an invenios company mikroglas technology and products mikroglas chemtech gmbh galileo-galilei-str....

an Invenios company

mikroglasTechnology and Products

mikroglas chemtech GmbHGalileo-Galilei-Str. 28, 55129 Mainz

Tel.: 06131/55550-0Fax: 06131/55550-52info@mikroglas.com

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.

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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

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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