mixing chamber
- mixing of two liquid or gaseous media
- 30 channels run parallel in a mixing chamber
channels:
width 65 µm
depth 150 µm
walls:
width down to 30 µm
depth 150 µm
Developed in co-operation with
Institut für Mikrotechnik Mainz GmbH
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Direct Nitration of Toluene
Example out of EC funded project NEPUMUC
Properties of the reaction
- two-phase reaction
- very exothermic (explosive !)
50 µm channels
In usual interdigital micromixers:
Within seconds the droplets agglomerate to large plugs !
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Column micromixer
free space between columns: 50 µm
bubble size: < 40 µm
 stable emulsion
emulsion after column micromixer
plug flow coming from interdigital
micromixer
Column height: 100 µm
20,000 columns !
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Cyclone Mixer for gas - liquid mixing
homogeneous mixing within 2 s
Mixing of O2 and water (isopropanol)
dimension of the 16 nozzles:
width 50 µm / height 150 µm
mixing chamber:
diameter 10 mm
height 2,15 mm
RESULTS:
- homogeneous bubble size (~ 150µm)
- dissolution: 35g/l (equilibrium: 45 g/l)
Developed in cooperation with IMM
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Fluidic Chip for Electrochemistry
Applying voltage
Voltage
Platinum electrodes:
diameter 250 µm
Liquid Flow
Geometry:
dimension of the feeding channels
width 400 µm / height 400 µm
dimension of the connecting channels
width 150 µm / height 150 µm
Developed in cooperation with the University of Hull
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Equipment for Electro Chemistry
plant
- with syrringe pumps
- mfc for gas feed (e.g. O2, CO2, N2)
membrane reactor for electro chemistry
- with electrodes out of Au, Pt, or Cu
- integrated electrical heater
in co-operation with University of Stuttgart (Prof. Klemm)
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Micro Reactor for Photochemistry
The 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
GEOMETRY:
Reaction channel:
outer dimensions:
channel dimensions:
exposure area:
1.4 ml internal Volume
118 mm x 73 mm x 6.0 mm
1.15 m x 2.0 mm x 0.5 mm
2300 mm²
mikroglas photo reactor with
XeCl excimer lamp (308 nm 10 W)
(Heraeus Noblelight GmbH)
integrated heat exchanger
material: Foturan-Glass
fluidic connection with teflon tubes
Temperature range: -20°C up to 120°C
flow: up to 30 ml/min.
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Local Plasma Deposition of Channels
Y-mixer und Y-separator
hydrophilic
Channel geometry:
separation: 150x200 µm²
reaction:
300x200 µm²
hydrophobic
separation of:
Toluol – red coloured water
Test setup
flows: 0,1 - 2 mL/min per liquid
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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
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.
"nose"
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Upscaling
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New mikroglas reactor for high troughput
Inlet Feed 2 1/8“
Inlet Feed 1 1/8“
Heat exchanger
Inlet/Outlet ¼”
Mixer/Reactor
5 parallel mixers:
• á 96 mm x 0.5 mm x 0.5 mm
• flowrate 9 l/h at 1.5 bar
Heat exchanger
2 x 17 parallel channels:
• á 75 mm x 2.0 mm x 0.5mm
• flowrate 150 l/h at 0.3 bar
Heat exchanger
Inlet/Outlet ¼”
Product Outlet 1/8“
mikroglas microreactor with
redesigned heat exchanger
for low pressure drop
and integrated preheater
for feed streams.
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New mikroglas reactor for high troughput
Pressure loss depending on volume flow
[Reactor]
1,80
Pressure loss [bar]
1,60
1,40
1,20
1,00
0,80
0,60
0,40
0,20
0,00
0,00
20,00
40,00
60,00
80,00
100,00
120,00
140,00
160,00
Volume flow [ml/min]
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New mikroglas reactor for high troughput
Pressure loss depending on volume flow
[Heat exchanger]
Pressure loss [bar]
0,30
0,25
0,20
0,15
0,10
0,05
0,00
0,00
500,00
1000,00
1500,00
2000,00
2500,00
3000,00
Volume flow [ml/min]
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Production scale
Number of reactors at 10 kg/h throughput per reactor
Product
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
50
14
6
4
1000 T/year
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/year
down to a feed concentration of 20 wt%!
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mikroSyn in Vitamin A production
8 heat parallel exchanger moduls
• inlet temperature 70°C
• outlet temperature < 60°C
• inlet pressure from 2 up to 3 bar
• outlet pressure 1 bar
• flowrate 200 l/h
Cooling water:
• inlet temperature 25°C
• outlet temperature < 40°C
• inlet pressure 3 bar
• outlet pressure 1 bar
• flowrate 200 l/h
Source: Roche AG
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Equipment
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Chemical Plant
Set screw
Inlet
Outlet
Outlet pressure
relief valve
microreactors
Sensor block
sensors
control software
fluidic connection
equipment
with pumps, heater/cooler,
automation, analytics
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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
pH-sensor
viscosity sensor
sensorblock for press. & temp.
with pressure reliefvalve
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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
E1
P1
P3
sensors
V3
V4
sensors
mixer
E2
P2
cooling
sensors
process control
by IR-measurement
exposure: XeCl lamp
(Heraeus Noblelight)
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IR- measurement: flow cell
transmission measurement
flow cell dimensions:
length: 8.5 mm
depth: 20/30/40 µm
Bruker Optics:
• FT-IR Spectrometer
• 375 cm-1 bis 7500 cm-1
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Photo reaction loop
E1
V3
E2
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
V4
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Electronic Control Unit
SIMATIC S7 for microreaction systems
(in co-operation with SIEMENS)
user defined receipt
mixing of 2 components
automatic modus
....with cooling circuit
• recording pressure
temperature
flow
reaction data
• controlling pumps
valves
heater/chiller
• runs with operator
as well as fully automated
(receipt control)
• safety features
pressure limit
leak detection
controlled stop function
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mikroglas Tool Box
micromixer
microreactors
mikroSyn EDU
for liquid-liquid reactions
sensors
interfaces
process control
mikroSyn II
For 2-step-reactions
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One Platform – Different Applications
mikroSyn for gas/liquid reaction
with back pressure valve
mikroSyn for
homogeneous catalysis
Different modules can be fixed easily and connected on top of a
platform with the "MicroChemTec" standard pitch.
mikroSyn for
heterogeneous catalysis
mikroSyn EDU with data collection
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New Concept for Multiple Purpose Use
mikroSyn (modular) for:
- gas/liquid, liquid/liquid reactions
- up to 3 reaction steps
- up to 5 reactants
mikroSyn for gas/liquid reaction
with back pressure valve
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Microreaction System "mikroSyn µflow"
- two step reaction
- mixing of up to 5 components
- syringe pumps for 1µl – 1 ml / min
- temperatur control (-20 to 120°C)
- Siemens SIMATIC S7
- mikroglas reactor
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Beispiel einer gelungenen KMUEntwicklung zur "nachhaltigen Chemie"
POlyKOndensation
im MIkroreaktor
Entwicklung und Test einer mikroverfahrenstechnischen Anlage mit
Steuerung und On-Line-Analytik
zur Durchführung Übergangsmetallkatalysierter C-C-Kupplungen
(Suzukikupplung) am Beispiel der
Polykondensation zu polymeren,
lichtemittierenden Halbleitern in
kontinuierlicher Produktion
Br
Pd
(II)
Br
Pd
Pd
(II)
OH
(0)
OH
B ( O H) 2
B ( O H) 2
OH
Pd
(II)
B ( O H) 3
OH
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Microreaction plants for different applications
ozonation
reaction type
reactor
pumps/tubing
detection
flow
temperature
pressure
residence time
other
reduction /
hydrogenation
polymerization
nitration
gas/liquid
homogeneous
liquid/liquid
catalytic
liquid/liquid/solid
two phase
liquid/liquid
falling film reactor
interdigital mixer
with long residence
time
capillary,
packed bed reactor,
mixing of up to 5
components
multiple feed mixer
with emulsification
piston pumps
mass flow controler
(gas)
rotary pumps
teflon tubing
gear pumps
stainless steel
capillaries
rotary pumps
teflon tubings
online MIR sensor
online MIR sensor
pH sensor
viscosity sensor
for molecular weight
pH sensor
NIR sensor
temperature sensor
liquid: 5 – 10 ml/min
gas: 100 ml/min
5 – 20 ml / min
0.1 – 1 ml / min
0.1 – 10 ml / min
0 to -60°C
0 to –15°C
80 – 120°C
10 – 40 °C
1 bar
1 bar
1 – 3 bar
3 – 6 bar
5 – 60 s
1 - 120 min
30 – 120 min
15 – 60 s
special safety
issues
special safety
issues
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Multi-Purpose-Equipment
Base Plate
Basis
Reactants
3 x liquids
1 x gas
1 x solvent
Pumps
3 Rotary Pumps
1 syrringe pump
2 gear pumps
1 MFC
µ-fluidic
Modules
Sensors
7 sensor blocks
3 T-sensors
1 IR-sensor
Valves
4x 2/2-valves
4x 2/3-valves
Reaction Plates
Ozonisation
Hydrobromation
Fluorination
Falling film
reactor
interdigital-mixer
residence mod.
Superfokus-M.
interdigital-mixer
residence mod.
catapillar-mixer
capillary reactor
3 T-sensors
2 T-sensors
2 T-sensors
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Multi-Purpose-Equipment
Baseplate
F1, F2, F3: liquid reactants
V1 – V4: 3-way valves
SB1 – SB3: sensor blocks in reactant stream SBff, SBT: sensor blocks for falling film / temp.
IR, T: IR- und temperaturesensors
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Multi-Purpose-Equipment for Ozonization
pump modules
massflow controller
electronic control module
valves
sensor blocks
reactors
exchangable
reaction 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
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