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T H E C ATA L O G U E

> chemical micro process technology made by imm

5/09

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THE NEW CATALOGUE – DIVERSIFIED IN PARTS & INTEGRATED AS APPROACH It is always a pleasure to introduce the next generation of development and to sum up what this is about and what is beyond. The new catalogue comprises a diversified, but also refocused offer of microstructured reactors and their processing plants. All ears on benefit New technologies create new opportunities and may strengthen the competitiveness, but also demand for careful implementation and use at the right spot. Technological overshoot and veering away from demand is to be avoided. IMM’s micro process technology ever since is truly devoted to real-life applications in the field of chemical processing, fuel processing, consumer goods, etc. guided by a wealth of experience in customers’ needs. This ‘echo box’ mirrors the long lasting and steady information exchange about user’s practise from innumerable direct discussions, but also arising from the excerpts and essences attained from the global platforms such as symposia, platforms and expert groups’ meetings. More than meets the eye Single developments into an entirely new direction should not be isolated, but should be governed and marshalled by a persistent general idea how to approach the endeavour. Leitmotifs of IMM’s process technology are: • Scale-out – from laboratory to production scale • System integration – from single devices to integrated reactors and plants • Holistic view – from conventional to novel process windows • Accommodate as appropriate – from micro to milli scale Continuing roots and shaping up for future quests

Central new feature in the ‘basket of goods’ are pilot- and production-scale microstructured reactors and whole respective reactor systems, stemming from validated and (partially) documented developments within industrial driven national and European projects; all oriented towards target production and prove (cost) competitiveness. Two such highlights exemplary for the whole approach & portfolio are a setup comprising a modular micro-reactor followed by a milli-scaled tube bundle for the production of ionic liquids at a capacity of 100 kg/d and pilot- and productionscale microstructured Falling Film Microreactors. Both have stood the test in demonstration processing at industrial sites. Both serve to show how micro process engineering can speed up the scale up process.

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Branch and whole tree Process intensification is a dramatic and far-reaching change in chemical production technology. The same holds for microreaction technology as the major PI approach. Needed is interdisciplinary bridging in the format of a comprehensive and holistic micro process development. This may be subsumed in five PI pillars “Catalysts – Fabrication – Reactors – Plants – Processes”. It is the vision and skills on catalysts, fabrication and processes which adds to the hardware development based on reactors and plants. Thus, as desired from the requirements of the customer functionalisa tion of the microstructured reactor can be supplied which is the key to performance improvement of many chemical reactions. Process windows which are far away from usual practise are often tailor-made to optimal micro processing – prolific soil on no man‘s land. The afore mentioned improved high-pressure operation and the use of special materials for high temperature applications are just two reactor construction measures in this direction. Fill in the blank and knocking at the door to new applications Besides a holistic system-oriented approach, the catalogue simply needs to be steadily complemented bit by bit. This is done shoulder to shoulder with IMM’s new research and development directions. Although not all of these have already been solidified in the new catalogue and if so not to the same degree, the present portfolio has closed gaps and extends the range of application beyond chemistry. • Micro processing architectures with modular building blocks for integration of mixing, reaction, and other operations • Separation and purification processes suited to continuous flow • New heating concepts (microwave) and solventless/-free processing (ionic liquids; supercritical fluids) • New applications: personal care, consumer goods, cosmetics, (functional) materials synthesis

Catalysts

Fabrication

Processes Plants

Reactors

IMM has developed brazing as a highpressure interconnection technique suited for large formats and numbers. This fabrication innovation assumed shape in the new numbered-up microstructured pilot reactors as depicted in this catalogue. IMM is well versed in catalyst optimisation and coating.

It is our desire that the users of the tools in the catalogue will achieve as much process intensification as possible, hopefully exceeding what is needed and what was hoped – mirrorrotating the motto, largely known in the microreactor community and synonym for avoiding “white elephant’s directives “as much ‘micro’ as needed, not as technically possible”. Enjoy reading this new compendium and we appreciate if you contact us for discussion or inquiry at catalogue@imm-mainz.de or +49-(0)6131-990 0. Volker Hessel Institut für Mikrotechnik Mainz GmbH

4-di-isocyanate 02 Plants Contents Organic Synthesis Plant Impinging-Jet Microreactor Plant for Precipitation Reactions Cream and Emulsification Plant Modular Microreactor Systems for Production Plants Falling Film Micro Reactor Plant Gas Phase Reactor Test Plant Fuel Processor Demonstration Plant Mixer-Settler Continuous Work-Up Plant 03 Components Contents Overview applications Mixing principles Liquid/Liquid and Gas/Liquid Mixers or Reactors Special Gas Liquid Reactors Gas Phase Reactors Heat Exchangers 04 Annex General terms and conditions of sale References 1 3 4 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 28 30 32 34 36 38 40 42 43 44 45 46 58 68 76 84 84 87 . Yellow 12 Hydrogenation of nitrobenzene Direct fluorination of toluene with elemental fluorine Sulphonation of toluene Direct hydrogen peroxide synthesis out of the elements [4+2] cycloaddition of singlet oxygen to cyclopentadiene to make cyclopentene-1.CONTENTS > superior products made by imm 3 Preface Contents Testing and quality control 01 Processes Contents Kolbe-Schmitt synthesis Michael Addition Solvent-free thiophene bromination Synthesis of an imidazole-type ionic liquid Phenyl boronic acid synthesis (S)-2-Acetyl tetrahydrofuran synthesis Synthesis of intermediate for quinolone antibiotic drug Nitro glycerine production plant Brominations of aromatics and alkylaromatics Synthesis of an azo pigment dye.4-diol Side-chain photochlorination of toluene-2.

Beyond multi-functionality. improvement of robustness. in absolute terms or as specific properties. For reasons of transparency the following specific technical quality features are given additionally on the backside of each micro device‘s description in the catalogue: • Specifications • Options • Performance Data • Applications & References tion channel platelets made of various materials.g. e. reac- Leakage rate tests Our devices meet the requirements of complex.g. IMM is aware that despite the novelty of the devices. This catalogue makes the first move to bring novel and highly innovative products for chemical micro process engineering to the customer. to characterise mixing. Specifications This is your guideline for your check on material compatibility and fit into existing environment (e. evaporation. leakage rates. more detailed information on processing is given. the first basic versions of the devices were usually tested by partners or third parties being experts in the field of the micro device‘s application. IMM tries to serve such demands on customized solutions. In selected cases. Any further information that is relevant and not included for reasons of limited space is referred in „Applications & References“. The result will be expressed in the well-established way to classify leakage classes. Relevant dimensions are listed here. The results are documented in many peer-reviewed publications which are referred in the respective device‘s description. Said data are supplemented by geometric parameters comprising information on internal volumes or surfaces. First of all. Performance characterization IMM aims at disclosing the functioning of its devices largely as well as at showing their limits. Reaction engineering data such as conversions or space-time yields may be given as well. e. detailed analyses and should not only be suited for making snapshots on feasibility. IMM thereby applies known and recommended procedures for leak testing of large-scale apparatus which are modified to the needs of microflow devices. etc. Here. Besides such in-house testing. different fluid connectors.g. vice versa. devices are regularly controlled by inhouse leakage rate tests. or incorporation of specialty functions (e. In this context. we identified application-unique uses for the micro devices and. produce more and more custom-designed tools. For instance.g. including description of hydrodynamics such as flow patterns or interfacial areas for selected parameter sets. This particularly provides an independent assessment – either from the industrial or scientific point of view – concerning the performance of the devices. as L0. The catalogue comprises both off-theshelf products and demonstrators that are ready for supply according to customers needs. and reaction processing. we do not only invest in scientific and technological promotion of our devices. From all these contents of Performance Data. but also in quality control. For this reason. our Quality Assurance policy is realised by a Quality Management System certified according to DIN EN ISO 9001. residence times and more. Our delivery times try to match our time demand to fabricate a small series or even individual pieces only as well as your wish to start work as soon as possible. If needed. This enables you to judge whether the device meets basic requirements of the process or not.01.g. three presently important aspects are exemplarily discussed more in detail below. internal dimensions or simply fluidic peripherals may need to be changed. Options Since different customers have different demands on how a reactor might fit best to their intended application. heat exchange.TESTING AND QUALITY CONTROL 4 Testing and quality control of IMM micro reactor devices and plants People often complain that innovations need too much time and consume too much money until they are available for industry and society. For this reason. The information on these applications result from own or by partners practised chemistry as well as disclosed customer processes. e. of an inspection window). applicable flow rates. The setting of these tests orients on ASME and EU standards on leakage testing. material. IMM regards such off-the-shelf delivery as indispensable to enable a technological break-through. Performance Data Performance Data include information on temperature and pressure stability. Development of measuring techniques IMM does not only use state-of-the-art measuring techniques for device performance characterisation but also actively develops new techniques that . they have to fulfil the demands of industrial processing. by comparing outer dimensions). Delivery Time As we know. leak tightness at the best possible rate is absolutely essential for correct balancing of all streams and avoiding contamination of the environment. all based on experimental evidence. Their functioning indeed can be thoroughly characterised and must be benchmarked to known apparatus and techniques. materials. leak tightness will be measured at elevated pressures and temperatures.and construction-based parameters. IMM runs several test set-ups. Our devices can act as multi-purpose tools for a diversified range of applications. supplying proper fluid connections. In addition to these basic. we typically offer a variety of. more data are summed up in a graph in our assembly manual. you do not have much time until you need to set work on your measurement or processing.

Means. NaOH. You can be sure that the list of citations comprises the latest and most relevant information available on IMM‘s micro devices. France (Ind. Applications & References Information that is missing in the product sections might be found in the citations. (Chem. The acid-catalysed reaction of potassium iodide with potassium iodate to elemental iodine competes with the faster neutralisation of the acid by a borate buffer-system. 101 (2004) 409-419). The formed iodine can be then detected as triiodide complex by UV-Vis spectroscopy with absorption band centred at 286 and 353 nm.➞ I3(detectable by UV/Vis spectroscopy) In the experiments a buffered solution of KI/KIO3 is mixed with diluted sulphuric acid. IMM tests its micro mixers with regard to mixing performance experimentally using the so-called “Villermaux/Dushmann method”. A large number of micro mixers using different functional principles is available in the meantime. IMM uses the chemical protocol described by S. 38. we would like to point out that IMM was the first to suggest an advanced mixing test procedure for flow-through devices (besides simple visual inspection of colouring/ neutralisation) by modification of an approach used for batch apparatus originally. we limited this list to most relevant books and reviews. . In case of ideal mixing the acid is only consumed by the fast neutralisation. KIO3. Res. J. The more iodine is detected the less ideal is the mixing perfomance. This solution was prepared directly in front of the experiments by mixing the following two solutions in a volumetric ratio of 1:1: Solution 2a: c(KI) = 0. However. if mixing is less ideal iodine is formed by the comproportionation reaction.00635 mol/L c(NaOH) = 0. Chem. Therefore. developed by the Villermaux group in Nancy.0909 mol/L c(H3BO3) = 0. Eng. H3BO3.0909 mol/L Experimental Determination of Mixing Performance of Microfluidic Devices by the “Villermaux/Dushmann method” Mixing has a decisive impact on the overall performance of microreaction processes. In this context. 3 (1999) 1075-1082). there is an increased need for measuring and comparing mixing performance. The determination of mixing performance by the Villermaux/Dushman method is based on the competition of two parallel reactions. In the following the concentrations and preparation of the two solutions.0909 mol/L Solution 2b: c(KIO3) = 0. pumped in the experiments at a volumetric flow rate ratio of 1:1 is given: Solution 1: A sulphuric acid solution with c(H2SO4) = 0.0909 mol/L c(H3BO3) = 0.5 are considered to comprise the essential information for the customer. Eng. Panic et al. Relevant chemical formulas: + H2BO3 + H ➞ H3BO3 (very fast) + 5 I. Solution 2: A solution of KI.030 mol/L.+ IO3 + 6 H ➞ 3 I2 + 3 H2O (fast) I2 + I.0319 mol/L c(NaOH) = 0.

PROCESSES 6 01 .

4-di-isocyanate 23 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 01 . Yellow 12 Hydrogenation of nitrobenzene Direct fluorination of toluene with elemental fluorine Sulphonation of toluene Direct hydrogen peroxide synthesis out of the elements [4+2] cycloaddition of singlet oxygen to cyclopentadiene to make cyclopentene-1.CONTENTS > processes made by imm 7 PROCESSES Processes Kolbe-Schmitt synthesis Michael Addition Solvent-free thiophene bromination Synthesis of an imidazole-type ionic liquid Phenyl boronic acid synthesis (S)-2-Acetyl tetrahydrofuran synthesis Synthesis of intermediate for quinolone antibiotic drug Nitro glycerine production plant Brominations of aromatics and alkylaromatics Synthesis of an azo pigment dye.4-diol Side-chain photochlorination of toluene-2.

4. efficient mixing and shortening of residence time to the kinetically limit become important drivers for process optimization. This benefit is counterbalanced by thermal degradation of the reactants and the products.KOLBE-SCHMITT SYNTHESIS 8 Motivation and Results 01 Low pressure operations under reflux conditions are typically favored for laboratory flasks and agitated tanks. a system pressure of 50 bar is enough to maintain single-phase operation (i.6-trihydroxy benzoic acid.4-dihydroxy benzoic acid (see scheme below) and 2. Applied Process Parameters • Pressure: 40 – 80 bar • Temperature: 100 – 220°C • Reaction time: 4 – 390 s Benefits through Process Intensification • Increase in space-time yield by factor 440 • Increase in productivity by factor 4 • Possibly circumventing the more tedious original KolbeSchmitt route with autoclave operation and aggressive earth alkaline hydroxide bases . For the aqueous-based Kolbe-Schmitt synthesis with resorcinol and phloroglucinol shortenings in reaction time by orders of magnitude (up to a factor of 2000) were achieved in this way. no gas content and no boiling) even at temperatures up to 100°C higher than boiling points of typical solvents. Accordingly. in particular by decarboxylation of the 2.T processing. Micro reactor rigs on the other side allow a simple operation of liquid phases under high pressures and high temperatures.e. the maximum temperature of many organic routes is often simply defined by the solvent boiling point. Thus. The faster operation at higher temperatures typically is paid by more side and consecutive reactions. This has been termed high-p. For instance.

while the experiments were extended up to 200°C. Yields of up to 99% at about full selectivity were achieved. In addition.MICHAEL ADDITION 9 The merit of high-p.T processing (see initial chapter and under Kolbe-Schmitt synthesis for definition) was investigated for six Michael additions of two α. Extended processing times of up to 48 hours were reduced in this way down to a few minutes. The duration of the batch processing times is here much larger than kinetically needed to avoid too large heat releases and therefore the reactant is added drop by drop (see also “all-at-once“ procedures). for the diethyl amine with a boiling point of -55°C. effects of higher temperature are given. best operation was at 100°C. For example. since the reaction is carried out at much higher temperatures than the boiling points of the amines.β-unsaturated carbonyl compounds and three amines. Reaction times and consequently space-time yields were reduced by order of magnitude in this way. 01 Applied Process Parameters • Pressure: 3 – 20 bar • Temperature: 20 – 90°C • Reaction time: 2 – 30 min Benefits through Process Intensification • Reduction of reaction time from 24 h (batch) to a few minutes • Increase in space-time yield by factor 650 • Increase in productivity by factor 4 • Yields up to 99% PROCESSES Motivation and Results .

The micro reactor operation led to yields of 2. Even then they often are added slowly drop by drop to allow heat transfer to be adjusted to heat release. which is better than for home-made (77% yield) and literature (50% yield) batch processing. This unnecessarily prolongs processing time and also the reaction then is carried out for a considerable part under totally changing reactant concentrations (from zero to full-load content). a fast parametric study could be done for finding optimal operating conditions. Applied Process Parameters • Pressure: 1 bar • Temperature: -10 – 0°C • Reaction time: A few ms Benefits through Process Intensification • Continuous process with flexible output at constant selectivity of 80% • Use of pure bromine. Using the pure feeds and higher temperature. at nearly complete conversion. microstructured reactors with their efficient heat and mass transfer have the potential to contact the full reactant load “all-at-once“. micro reactors can cope with concentrated solutions or even pure liquid reactants. In addition. this may take a long time. up to hours. The bromination of thiophene investigated used pure thiophene and pure bromine flows at temperatures from -10°C to room temperature.S O LV E N T. On the contrary. decomposed at the spot • Simple control over substitution degree . Due to the easiness to change reactant ratios and temperatures in the micro reactor rig. the space-time yields were by order of magnitude higher for the continuous micro reactor process. There are several examples known that such “all-at-once“ or solvent-free procedures are feasible in micro reactors with reasonable selectivity. Correspondingly. whereas the same contacting led to vigorous reactions and even explosions (when done under special safety precautions with miniature volumes).F R E E T H I O P H E N E B R O M I N AT I O N 10 Motivation and Results 01 In batch processing aggressive reactants typically are diluted to prevent thermal overshooting and runaway. In some cases. the reaction time was decreased from about two hours (for batch) to less than one second (for micro mixer reactor).5-dibromothiophene up to 86%.

Exemplarily. i. and addresses especially the need for temperature control during the reaction. In order to improve heat removal for the higher flow rates.g. the formation of unwanted side products. The maximum temperature rise above thermostat temperature was reduced from 50°C to 10°C with this reactor modification. The challenge is further increased by favourably working without any solvents which is expected to result in temperature increase. therefore the first two reactor sections where exchanged by 1/16˝ tubes with same internal volume as the replaced 1/8˝ tubes. Obviously. The exothermic synthesis of an ionic liquid was carried out in this way in a micro reactor rig. This finding.48 ml/min beginning at a reactor volume of 15%. Furthermore. however. With regard to production purposes based on these experimental results an adapted reactor concept for higher flow rates was derived. since a good portion of the reaction is occurring after the first two tube sections and therewith not affected by smaller dimensions in the first two tubes.96 ml/min) the modification did not prevent hot spot formation. however. The testing is now in preparation.g. an approach was to use finer structures. the heat removal capacity of the 1/8˝ tubes is sufficient in large parts of the reactor. 1/16˝ tubes instead of 1/8˝ tubes. The smaller tubes. Therefore. for a total flow rate of 3. since too high temperatures will lead to formation of unwanted side products decreasing product quality which is already visually observable by the yellow colouring of the otherwise clear product. The chemistry cannot be disclosed due to intellectual properties rights of the industrial user. For the highest flow rate (6. impose an increase of pressure drop which may become a limiting operational parameter. the obtained temperature profiles with such a set-up for a total flow rate of 3. 01 Applied Process Parameters • Pressure: 1 bar • Temperature: 50 – 60°C • Reaction time: 1 – 4 min Benefits through Process Intensification • Successful transfer of a batch process into a continuous one with in-line and realtime temperature monitoring • Controlled reaction albeit high exothermicity (about 100 kJ/mol) • Direct and one step contacting of the reactants in almost stochiometric ratio (“all-at-once“) • Reduction of processing time from a few hours down to 1 min • Side product formation – coloring of the product – considerably diminished • Safety issues reduced – low control & automation expenditure to prevent thermal runaway with hazardous reactants • Modularity – flexibility for different IL syntheses • Easy scalability – short time-to-market • Small CAPEX costs at reduced plant footprint • Legislation – fast authority approval • High share of working loads as compared to plant shutdown . e. yielding a clearer product.48 ml/min are given in Figure 7 with the corresponding profile of the set-up with all 1/8˝ tube sections as comparison. one can observe for a thermostat temperature of 50°C an increasing yellow colouring of the product. the reactor or the selected dimensions are not capable of removing reaction heat in a sufficient manner. Even under the advanced thermal control of a microstructured reactor.SYNTHESIS OF AN IMIDAZOLE-TYPE IONIC LIQUID 11 PROCESSES Motivation and Results A variant of the novel chemistry concept is to use solventfree processes with aggressive reactants which exhibit heattransfer sensitivity. the micro reactor rig was rebuilt in stainless steel allowing in future extending the investigations to other ionic liquid synthesis requiring higher temperatures and pressures. e. the determination of temperature profiles becomes so important by locating the reactor section where smaller tubes have to be used and therewith to minimise the use of smaller tubes to where necessary.e. As can be seen from the temperature profiles. In the following. can be explained by looking at the determined temperature profiles. The micro reactor consists of a stack of platelets and heat removal is improved by integration of microstructured heat exchangers.

This can be changed when using microstructured reactors. from 5% to 1% • Process simplification: Eliminating the distillation step • Favourable room temperature operation instead of cryogenic one • Better costing of micro reactor process: Less invest (no distillation column). The yield was raised by about 25% as compared to the industrial batch production process. Thus. but also downstream purification. thereby rendering the former energy-consumptive distillation step unnecessary. having higher selectivity did not only affect the reaction itself. Applied Process Parameters • Pressure: 1 bar • Temperature: 50 – 60°C • Reaction time: 6 – 120 s Benefits through Process Intensification • Increase of yield of pure product by 25% • Decrease of impurity level of crude product by factor 5. Energy savings are both given by shifting the former cryogenic process to room temperature and by achieving a highly pure crude product. the phenyl boronic acid synthesis from phenyl magnesium bromide could be performed at high selectivity even at room temperature. In this way.PHENYL BORONIC ACID SYNTHESIS 12 Motivation and Results 01 Mixing sensitivity is particularly pronounced for the class of organometallic reactions. less energy consumption. less waste disposal . Often these reactions are carried out under cryogenic conditions to get acceptable yields.

i. Accordingly.56% to 0. The Grignard reaction can not only cause safety and hazardous problems at industrial scale. there are selectivity issues. Further.56% 0.4% as compared to 97. The optical purity of the micro reactor product was 98. The α-hydrogen of the starting material is unstable under basic conditions.18% Optical purity 97. while the batch impurity was 1.18% • Chirality conserved during reaction .2%.e.4% Applied Process Parameters • Pressure. the productivity and economics are increased • Minimizing back-mixing during reaction reduces impurities by factor 8.56%. Reaction time: Not disclosed Benefits through Process Intensification • With fine thermal and flow control. The micro reactor impurity was 0.18% by minimization of back-mixing. with fine thermal and flow control. Also. and consequently. Temperature. from 1. an over-alkylation to tertiary alcohol must be avoided. 01 Individual impurity Batch MRT 1. the productivity and economics of this process are increased. but there are also issues of chirality conservation. racemization may occur.(S)-2-ACETYL TETRAHYDROFURAN SYNTHESIS 13 PROCESSES Motivation and Results In the (S)-2-acetyl tetrahydrofuran (ATHF) synthesis. the individual impurity level must be less than 0. the Grignard reagent MeMgCl is very reactive and not easy to handle in large scale.9% at batch level.7% 98.

14 01 S Y N T H E S I S O F I N T E R M E D I AT E F O R QUINOLONE ANTIBIOTIC DRUG Motivation and Results Five different types of reactors. Among several types of reactors investigated. were tested for the synthesis of an intermediate to yield a quinolone antibiotic drug. the microstructured reactor was successfully applied to the synthesis of a pharmaceutical intermediate via a fast exothermic Boc protecting reaction step. Conversions as high as 96% were achieved. including conventional tube reactors and Kenics static mixers. static mixers and a microstructured reactor. including tube reactors. By using the microstructured reactor the heat of reaction was completely removed so that virtually no byproducts were produced during the reaction. with the figures of merit being maximal yield and temperature close to ambient • 97% yield . which need to be operated at 0°C or -20°C to avoid side reactions. named Gemifloxacin (FACTIVETM). Applied Process Parameters • Pressure: 1 bar • Temperature: 15°C • Reaction time: Not disclosed Benefits through Process Intensification • Micro reactor was the best out of 5 different reactor concepts. The micro reactor operation can be compared with other reactors. however. The reaction temperature was isothermally controlled at 15°C.

is going to be developed and currently under negotiation. Advanced simulations were made to solve the problems with equipartition volume flow through the multi-tube reactor and some new. The plant could be operated safely. Taking all reactants. e. The main challenge for such kind of plant is to ensure safety for all. Therefore. of notably larger size and complexity as the reactor plant.N I T R O G LY C E R I N E P R O D U C T I O N P L A N T 15 A continuous nitro glycerine pilot plant with microstructured mixer/multi-tube reactors was installed at Xi’an site in China and was operated at a production rate of 15 kg/h nitro glycerine meeting all specs. The manufactured nitro glycerine will be used as medicine for acute cardiac infarction. the micro reactor nitro glycerine plant may also encompass formulation and packaging. one of the next targets is to have it fully automated. and the test runs indeed revealed higher selectivity and purity. oleum and glycerine into account the total annual throughput is in the range of 900 cubic meters. Therefore. In a final stage. even worst operational conditions. a bunker. A rough calculation for annual throughput gives a production rate of nearly 130 metric tons per year. 01 Applied Process Parameters • Pressure: 1 bar • Temperature: 30 – 40°C • Reaction time: Some min Benefits through Process Intensification • Nitro glycerine production (15 kg NG. > 100 l/h solution) • Manufactured nitro glycerine used as medicine for acute cardiac infarction • Product quality on highest grade • Plant to operate safely and fully automated • Environment protection by advanced waste water treatment and closed water cycle PROCESSES Motivation and Results . As a second step. the necessary space for the plant in a safe environment. specific micro-macro interconnects for fluid-flow guidance were developed and integrated. all reactants must be pre-cooled before entering the microstructured mixer. Environmental pollution should be excluded by advanced waste water treatment. Also the mixer itself is actively cooled by means of an integrated heat exchanger as well as the multitubular reactor.g. a plant for downstream purification by washing and drying the nitro glycerine. fuming nitric acid. The plant is comparably small and thus. can be reduced. i. the product quality must be on highest grade.e.

at 200°C and higher being 80%).e. Applied Process Parameters • Pressure: 15 bar • Temperature: 170 – 230°C • Reaction time: 2.25 to 1. Molar ratios of bromine to m-nitrotoluene ranging from 0.T) side-chain bromination of alkylaromatics. The transformation from batch to continuous processing. the safe operation with bromine at temperatures over 170°C and the decrease of reaction time. At temperatures of about 200°C nearly complete conversion is achieved.00 were applied. were drivers for the development here. The reactants were contacted in an interdigital micro mixer followed by a capillary reactor.16 01 B R O M I N AT I O N S O F A R O M AT I C S A N D A L K Y L A R O M AT I C S Motivation and Results The bromination of meta-nitrotoluene is an example for a high-temperature. i.6 min Benefits through Process Intensification • Process simplification: Thermal process instead of photochemical one • Energy savings for the latter reasons • Solvent-free process with pure bromine • Considerable speed up of reaction by high-p. The selectivity to the target product benzyl bromide is reasonably high (at best being 85%. the two-fold brominated side-chain product. The main sideproduct formed is the nitro-substituted benzal bromide. respectively increase of space-time yields. high-pressure (high-p.T operation • Quenching of non-reacted bromine on-line and instantly after use .

since less raw material has the same effect Easy scaling out of powder synthesis. YELLOW 12 17 PROCESSES Motivation and Results By the use of microstructured mixers. since the well-defined and predictable mixing improves the preparation all the way from seed generation until particle agglomeration. lower contents of the costly raw material in the commercial dye products can now be employed which increases the profitability of the pigment manufacture. 01 Applied Process Parameters • Pressure: 1 – 2 bar • Temperature: 20°C • Reaction time: A few s Benefits through Process Intensification • • • • • Benefits through process intensification Increase of glossiness by 73% and Increase of transparency by 66% Better costing.SYNTHESIS OF AN AZO PIGMENT DYE. pigment and other particle syntheses can be improved. In this way. The particles formed in the microstructured mixer have better optical properties such as the glossiness or transparency at similar tinctorial power. Since the micro mixer made pigments have more intense colour. which otherwise may be complex . finer particles with more uniform size distribution were yielded for the commercial azo pigment Yellow 12.

for intensified gas liquid contactors kLa can reach 3 s-1. As a comparison. prepared by different preparation routes.H Y D R O G E N AT I O N O F N I T R O B E N Z E N E 18 Motivation and Results 01 The hydrogenations of nitro aromatics have high intrinsic reaction rates. After reactivation. a conversion was found slightly higher than for the sputtered one. In this way. Applied Process Parameters • Pressure: 1 – 4 bar • Temperature: 60°C • Reaction time: 5 – 20 s Benefits through Process Intensification • One of the first g-l-s processes reported in microstructured reactors • Process not benchmarked in detail to batch ones . A sputtered palladium catalyst exhibited low conversion and large deactivation of the catalyst (60°C. all intermediates except phenylhydroxylamine were identified. the longer the catalysts could be used before reactivation. Otherwise. which however cannot be exploited by conventional reactors as they are unable to cope with the large heat releases due to the large reaction enthalpies -1 (500 – 550 kJ mol ). The hydrogenations of nitro benzene over supported noble metal catalysts were investigated in a microstructured falling film micro reactor. 4 bar). depends on the catalyst loading which is related to the preparation route. The best performance of all catalysts investigated was found for an incipient-wetness palladium catalyst. decomposition of the nitro aromatics or of partially hydrogenated intermediates can occur. thus regaining complete conversion. Selectivity decreased with time. but for bubble columns and -1 agitated tanks it does not exceed 0. The corresponding selectivity was also low. As side products.2 s . A slightly better performance was obtained after an oxidation / reduction cycle. Having initially more than 90% conversion. A wide variation of preparation procedures for the palladium catalyst was tested. The larger the loading. The catalyst life-time or the four types of catalysts. initial activity was recovered. but remained still at a high level. thereby controlling reaction rate. A similar spectrum of side products as for the sputtered catalyst was given. For this reason. complete conversion was achieved and maintained for six hours. the overall mass transfer coefficient kLa was conservatively estimated (based on the film thickness in the middle of the channels) to be in the -1 range 3 – 8 s . the hydrogen supply is restricted. For nitrobenzene hydrogenation. Following a steep initial deactivation. a 75% conversion at selectivity of 80% was reached for long times on stream. selectivity approached initially 100%. For an impregnated palladium catalyst. For a UV-decomposed palladium catalyst. The four catalysts had the following sequence of life-time and activity: Wet impregnation > incipient wetness > UV-decomposition of precursors > sputtering Several reactivation routes of the used catalyst were tested such as dissolution of organic residues by dichloromethane or burning of them by heating in air. the catalyst activity stabilised at 2 – 4% conversion and at about 60% selectivity.

g. not far from the total selectivity of all the Balz-Schiemann steps to achieve the same result. it is completed within seconds or even milliseconds when using a miniature bubble column.000 Increase in productivity by factor 5 Single-step operation replaces tedious Balz-Schiemann route • Less waste generation • Less reactor investment and process simplification ..D I R E C T F L U O R I N AT I O N O F T O L U E N E W I T H E L E M E N TA L F L U O R I N E 19 PROCESSES Motivation and Results One way of process simplification is to make molecular complex compounds out of much simpler building blocks (e. with toluene. by multi-component one-pot syntheses like the Ugi reaction). but lacking of selectivity. Especially in the latter case. Since the heat release cannot be controlled with conventional reactors. this is often quoted as “dream reaction“. the process is deliberately slowed down. operating close to the kinetic limit. such routes have been realised so far from hazardous elements. easily undergoing reaction.g. Waste reduction is less since a single step synthesis is undergone. While for this reason the direct fluorination needs hours in a laboratory bubble column. showing that unselective radical paths are largely absent. e. Productivity is much higher. as demonstrated by the order of magnitude larger space-time yields. Favourable electrophilic substitution is achieved. at best directly out of the elements. 01 Applied Process Parameters • Pressure: 3 – 20 bar • Temperature: 20 – 90°C • Reaction time: 2 – 30 min Benefits through Process Intensification • • • • Reduction of reaction time up to ~ 1000 Increase in space-time yield by factor 10. Typically. The overall selectivity of this non-optimised process amounts to about 25%. One example for this is the direct fluorination starting from elemental fluorine which was performed.

water is added to the reaction mixture after the residence time module. As shown in reaction (1). Very recently also the last hydration step was executed successfully. From literature. the selectivity of the orthosulphonic acid was 17. To convert the sulphonic acid anhydride to sulphonic acid. At a mole ratio of 13/100.4% for the para-sulphonic acid. Even so.6%. Nitrogen is further added so as to dilute the system and the stream is then passed into a separator with the purpose of removing any traces of liquid. with increasing SO3/toluene mole ratio. sulphonic acid is produced here via the desired reaction step.2%. a gas stream is allowed to flow through to a microstructured reactor where it reacts with the liquid toluene. The final hydration step has not taken place. a mixed anhydride and sulphonic acid anhydride are also formed by side reactions. 1.5% for the meta-sulphonic acid and 90. the selectivity of the undesired by-products decreases while the selectivity of sulfonic acid stays nearly constant. Up to date. Evidently. the selectivity of sulfonic acid is approximately 80% while that of sulfone decreases to approximately 3% and that of the sulfonic acid anhydride to approximately 1. The isomer selectivity was also determined to be 8. the reaction has been carried out up until the residence-time module. first results are encouraging. In order to evaluate reaction conditions. was varied and the selectivity of the desired product (sulfonic acid) and of the by-products (sulfon and the anhydride mixture) was determined.S U L P H O N AT I O N O F T O L U E N E 20 Motivation and Results 01 Toluene is heated up to 40°C using a microstructured heat exchanger while at the same time liquid sulphur trioxide is heated up to 60°C in order to evaporate it.4. sulfur trioxide and toluene. Sulphone cannot be converted further but the mixed anhydride reacts in the residence time module with toluene and forms the desired product.2% and that of the para-sulphonic acid was 81. at a SO3/toluene mole ratio of 13. Thus. of the meta-sulphonic acid 1. Applied Process Parameters • Pressure: 1 bar • Temperature: 40°C • Reaction time: 5 – 15 s Benefits through Process Intensification • One of the first complex micro-flow process designs for a multi-step synthesis • Better para-isomer selectivity . the mole ratio of the two reactants. though. as shown in reaction (3). To achieve this. sulphonic acid. At the same time. Thus the improvement of the selectivity for the para-sulphonic acid can already be seen from these results. a hydration step is required (reaction (4)).3%.1% for the ortho-sulphonic acid. sul-phone (reaction (2)).

This stands for a direct route from the elements. from 6.DIRECT HYDROGEN PEROXIDE SYNTHESIS OUT OF THE ELEMENTS 21 PROCESSES Motivation and Results Several examples were reported for conducting routes in the explosive regime. The safety is not only related to avoiding thermal runaway. saving valuable raw materials. using pure hydrogen and oxygen mixtures. used at industrial scale. and usage of smaller oxygen/ hydrogen ratios. when explosive reactions are carried out in micro channels. but relates to mechanistic reasons by breaking the radical chain by enhanced wall collision in the small channels with their large specific interfaces.000 t hydrogen peroxide per year was done by UOP. basic engineering for a new site for the production in the order of about 150. and not water. Using UOP process specs. A selectivity as high as 85% at 90% conversion was achieved so far (oxygen/hydrogen ratio of 1. Otherwise. Calculations of explosion limits clearly demonstrate that there is a considerable shift. a space-time yield of 2 g hydrogen peroxide per g catalyst was achieved which exceeds literature values. is given. from 120 to 30 bar • Increase in space-time yield by 25%.5 (OPEX costs) • Safe operation at all oxygen to hydrogen ratios in the explosive envelope • Full cost analysis for world-scale plant (162kMTA) with improved OPEX costing • 78% selectivity .0 g h/gcat • Favourable decrease in oxygen to hydrogen ratio by factor ~ 4. Pilot processing and economic calculation of the production process has been performed.5 – 3). Based on microstructured mixing units. The key to a high selectivity is to have a noble-metal catalyst in a partially oxidised state. operation at only 20 bar. It could be clearly shown that improved selectivity and conversion is given at explosive oxygen/hydrogen ratios. considerably lower than for the published processes. Using this direct route to hydrogen peroxide. avoiding the circuitous Anthraquinone process.8 to 1. Among them and most prominent was the detonating-gas reaction. Peroxide testing at IMM used such a hydrogen peroxide selective catalyst placed within a mini-trickle bed reactor equipped with a micro mixer. UOP then carried out pilot-scale tests at other pressures in a fully automated explosion cell to reproduce vendor work and to study conditions and kinetics. In addition.5 to 2. the new process is realised by direct contacting of hydrogen and oxygen (without inert gas) in the presence of a heterogeneous catalyst. 01 Applied Process Parameters • Pressure: 30 bar • Temperature: 50°C • Reaction time: A few s Benefits through Process Intensification • Reduction of system pressure by factor 4. With special catalysts hydrogen peroxide. is obtained as value product. from 1. only water is formed or no reaction is achieved.

g. The sensitizer absorption.4-DIOL Motivation and Results This reaction of industrial interest utilises singlet oxygen generated by irradiation in the presence of Rose Bengal. 50 µm.4-diol was demonstrated. Sample heating is reduced and so is radical recombination.22 01 [4+2] CYCLOADDITION OF SINGLET OXYGEN T O C Y C L O P E N TA D I E N E T O M A K E C Y C L O PENTENE-1. The feasibility of safely carrying out the oxidation of cyclopentadiene by singlet oxygen to 2-cyclopentene-1.4-diol a yield of 19. unlike macro-scale photo processing.4-diol by reduction with thiourea. It is assumed that molecules in thin liquid layers face a broadly similar photon flux. For the oxidation of cyclopentadiene by singlet oxygen to 2-cyclopentene-1.5% was found. Due to the small length scales in micro reactors. high concentrations of a sensitizer may be used. An endoperoxide is formed as intermediate which is converted to 2-cyclopentene-1. Low-intensity light sources should give efficient irradiation of thin liquid layers. is not over the tolerable limit since only small optical paths are employed. In addition. oxygen-enrichment of solutions before and after micro reactor passage can be handled differently and is no longer a major safety problem. Applied Process Parameters • Pressure: 1 bar • Temperature: 0 – 15°C • Reaction time: 5 – 20 s Benefits through Process Intensification • • • • • High quantum efficiency Safe on-site conversion of endoperoxides generated Reduction of energy consumption Use of high sensitizer concentration Reduced thermal overshooting of sample due to lowering light intensity . The explosive intermediate endoperoxide was generated and without isolation used on-site for a subsequent hydration reaction. As these materials typically have high costs. e. despite the large molar extinction coefficient. recycle loops with low inventory can be employed to consume only a low overall amount of sensitizer.

By using an iron plate.3 mol/(l h). hence having a selectivity which is higher by about a factor of 2. Here.C H A I N P H O T O C H L O R I N AT I O N O F T O L U E N E . Control experiments in a batch reactor at 30 min reaction time resulted in a space-time yield of only 1.D I . this may lead to the use of low-intensity light sources and considerably decrease the energy consumption for a photolytic process. respectively yields from 24% to 54%. Illuminated thin liquid layers should have much higher photon efficiency (quantum yield) than given for conventional processsing. Conversions from 30% to 81% at selectivities from 79% to 67%. In turn. which can be kept when increasing throughput by numbering-up.8 – 13.2 . 81% instead of 65% for batch Increased space-time yield by two orders of magnitude. Control experiments in a batch reactor (30 ml reaction volume) at 30 min reaction time resulted in a conversion of 65% at 45% selectivity. hence are by orders of magnitude smaller. 4 . spacetime yields up to 346 mol/(l h) were achieved in the Falling Film Micro Reactor. were found when using a Falling Film Micro Reactor (4.7 s.S I D E .I S O C YA N AT E 23 Side-chain photochlorination of toluene isocyanates yield important industrial intermediates for polyurethane synthesis. The motivation for micro channel processing stems mainly from enhancing the performance of the photo process. Due to the planar layer structure of most micro reactors a uniform illumination is yielded in addition. only a larger one. 79% instead of 45% for batch Increased conversion. the individual reaction units are assembled in parallel again on a plane. one of the most important classes of polymers. By using a nickel plate. 130°C). 01 Applied Process Parameters • Pressure: 1 bar • Temperature: 130°C • Reaction time: 5 – 15 s Benefits through Process Intensification • • • • High quantum efficiency Increased selectivity. 401 mol/(l h) instead of 1.3 mol/(l h) • Reduction of energy consumption • Reduced thermal overshooting of sample due to lowering light intensity PROCESSES Motivation and Results . space-time yields up to 401 mol/(l h) were achieved in the Falling Film Micro Reactor.

PLANTS 24 02 .

CONTENTS > plants made by imm 25 Plants Organic Synthesis Plant OSBP Impinging-Jet Microreactor Plant for Precipitation Reactions IJMP Cream and Emulsification Plant CSBP Modular Microreactor Systems for Production Plants Falling Film Micro Reactor Plant FFMR-BSP Gas Phase Reactor Test Plant Fuel Processor Demonstration Plant Mixer-Settler Continuous Work-Up Plant CWUP 26 28 30 32 34 36 38 40 02 PLANTS .

and epoxidations in such micro mixer/tube reactor bench-scale units. the general bench-scale unit concept can be modified towards more complex design. a micro mixer. a 5/2-way valve. It comprises two pre-heating loops (as option: microstructured heat exchangers). The concept is amenable to supercritical processing as well. utilizing innovative micro reactor components in connection with well-proven conventional small-fluidic equipment.ORGANIC SYNTHESIS PLANT O SB P 26 02 OSBP for 2-step reaction Principle In micro reactor literature. and 4 delay loops of different length collected to one outlet which allows to change the residence time for a given set of parameters during the reaction by simply switching the valve. the most frequently used approach for organic synthesis is the micro mixer/tube reactor. The organic synthesis bench-scale unit relies on this concept and has in addition control and measuring functions. IMM has gained huge experience with carrying out organic reactions e. ethoxy silylations. It is based on the reliable hybrid concept of IMM. metal-organic syntheses. On demand.g. OSBP for single-step reaction (top view) OSBP for single-step reaction (inside view) . As a result this unit concept was developed and tested to yield the bench-scale unit actually offered now.

foams).2-R600/12 4 changeable delay loops have a different length of approx.e. 20% and 100% (the absolute lengths will be adjusted to the applied mixer to yield reasonable residence times) L0.5 for mixer SIMM-V2 2. it might be differentiated and/or extended where needed.1 Further Applications Based on the IMM knowledge on general demands for a chemical synthesis plant. 1%.05 – 2. switchable online via a 5/2-way valve • 1 tube-in-tube heat exchanger (as option: Microstructured heat exchanger) at the outlet • All above devices mounted on a metal plate • Assembled set-up fits into a heating bath Options • • • • Temperature and pressure measurement unit Pumping units Process control unit. this basic set-up was designed. 5%.5 – 30 for mixer CPMM-V1. even catalyst slurries might be processed.g. for gas/liquid or liquid/liquid mixing homogenuously or dispersing (emulsions. programmed in LabView Other materials on request Pilot-scale plant for nitro glycerine production PLANTS . Though it should be directly applicable for many typical (organic) syntheses i. If the standard version is not sufficient. 02 Leakage Class Specification of the Basic System • 2 pre-heating loops (as option: Microstructured heat exchangers) • 1 SIMM-V2-mixer or 1 CPMM-mixer with housing material stainless steel • 4 delay loops with different residence times. e.27 Typical flow charts for Organic Synthesis Plant Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (s) -50 – 180 30 for stainless steel 3 for PTFE 0. Insofar. this set-up represents a versatile tool to directly enter into micro chemical process engineering. for multi-step processing.

Another option is to use the Separation Layer Interdigital Micromixer SLIMM instead of IJMM to carry out precipitations. enabling a fast and efficient temperature control. the mixer. . The position of the IJMM in the mixing chamber can be adjusted in the vertical direction which allows best fitting connection of an outleaving (reaction) tube downstream. The delay loop was removed and the remaining blocking sensitive part. substituted by the simplest nonfouling component for continuous mixing-processing. in case the mixing section tends to spraying causing contamination of the mixing chamber.IMPINGING-JET MICROREACTOR PLANT F O R P R E C I P I TAT I O N R E A C T I O N S I J M P 28 Main part of the IJMP with mixing chamber and heat exchangers 02 The balance system for mass flow control combined with gear pumps as well as the process control system is not shown here Principle The Impinping-Jet Microreactor Plant IJMP is the logical advancement of the Organic Synthesis Bench-Scale Plant OSBP for precipitation reactions which cause blockage by main or side products and cannot be processed in our standard OSBP. Additional (inert) gas flushing is integrated. Educt streams are tempered via two microstructured heat exchangers HX204 before entering the mixer. the Impinging-Jet Micromixer IJMM. The overall pressure and temperature stability is mainly limited by the windows and gasket of the mixing chamber.

1. typically for IJMM: 350 µm diameter Other materials like Hastelloy.g. nitrogen Flow chart of the IJMP including balance system 02 Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Standard material Standard mixing channels (µm) Options Impinging-Jet Microreactor Plant IJMP main part depicted left: approx.4 – 3.4571 Glass depending on used mixer. W 50 cm x H 80 cm x D 30 cm 1/4˝ / 1/4˝ Housing.g.0 l/h watery flow The LabView-based process control system for the IJMP PLANTS . overnight experiments) easily compiled with the integrated program editor. for IJMM-350 e. The collected data are as ASCII-files easily importable e.29 nitrogen nitrogen thermostat The mixing chamber with height-adjustable IJMM inside The process control system of the Impinging-Jet Microreactor Plant IJMP allows for both educt flows the exact mass flow regulation with gear pumps and balances as well as measuring and controlling their inlet temperature into the mixing chamber. Monell or Titan on request Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) -200 °C to + 250 °C @ 1 bar 0 .g. Besides complete data acquisition including system pressure this LabView-based system can run given programs (e. mixer: 1. into Excel for further use.40 bar @ 25 °C depending on used mixer.

The 4 solid components can be fed via temperature-controlled heated funnels into tempered flask whereof being pumped. Respectively. The general bench-scale unit concept can be modified towards more complex design. Besides. The CSBP-Demonstrator is based on the reliable hybrid concept of IMM. The liquids are heated up with simple heating loops. Respectively. Cream Plant positioned on a holder for easy maintenance. to 1 – 15 l/h depending on type and 140°C are used to convey up to 4 liquids and 4 solids being molten in the comprised heat bath into a mixer array as the 8 Component Caterpillar Micromixer (8CCPM) directly yielding the hot emulsion. cleaning and device exchange . a versatile tool concept is offered herewith enabling even a fast change of cream recipes within less than a minute.C R E A M A N D E M U L S I F I C AT I O N P L A N T CSBP 30 02 Cream Synthesis Bench-Scale Plant for 5 different chemicals Principle Generating emulsions is typically a process where all materials are being balanced or measured. Further taking the advantage of small hold-ups despite the pilot-scale productivity. creams. small gear ring pumps for max. bath-fed or electrically driven heat exchangers depending on total flow rate need. more narrow droplet size distribution can be achieved within a shorter time as conventional techniques as only passing once through within milliseconds yields the result. enabling a full continuous processing even in case of production need. lotions within short time can be produced as samples or in larger amounts. Micromixers insofar proved in literature to reduce energy input by factor 10. utilizing innovative microreactor components in connection with wellproven conventional small-fluidic equipment. The concept is amenable to unusual processing as well. placed in a flask or vessel and then vigorously stirred or homogenised with high energy consumption. a multitude of different pastes.

8CCPM Special StarLaminator10. 4CCPM. of PMMA. to mix 3 components at once.5 – 60 L0. 5-80 l/h PLANTS .31 Cream Synthesis Plant or 4 solid and 4 liquid educts and continous use Cream Synthesis Plant for 1 solid and 1 liquid educt and continous use Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Leakage Class 20 – 140 20 for stainless steel 3 for PTFE 2. ca. programmed in LabView • Other materials on request Array of 3 CPMM to mix 4 components nearly at once.1 Specification of the Basic System • Up to 8 electrical pre-heating storage tanks • Eightfold-CPMM-mixer with housing material stainless steel or PTFE • Micro annular gear pumps • All above devices mounted on a metal plate • Assembled set-up fits into a heating bath 02 Options • Temperature and pressure measurement unit • Process control unit. 3-60 l/h Seven CPMM structures to mix 8 components. ca.

32 02

MODULAR MICROREACTOR SYSTEMS FOR PRODUCTION PLANTS

Exemplary basic unit of a Modular Microreactor System consisting of distributor, three reaction modules and collector

Principle
Recent R&D efforts led to the development and realisation of modular microreactor based systems for production plants. The concept was developed to execute reactions which benefit from the outstanding properties of microstructured devices, especially concerning heat transfer and mixing. Mainly for fine and specialty chemistry reactions the size of the modules allows scaling up processes up to the production scale. The basic unit thereby consists of newly developed, flangeable modules made of stainless steel. The modules are manufactured of vacuum brazed microstructured plate stacks which can withstand higher pressures. Each basic unit is composed of a distributor module which spreads the feed stream to all channels of the stack, a variable number of reaction modules with integrated heat exchanger function and a subsequent collector module. Each module can be tempered on its own temperature level if required. This basic unit can then be extended to an overall modular system following the multiscale approach, e.g. the microstructured modules can be followed by a mini-scale multitube reactor which exhibits sufficient heat transfer properties to complete the reaction. The basic units can furthermore be supplemented with microstructured heat exchangers, e.g. of the HX or WT series, and micromixers, e.g. of the CPMM-V1.2 or of the StarLam series.

Configuration with heat exchangers (HX-series), tempered caterpillar mixer (CPMM-V1.2-HEX), distributor, reaction module and collector

33
reactant 1 heat transfer medium micro heat exchanger heat transfer heat transfer heat transfer heat transfer heat transfer medium medium medium medium medium heat transfer medium coolant

micromixer heat transfer medium reactant 2 flangeable basic unit micro heat exchanger distributor microstructured microstructured microstructured collector module reaction module reaction module reaction module module

R(n+1) conventional micro heat (multi) tube exchanger reaction module

product

Flow chart of a typical configuration of a modular microreactor system for production plants

Operating Conditions (exemplary)
Temperature (°C) Pressure stability (bar) Flowrate (l/h) + 200 °C @ 50 bar (higher temperature on request) 50 bar @ 200 °C (higher pressure on request) depending on the reaction, module system e.g. 1 to 10 (more upon request)
4.0 1.0 0.8

02

Bo = 90
F(Θ)

3.5 3.0 2.5

F (Θ)

2.0 1.5
E(Θ)

0.4 0.2 0.0 0.0 0.5 1.0 1.5 2.0

1.0 0.5 0.0

Θ=t/τ[-]

Normalised residence time distribution function for a basic unit with 2 reaction modules at 3 l/h flowrate

E(Θ)

0.6

Multi-tube module

Vacuum brazed reaction module with open reaction channels

Distributor/collector module

Basic unit and subsequent multi-tube module

PLANTS

FA L L I N G F I L M M I C R O R E A C T O R P L A N T
FFMR-BSP

34 02

Falling Film Micro Reactor Plant

Principle
The Falling Film Microreactor BenchScale Plant comprises besides the Falling Film Microreactor, a mass flow controller for the gas flow, a cryostat, a supply- and a withdraw-pump for the liquid flow. The precise assortment of the peripheral equipment components basically depends on the different chemical reactions which the customer wants to perform. This means, the general bench-scale unit concept can be modified towards more complex design. Operation in the Falling Film Microreactor device can be performed up to 300°C at a pressure of max. 10 bar by using the standard version (upper housing with inspection glass) or max. 20 bar with the special upper housing without window. The suitable liquid flow rates depend on the channel geometry of the corresponding reaction plate and the property of the reactant (e.g. viscosity). For example, the max. liquid flow rate by using isopropanol and a channel size of 1200 µm x 600 µm is 1.5 l/h.

35

02
Flow charts of a Falling Film Microreactor Plant

Technical Data
Name
Order number Connectors (Inlet/Outlet) Material of FFMR

Specification of the Basic System
Falling Film Microreactor Plant
FFMR-BSP 1/4˝ / 1/4˝ 1.4571 for housing and reaction plate copper for cooling plate borofloat glass for inspection 300 x 100 (64 channels) 600 x 200 (32 channels) 1200 x 400 (16 channels) Other materials like Hastelloy, Monell or Titan on request

• • • • • •

Falling Film Microreactor (FFMR) Flow controller for reaction gas Supply pump for liquid reactant Withdraw pump for product Low temperature thermostat; cryostat respectively Connecting tubes

Standard mixing channels of FFMR (µm) Options

Options
• Mass flow controllers • Temperature and pressure measurement unit • Process control system

Operating Conditions
Temperature (°C) Pressure stability (bar) Flowrate (l/h) 180 (option 300) 10 (without Borofloat glass: 20) 0.05 for channel geometry 300 µm 0.6 for channel geometry 600 µm 1.5 for channel geometry 1200 µm 0.8 – 20 25 – 100 L0.01

Residence time (s) Liquid film thickness (µm) Leakage Class

PLANTS

GAS PHASE REACTOR TEST PLANT

36 02

Bench-scale catalyst evaluation unit for fossil and alcohol fuel processing

Principle
This bench-scale unit serves for investigations in heterogeneous catalysis with respect to fossil fuel and alcohol fuel processing, e.g. concerning the determination of the activity/selectivity and stability of catalysts, as well as process optimization studies of this class of gas-phase reactions by fast serial variation of process parameters such as temperature, pressure, gas flow velocity, and gas composition. The bench-scale unit comprises commercial mass-flow controllers for control of the gas feed, flame arresters to stop flame propagation, and a microstructured evaporator fed by a liquid tank, which produces steam or organic vapours (optional), all mounted on a metal board. Steam and gas feed are mixed and enter a micro device composed of two laser-welded microstructured platelets having one inlet and outlet tube, also welded to the two-platelet stack. Operation in the micro device can be performed up to 900°C at a pressure of 10 bars, using external resistance heating. The catalyst is usually introduced into the micro channels prior to interconnection, e.g. by the wash-coat route and subsequent impregnation. By laser-welding the thermal treatment is spatially confined so that the catalyst is not destroyed during interconnection. The welded micro device can be cut after use so that analytical studies can be carried out with the catalyst layers that were exposed to the reactants during time on stream. Besides using the two-platelet stack micro reactor, any other IMM or othersource micro reactor can be integrated into this bench-scale unit. In this case, please contact IMM prior to the construction of the bench-scale unit so that the required modifications can be arranged.

nitrogen. hydrocarbons. Here. besides general information. IMM has in particular gained experience in building bench-scale units for all kind of fuel processing unit operations and in operating respective micro devices. The performance of the reforming bench-scale unit was demonstrated in detail for propane steam-reforming. carbon dioxide. preferential oxidation of carbon monoxide. manometers. detailed documentation on experiences gained with operation of this bench-scale unit. The bench-scale unit was in detail investigated not only for numerous steam reforming and partial oxidation reactions of alcohol and hydrocarbon fuels. and for the methanation of carbon monoxide. preferential oxidation and methanation. a process parameter monitoring program based on the LabView software can be supplied that allows automatic acquisition of temperature and pressure data.37 In conjunction with bench-scale unit construction. Specification of the Basic System • Mass flow controllers for hydrogen. flame arresters • Temperature controllers • Pressure controller (optional) • All above devices mounted on a metal frame • Available IMM-reactors for testing catalyst performance 02 Options • Additional mass-flow controllers (e. carbon monoxide. In case of further questions and desires. An extension of the use of benchscale units for other types of heterogeneous catalytic studies is principally possible and requires in most cases only minor modifications of the bench-scale unit construction. oxygen) • Additional periphery heating (pipes) • Additional liquid storage tanks (required for long term operation) • Additional temperature sensors PLANTS . an IMM contact person can be consulted by mail or phone. water-gas shift at high and low temperature. Exemplarily. IMM services include provision of a manual which contains. for air. operational modes are given so facilitating the first experimental steps when starting bench-scale unit operation.g. methanol and ethanol steam-reforming. this requires the coating of another catalyst. information on the exact process desired is required from the customer and a special offer will be prepared by IMM. Besides constructional changes in the set-up. By special request. partial oxidation of propane. air and water (choice of selection optional) • Stainless steel vessels for water and organic liquids • Evaporator • Valves. but also for CO clean-up such as water-gas shift.

g. The unit is designed for tests of startup. which may be a microstructured device or a conventional reactor type (metallic monolith or fixed bed reactor). Operation in the microstructured reactors may be performed up to 900°C at pressures of up to 5 bars. and gas composition are possible. The catalyst is usually introduced into the micro channels prior to the sealing procedure (normally laser-welding). which is fed by a liquid tank. Fast serial variation of process parameters such as temperature. by the wash-coat route and subsequent impregnation. By laser-welding the thermal treatment is spatially confined so that the catalyst is not destroyed during interconnection. Steam and gas feed are mixed and enter the reactor. steady-state and transient reactor behaviour and for long-term tests. flame arrestors to stop flame propagation. By-pass lines are introduced. water-gas shift and preferential oxidation reactors) are integrated into the unit. The evaporator. pressure. reforming. The test bench comprises commercial mass-flow controllers for control of the gas feed. gas flow velocity. Process optimization studies may be performed. produces steam or organic vapour. e.g. for maximum temperature of 500°C at pressures up to 100 bars.F U E L P R O C E S S O R D E M O N S T R AT I O N P L A N T 38 02 Test bench for single reactors and multiple reactor arrangements Principle This test bench serves for investigations in reactor performance testing with focus on fuel processing applications such as fossil and alcohol fuel reforming and catalytic CO-clean-up. using either external resistance heating or integrated catalytic burners. Also internally cooled reactors (heat exchangers) and combinations of these reactor types may be tested in the test bench. All devices are mounted onto a metallic frame. if serial combinations of several reactors (e. thus allowing for switching off the individual reactors under test. and various evaporator types (evaporation power between 10 s of watts up to kilowatts). .

carbon dioxide. (Nl/min) Max. an IMM contact person can be consulted by mail or phone. flame arresters • All above devices mounted on a metal plate • Available Reactors Options • • • • Additional massflow controllers (e. flowrate (gas) approx. information on the exact process desired is required from the customer and a special offer will be prepared by IMM. evaporator temperature (°C) 10 20 about 500 about 5000 200 02 Specification of the Basic System • Mass flow controllers for hydrogen. besides general information. manometers. for water-gas shift and for the preferential oxidation of carbon monoxide. Here. all up to the 10 kW range (lower heating value of the hydrogen produced/processed). IMM services include provision of a manual which contains. flowrate (liquid) approx. nitrogen. a process parameter monitoring program based on the LabView software can be supplied that allows automatic data acquisition of temperature and pressure. air and water (choice of selection optional) • Stainless steel tanks for water and organic liquids • Evaporators • Temperature controllers • Pressure controller (optional) • Valves. Exemplarily. (g/h) Max. for air. carbon monoxide. In conjunction with test bench construction. however it may – on special customer request – be modified to allow for investigations of other types of heterogeneous gas-phase reactions.g.39 Please contact IMM prior to the construction of the test bench so that the modifications required can be arranged. reservoir of water or organic liquid for one continious run (l) Max. In case of further questions and requests. pressure (bar) Max. Operating Conditions Max. By special request. operational modes are given so facilitating the first experimental steps when starting bench-scale unit operation. The bench-scale unit was in detail investigated for steamreforming and autothermal reforming of fossil fuels. hydrocarbons. detailed documentation on experiences gained with operation of this bench-scale unit. oxygen) Additional periphery heatings Additional liquid storage tanks Additional temperature and pressure sensors PLANTS .

the same procedure is repeated. the organic phase is contacted with an aqueous washing phase via a Caterpillar Micromixer and separated subsequently in a second settler. CWUP. A sensor is measuring the pH-value of the waste aqueous phase of the second washing step and thereby monitoring washing success of the organic phase. One settler-unit is composed of a glass tube. Operating Conditions Total flow rate Operating pressure Temperature up to 150 ml/min atmospheric up to 80°C Specification of the Basic System • Three settlers (glass tube and siphons) • Two Caterpillar Micromixers • Two + two gear pumps • Four filling level sensors • Filling level-flow rate controller • Lab hood-like housing with transparent doors . The flow of the organic phase in the two washing steps is automatically regulated by gear pumps based on the measurement by special filling level sensors. This plant consists of a combination of mixers and settlers to cover the functionality of inital phase separation and of two washing steps with water for the organic phase. In the next step. attached with special fittings on both ends. The water level in a settler is adjusted by a flexible tube siphon.g. Based on this the flow rate of the aqueous phase is adjusted automatically. separation of an incoming biphasic system and subsequent 2-step washing with micromixer-settler-siphon system. A biphasic reaction mixture (e. gravity driven mini-settler. IMM has developed a matching Continuous Work-Up Plant.MIXER-SETTLER CONTINUOUS WORK-UP PLANT CWUP 40 Principle 02 Against the background of a twophase liquid/liquid reaction performed in a microreactor based set-up. organic phase and aqueous phase) is separated by an initial. In the third step.

settler pH-sensor Main components of the CWUP PLANTS .41 distilled water distilled water inlet for biphasic reaction mixture product optional inlet for homogeneous reaction mixture aqueous waste aqueous waste aqueous waste 02 Typical process flow chart for the Mixer-Settler Continuous Work-Up Plant 1. mixer 2. settler pump 2x sensor mixer 3. settler pump 2x sensor 3x siphon system Detail view on settling process (above). overview on plant components for a double washing unit (left).

COMPONENTS 42 03 .

-R2400 46 Star Laminator StarLam group class -30. -R600. -300. -R300.2 group class-R150. -3000. -R1200. SIMHEX.CONTENTS > components made by imm 43 Components Liquid/Liquid and Gas/Liquid Mixers or Reactors Overview Applications Mixing Principles 44 45 Caterpillar Split-Recombine Micromixer CPMM-V1. -30000 Slit Interdigital Micromixer SIMM group class SIMM-V2. SSIMM Liquid/Liquid Microreactor LLMR-MIX SuperFocus Interdigital Micromixer SFIMM-V2 Impinging-Jet Micromixer IJMM 50 54 58 60 62 Special Gas Liquid Reactors Falling Film Microreactor FFMR 64 Gas Phase Reactors Gas Phase Microreactor GPMR Gas Phase Microreactor with Mixer and Internal Heating/Cooling GPMR-Mix Catalyst Micro Burner Reactor CMBR Catalyst Testing Microreactor CTMR 68 70 72 74 Heat Exchangers Laser-welded Micro Heat Exchanger WT-series Brazed Micro Heat Exchangers HX-series Tube Heat Transfer Micro Device THTMD Laboratory Evaporator 76 78 80 82 03 COMPONENTS . HPIMM.

CPMM. CPMM and StarLam • • • • HPIMM Reactions at high pressure • Alkylation of aromatics with supercritical CO2 • Direct H2O2 synthesis • Mixing of silicon oil and water • Mixing of diesel and water • Addition reaction with liquid ethylene oxide synthesis • [2+2] Diels Alder photooxygenation of olefines • Photochemical chlorination of alkylaromatics • Hydrogenation of C=C double bonds Dispersion and emulsion formation Mixing of liquids differing in viscosity Photochemical reactions SIMM. + solid. IJMM. . + solid. MBC. StarLam. SSIMM. SFIMM-V2 Application Examples • • • • • • • • • • • • • • • • • Grignard reaction Kolbe-Schmitt synthesis Sonogashira couplings Formation of polyacrylates Formation of blockcopolymers Phenyl boronic acid synthesis Benzal chloride hydrolysis Dendrimer synthesis Michael reaction Nitro glycerine synthesis Bromation of alkylaromatics with elemental bromine Synthesis of (S)-2-Acetyl-tetrahydrofuran (antibiotic drug intermediate) Synthesis of an intermediate for Gemifloxacin (FACTIVETM) Isomerisation of allyl alcohols H-transfer reduction of citraconic acid ester Aromatic nitrations Aliphatic nitrations Direct fluorination of toluene Sulfonation of aromatics Hydrogenation of nitrobenzene Hydrogenation of cinnamic acid esters Special gas/liquid reactions FFMR.Steroids (disp. CPMM SSIMM • Bipyridine (precipitation) • Starch (dispersion + solidification) • Azopigment Yellow 12 (precipitation) • Azopigment Clariant (precipitation) • Polystyrene (dispersion + solidification) • Model prot. StarLam Produced with window: SFIMM-V2. PSA-in-LGPA (disp. MBR Reactions with catalytic suspensions Particle and pigment synthesis Inorganic particles CPMM SSIMM. IJMM.) • Nanocomp. CPMM HPIMM.) • Stearate/phenofibrate (self-assembly) • Amphiphilic vesicles (self-assembly) • Block copolymer vesicles (self-as. SLIMM • • • • Titanates (precipitation) CaCO3 (precip. CPMM SSIMM. StarLam SFIMM-V2. Pt/C (reduction) {N-doped TiO2 (hydrothermal process)} Organic particles Pigments Polymer particles Microcapsules Amphiphilic particles SSIMM.OVERVIEW 44 03 > applications Applications Liquid/liquid and gas/liquid reactions Type of Standard Mixers and Reactors SIMM. CPMM. SIMM. FFMR.) . SLIMM SSIMM. CPMM. CPMM. SIMM.) Au (GNP).

1.1l/h .0l/h) COMPONENTS .> mixing principles by imm 45 Constructional principles Recirculation Split-recombine Multi-lamination Jet collision Bas-relief Ramp-up/down Interdigital channel array Interdigital disk array Tilted jets Product classes Slit Triangular Caterpillar CPMM Standard SSIMM Super-Focus (V2) SFIMM Star Laminator StarLam Impinging-jet IJMM Version 2 SIMM-V 2 Heat Exchanger SIMHEX Products High-Pressure HPIMM 03 CPMM R150/12 (0.

The higher flowrates enable production scales of a few up to about 100 tons per year with all the advantages of our micro mixers. availability of different housing materials and safety gains. 2 G R O U P C L A S S -R 1 5 0 . in a split-and-recombine fashion. .R300.V 1 . e.or l/ldispersing. At very low Re numbers. providing highest performance for l/l-mixing as well as for g/l.g. . the mixing mechanism may change and a near-multilamellae type flow pattern arises which uses diffusion mixing in thin layers. . for viscous flows at low flow rates. As they consist of a structured single channel.R2400 46 03 CPMM group class Principle The Caterpillar Micromixers are particularly suitable for applications where fast mixing at higher throughput is desired.R1200. .C AT E R P I L L A R M I C R O M I X E R CP M M . these devices may also be used successfully if precipitation occurs during the reaction or if fine slurries shall be processed. The Caterpillar Micromixer has internal bas-relief structures which induce recirculation flows transverse to the flow direction which result in efficient chaotic mixing. such as mixing quality.R600. Simulated “real“ flow profiles at high flow rates in Caterpillar Micromixers .

Development here has been accompanied by modelling works to learn and understand fluidic behaviour. from left: R150. They combine the unique properties of the Caterpillar Micromixers and their less clogging-sensitive structures with the aim to process higher throughputs. R600. R1200. COMPONENTS . and fluid equidistribution when numbering up. R2400 03 Caterpillar Micromixer Arrays & Stacks Research Topics at IMM In the context of IMM´s efforts in the continuous advancement of our components for production purposes two prototypes of numbered-up versions of the CPMM-R600/12 mixer have been realized recently.47 Single Caterpillar Micromixers CPMM sizes. mixing. In the STACK-10x-CPMM-R600/12 ten caterpillar structures on plates are stacked and brazed together allowing high pressure applications. This mixer has been successfully tested for a dispersion step with a throughput of up to 600 kg/h. R300. In the ARRAY-16x-CPMM-R600/12 the caterpillar structures are arranged in a different manner requiring also a new feed distribution system but decreasing pressure drop.

PTFE or other plastics on request Operating Conditions Order number Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (µl) Max Viscosity (mPas) Leakage Class CPMM-V1.001 CPMM-V1.01 CPMM-V1. eddies can be prevented in this region and therefore fouling is diminished or even prevented. .32 – 72 300 100 < L0.2R300 Caterpillar Micromixer R600 CPMM-V1.2R2400-so -40 – 220 30 15 – 250 4.V 1 .4435 51 x 45 x 30 1/8˝ / 1/8˝ 1200 x 1200 1.2R2400 Caterpillar Micromixer R300straight outlet CPMM-V1.4435 51 x 45 x 20 1/16˝ / 1/16˝ 300 x 300 1.4435 Heat exchanger function is possible.01 CPMM-V1.6 – 60 250 100 < L0.4435 70 x 45 x 30 1/4˝ / 1/4˝ 2400 x 2400 1.g.2R600-so -40 – 220 30 2 – 40 2. Technical Data Name Caterpillar Micromixer R300 CPMM-V1.001 CPMM-V1.4435 60 x 45 x 30 1/8˝ / 1/8˝ 600 x 600 1. Due to the construction principle only 30 bar system pressure can be applied. 2 G R O U P C L A S S -R 1 5 0 .2R2400 -40 – 220 100 15 – 250 3.2R300-so Caterpillar Micromixer R600straight outlet CPMM-V1.5 – 4 5.4 – 108 15 100 < L0.05 – 81 90 100 < L0.2R1200-so Caterpillar Micromixer R2400straight outlet CPMM-V1.01 .2R1200 Caterpillar Micromixer R2400 CPMM-V1. CPMM with a straight outlet made of PP As the emerging reaction fluid is not forced to leave the mixer via the 90° elbow flow configuration and in addition the rectan-gular mixer geometry is smoothly adapted to the round shape outlet tube. These mixers consist of a single structured mixer channel with an adapted outlet.2 78 100 < L0.C AT E R P I L L A R M I C R O M I X E R CP M M .001 CPMM-V1.2R2400-so Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Standard material Options all: bas-relief.7 – 54 30 100 < L0.4435 79 x 45 x 30 1/4˝ / 3/8˝ 2400 x 2400 1.01 CPMM-V1.2R600 Caterpillar Micromixer R1200 CPMM-V1.2R600 -40 – 220 100 2 – 40 2.2R1200-so -40 – 220 30 4 – 80 4.2R300-so -40 – 220 30 0.2R600-so Caterpillar Micromixer R1200straight outlet CPMM-V1.25 – 45 25 100 < L0. Monell. .R300.R1200.001 CPMM-V1. recirculation flow (chaotic) 60 x 45 x 20 1/16˝ / 1/8˝ 300 x 300 1.4435 51 x 45 x 30 1/8˝ / 1/8˝ 600 x 600 1. nonetheless enabling production of slurries containing up to some 100 kg per year of fine powders. PTFE.15 – 70. .R600. .4435 60 x 45 x 30 1/8˝ / 1/4˝ 1200 x 1200 1.2R300 -40 – 220 100 0.2R1200 -40 – 220 100 4 – 80 3.R2400 48 Single Caterpillar Micromixers with straight outlet 03 CPMM with a straight outlet The Caterpillar Micromixers with straight outlet are particularly suitable for applications where fast mixing is desired though precipitation occurs during the reaction or if fine slurries shall be processed.5 – 4 3.6 – 72 10 100 < L0. Titan. This effect can further be promoted by the application of suitable special housing materials as e. other materials like Hastelloy.

heat exchanger delay loop) thus extending the application range to more exothermic reaction or application of molten materials.49 Single Caterpillar Micromixers with Heat Exchanger Function CPMM-R2400/10-HEX-ss-wt assembled (left) and disassembled (right) Multiple Caterpillar Micromixers 03 8CCPM-R1200/8.7-PMMA For special mixing or dispersion applications. turning the two heat exchange passages into service free units and enabling even for the gasketed center mixing section high system pressures and temperatures. typically brazed. With such arrays e. the Caterpillar Micromixers with heat ex-changer function are. notwithstanding the above photo of a gasketed one. . where no residence time/delay loop is needed.2-R1200/8. 4CCPM-R952/8. this heat exchange version may also be combined with the straight outlet and its housing can be produced in nearby any material desired. Of course.g. multi-component creams can easily be generated.g. Meanwhile.1-ss-hplc COMPONENTS As an additional feature the Caterpillar Micromixers may be offered with an integrated heat exchange function particularly suitable for applications where pre-heating/ -cooling of the mixture is desired prior to the subsequent reactor (by means of e. the Caterpillar Micromixers may be combined to arrays thus enabling a nearby simultaneous mixing of more than 2 fluids at once.

the StarLam series expands the range of operation from pilot-scale microstructured mixers of the Caterpillar series into production applications. . A classification of the mixing efficiency versus the power input confirms this continuity as well. Therefore. a 3 throughput of about 3 m /h at a pressure loss of 0.7 bar was determined for watery sys-tems. The apparatuses yield at higher flow rates a mixing efficiency which compares the high performance of today’s low-capacity (l/h) micromixers. In this way. . . -300. They create an alternate. a finely-dispersed injection of two fluid streams is achieved.g. continuity from the “real” micromixers over the herein described high-throughput tools to conventionally manufactured static mixers with even higher flow rates is given.3000. The novel Star Laminators are largecapacity microstructured mixers reaching volume flows up to the m3/h domain.30000 50 03 The StarLam family Principle The Star Laminators are the first real production tools of IMM for mixing purposes.S TA R L A M I N AT O R STAR L A M G ROUP C LA S S -3 0 . In this way. interdigital-type feeding array which is generated by stacking thin foils with star-like through-holes. The foil stack is inserted into the recess of a housing where it is tightened by applying compression. For the Star Laminator StarLam 3000 e.

4401 Other materials like Hastelloy.001 03 COMPONENTS . Other materials like Hastelloy.4571 Foils: 1.4571 Foils: 1. Monell or Titan on request Monell or Titan on request Monell or Titan on request Monell or Titan on request Operating Conditions Order number Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (ml) Max Viscosity (mPas) Leakage Class StarLam 30000 StarLam 3000 StarLam 300 StarLam 30 f o r F KM: .4571 Foils: 1. Other materials like Hastelloy.001 100 12 – 150 24 – 840 2.4401 Star Laminator 300 StarLam 300 Multi-Lamination 40 x 40 x 64 8 mm/10 mm 100 Body: 1.001 100 80 – 1000 1.8 10000 < L0. f o r FFKM: -20 to +315.2 0 t o + 2 2 0 .4401 Star Laminator 30 StarLam 30 Multi-Lamination 40 x 40 x 64 8 mm/10 mm 50 Body: 1.51 StarLam 30000 StarLam 3000 StarLam 300 StarLam 30 Technical Data Name Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Star Laminator 30000 StarLam 30000 Multi-Lamination 220 x 425 x 480 DN 80/DN 50 Star Laminator 3000 StarLam 3000 Multi-Lamination 95 x 95 x 150 DN 15/DN 25 250 Body: 1. for graphite: -100 to +500 (old S tarLam versions ) 100 5000 – 30000 180-1100 1500 (623 mix section) 10000 < L0.4401 Standard mixing channels (µm) 250 Standard material Options Body: 1.4571 Foils: 1. Other materials like Hastelloy.7 – 220 5 10000 < L0.001 100 600 – 8000 72 – 960 160 10000 < L0.

p.30000 52 03 A B A Mixing channel A B The feed plates of the StarLam series (here StarLam 3000). as simulations and reaction-type mixing experiments confirm. . e.e. the feeding of the educts can also be adjusted by the mixing foil thickness as to enable mixing ratios of up to 1:100. at the same pressure drop an equal mixing efficiency is yielded independent which microstructured mixer is chosen as to be expected for a turbulent mixing scheme. StarLam 3000 foils during assembly on the assembly rods StarLam 3000 StarLam 30 StarLam 30/300 disassembled StarLam 300 Feed plates of StarLam 30. Finally. Due to the geometry of the StarLam a multicomponent mixing can be easily realised by re-allocating the 12 single holes. the feeding section is most sensitive to particles and fouling. 4 educts via 4x3 holes or… For such an application the conventional housing needs only other housing bottom parts as to feed those single holes accordingly. the StarLam series can be cleaned in a straightforward manner. The plates of each layer are turned by 30° so that separate feeds result. -300. mixing occurs by turbulence. As for any microstructured mixer.S TA R L A M I N AT O R STAR L A M G ROUP C LA S S -3 0 . A star-like plate serves for fluid injection.g. a segregation of fluid layers is given so that mixing is here not effective enough. owing to their simple reversible assembly. 3 educts via 3x4 holes or 6 + 2x3 holes (cf. When plotting mixing efficiency versus pressure drop it becomes evident that a continuity is given to the Caterpillar series. On the contrary. 2 educts via 2x6 holes (standard). 53 detail in photo top left). i. However. the housing is made by precision machining. the StarLam apparatus cannot be used at very low flow rates. 4. which are alternately stacked. 300 and StarLam 3000 Concerning the high flow rates used for practical applications. if fouling was noted. In this flow regime.component housing can be easily rebuild as 2 component housing.g. . at high flow rates experimental characterization of mixing efficiency by using competitive reactions shows that by increased turbulent action an increasing mixing performance of the Star Laminators is reached which then compares with the high quality of the smaller micro mixers. The circular outlet channel has macroscopic dimensions so that also here particles will not be detrimental.3000. The foils of the Star Laminators are fabricated by laser cutting. which is a mounted foil stack. . e. another plate with circular conduit serves for forming the mixing channel and separation of the plates. As to be expected. supplied by IMM. the housing of StarLam30 and StarLam300 are identical and those mixers vary only in height and inner geometry of the mixer foil stack. Despite the fact that such a 3-.

53 StarLam for mixing 3 components at once. 3CSL StarLam 30/300/3000 connected in a multi-testing pilot plant 03 COMPONENTS .

It has been used by a large number of customers. combining the unique properties of the interdigital mixers and their small structures with the wish to process larger throughputs. They combine the regular flow pattern created by multi-lamination with geometric focussing which speeds up liquid mixing.S L I T I N T E R D I G I TA L M I C R O M I X E R SIMM GROUP CLASS SIMM-V2. Ten mixing elements are operated in parallel using common feed structures. SIMHEX. Two kinds of upper housings have been realised: One collecting all ten single outlet streams in one and one with ten separated outlets. the slit mixers are amenable to wide variety of processes such as mixing. SSIMM 54 03 SIMM-V2 SSIMM HPIMM SIMHEX SIMM group class Principle This group class of micromixers is a classic amongst all IMM chemical micro processing products. Extensive knowledge on hydrodynamics. . The latter allows systematic equidistribution measurements. The device has been developed for a liquid/liquid dispersion step. Due to this double-step mixing. mixing performance and reaction engineering for diverse applications of these mixers has been documented worldwide. HPIMM. Interdigital flow passes slit to create multi-lamellae Research Topics at IMM One important task at IMM is the continuous advancement of our components for the use in production. is cited multiple times in literature. single-phase and multiphase organic synthesis. emulsification. The pictures here show our latest efforts for a 10-fold scaled-up version of the SIMM-V2 mixer (ARRAY-10x-Slit Interdigital Micromixer). and is indeed one of our best sellers.

The mixer also comprises expansion-free outlet channel geometry. As a consequence.4571 Inlay: 1. i. as it employs HPLC connectors. g.5 14. Deliberately avoiding volume expansion.04 – 2.4 – 720 8 10000 < L0. Compared to the connectors of the standard version SSIMM.04 – 2. the limits of pressure and temperature during operation are much higher than for flat-seal tightened devices. Monell or Titan on request Technical Data Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Standard material Options HPIMM Multi-lamination 25 x 21 x 37 1/16˝ / 1/16˝ HPLC approx. but relies on multi-lamination and geometric focusing only. Technical Data Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Standard material Options SIMM-V2 Multi-lamination 30 x 40 x 30 1/16˝ / 1/16˝ HPLC 45 x 200 Body: 1.4571 Inlay: 1. e. to pumps and tube reactors. Principle This micromixer was optimized using a metal sealing for tightening the two parts of the housing. renounces on jet mixing.4401 Other materials like Hastelloy.e.55 SIMM-V2 HPIMM Individual parts of the SIMM-V2 device Individual parts of the HPIMM Principle This version has all the benefits of mixing using multi-lamination and focusing only.5 27 – 1350 15 10000 < L0. coming along with improved fluidic connections.4435 Other materials like Hastelloy.001 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (µl) Max Viscosity (mPas) Leakage Class -40 – 500 600 0. Monell or Titan on request 03 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (µl) Max Viscosity (mPas) Leakage Class -40 – 220 100 0.001 COMPONENTS . the HPLC joint to steel tubing improves leak tightness and higher pressure operation can be achieved. 45 µm x 200 µm Body: 1. the inner volume could be decreased to only 8 µl.

It combines the regular flow pattern created by multi-lamination with geometric focussing and subsequent volume expansion. Monell or Titan on request. SIMHEX. the limits of pressure and temperature during operation are limited but conveniently provide the possibility of heating or cooling the device. SSIMM 56 SIMHEX SSIMM 03 Slit Interdigital Mixer Heat Exchanger (SIMHEX) Standard Slit Interdigital Micromixer (SSIMM) Principle This micromixer was optimized considering a heat exchange function within the mixer. incl.5 1/16˝ / 1/16˝ soft tube 45 x 200 Body: 1.4435 Other materials like Hastelloy. which speeds up liquid mixing of the multi-lamellae and leads to jet mixing. Technical Data Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Standard material Options SIMHEX Multi-lamination 25 x 25 x 20 1/16˝ / 1/16˝ HPLC 40 x 300 Body: 1.001 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (µl) Max Viscosity (mPas) Leakage Class -20 – +100 3 0. The mixer also comprises expansionfree outlet channel geometry. Principle This micromixer is the classic one amongst all IMM chemical micro processing products. Due to the volume expansion the mixer contains an inner volume of 40 µl and is only offered with non-stainless soft tube connectors. renounces on jet mixing.4401 Other materials like Hastelloy.S L I T I N T E R D I G I TA L M I C R O M I X E R SIMM GROUP CLASS SIMM-V2. heat exchanger function Technical Data Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Standard material Options SSIMM Multi-lamination 19 x 30 x 16. using a graphite sealing for tightening the two parts of the housing.04 – 1. HPIMM. Monell or Titan on request Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (µl) Max Viscosity (mPas) Leakage Class -100 – 500 50 0.001 .4571 Inlay: 1. but relies on multi-lamination and geometric focusing only.5 72 – 3600 40 10000 < L0.e. i.4571 Inlay: 1. As a consequence.04 – 2.0 18 – 900 10 10000 < L0.

order numbers SMI-Ni25. The size of SMHXI inlays: 20 mm x 6 mm The following inlays are available: • Laser-cutted inlays (channel width 45 µm. SMI-Ni40. or other channel dimensions on request. or other channel dimensions on request. SMI-Ag25 or SMI-Ag40 • ASE (thermally oxidised silicon.57 Slit mixer inlays SMI (for SIMM-V2 and SSIMM) SIMHEX inlays SMHXI High pressure mixer inlays HPMI Laser ablation Inlay for SIMM-V2 and SSIMM Laser-cut Inlay for SIMHEX Laser-cut Inlay for HPIMM This inlay fits the standard mixer as well as the version 2.6 mm thickness with different possible channel sizes and depths. extra bases of 3. order number SMI-Lasab45200 • LIGA technology (channel width 25 µm or 40 µm) made from silver or nickel on copper with 300 µm channel depth. 250 µm channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request. order numbers SMI-Si30 or SMI-Si50.5 mm and ~ 3. As these inlays are only 0. order number HPMILas45250 03 COMPONENTS . channel width 30 µm or 50 µm) with 100 µm channel depth. The size of HPMI inlays: 8. 250 µm channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. The following inlays are available: • Laser-ablation (channel width 45 µm. 200 µm channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. For both versions the inlays have a size of 11.6 mm thick. order number SMHXI-45250 This inlay fits the high-pressure slit mixer exclusively.0 mm in diameter and 250 µm in thickness The following inlays are available: • Laser-cutted inlays (channel width 45 µm.0 mm thickness are needed This inlay fits the slit interdigital mixer heat exchange exclusively.0 mm x 7.

known from the SIMM series.3 – 18 s range. The reactor can be used up to 50 bar and 180°C (Viton. with residence times in the 0. Chemraz gasket) or higher if graphite is applied. whilst the fast mass transfer derives from the meanwhile incorporated interdigital micromixer.LIQUID/LIQUID MICROMIXER LLMR-MIX 58 03 Liquid/Liquid Microreactor with internal Mixer – LLMR-MIX Principle The Liquid/Liquid Microreactor is mainly designed for highly exothermic reactions and can also be applied for contacting two immiscible liquids and performing a reaction thereby. The laser-cut inlay of the LLMR-MIX . Insofar. it is particularly designed for reactions that benefit from excellent heat transfer as well as fast mass transfer. Flow rates Detail of the internal mixing section from 50 ml/h up to 2 l/h are feasible. The heat transfer is provided by specific surfaces of 10. The LLMR-MIX can be offered of different materials on request besides the standard stainless steel. It comprises two microstructured plates with integrated micro mixer and micro heat exchanger.000 m2/m3 in micro channels of a width of 200 µm at an aspect ratio of 6.

Monell.01 Standard cooling channels (µm) 200 x 1200 Standard material Housing.4539 Inlay: 1.4404 Other materials like Hastelloy. reaction and cooling plate: 1. a reactor with internal arrangement of 4 LLMRMIX including delay loop 03 Technical Data Name Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Liquid/Liquid Microreactor LLMR-Mix Multi-lamination 45 x 120 x 26 1/16˝ / 1/16˝ for chemicals 1/4˝ / 1/4˝ for cooling fluid 45 x 200 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Max Viscosity (mPas) Leakage Class -20 to + 300 50 0.59 LLMR-MIX-HC276 disassembled LLMR-MIX explosion drawing LLMR-MIX made of Hastelloy LLMR-SY.3 – 18 1000 < L0.4571 or 1.05 – 2 0. Titan or plastics on request Options COMPONENTS .

a large circular arc was chosen for the feed array. to have a robust steel design. For the SuperFocus SFIMM-V2 throughput of about 350 l/h at a pressure loss of 3. defined time frame. Although steel is employed as construction material. characteristic for the SIMM components. thus being less particle sensitive.5 bar was determined for watery systems. which is e. for high-pressure operation and to use a still higher focusing ratio. The latter is dependent on the volume flow. characteristic of the StarLam series and uniform flow patterns.g. To arrange as many as 138 nozzles. Specialty designs with notably reduced focusing time are possible. . as the ratio of outer to inner lamellae is 136:2.g. allowing one to perform fast temperature switches for starting and ending reactions in a very short. Compared to the predecessor design more nozzles enable fluid feed. e. the focusing ratio was increased from 40 formerly to now 178 (and can be set higher on demand). Disassembled SFIMM-V2-300 The mixing time achievable is 4 ms according to calculation and experiments made with the former design. i. The formation of flow patterns is very uniform. The same holds for integrated mixing-heating element configurations. this means having a nozzle feed array. Development target was to achieve even higher throughputs. albeit the final focused lamellae width of about 4 µm was kept. design and characterisation of the former version SFIMM. to reduce the sensitivity towards blockage.g.e.g. Physically speaking. The nozzle width was enlarged. a triangular-type focusing chamber and a thin mixing channel. that lamellae are thicker at the wall (boundary) than in the interior of the flow. The mixing channel width and length compares to the former design so that the semianalytical and experimental reaction type based findings on the mixing time can be largely transferred to the new design. as e. e. In particular this deviation should be less here compared to other systems.e. which is e. The SuperFocus Mixer Version 2 (SFIMMV2) bases upon the simulation. albeit excluding the time needed for flowing through the focusing chamber.V 2 60 03 SuperFocus microstructured mixer SFIMM-V2-300 Central plate of the SFIMM-V2-300 Principle Focusing mixers perform a multi-laminating step and geometrically focus the streams (in a way similar to hydrodynamic focusing) to thin the lamellae and then mix by diffusion.S U P E R F O C U S I N T E R D I G I TA L M I C R O M I X E R SF I M M .g. an optional inspection window may allow the monitoring of the flow patterns and of the mixing course. The SuperFocus mixer thus combines both high throughput. i. a multi-lamellae flow is found all over the focusing chamber until the mixing channel is reached. The known deviations from ideal given for any multi-lamellae flow are found as well. done in quench-flow analysis. e.g.

4435 Other materials like Hastelloy.001 03 Mixing structure of SFIMM-V2-30 SFIMM-V2-30 with straight outlet for high viscosity emulsions COMPONENTS . Monell or Titan on request.61 Multi-lamellae flow in the SuperFocus microstructured mixer SFIMM-V2-300 Technical Data Name Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (µm) Number of feeding channels Width of feeding channel Focusing ratio Standard material Options SuperFocus Interdigital Micromixer Version 2 -300 SFIMM-V2-300 Multi-lamination 140 x 140 x 40 1/4˝ / 1/4˝ 500 µm x 5 mm 138 260 178 1. named SFIMM-V2-30 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Max Viscosity (mPas) Leakage Class -40 – 220 100 10 – 300 10000 < L0. heat exchanger function is possible The SFIMM is meanwhile also produced as smaller device for about one tenth of the original throughput.

by two pump-driven. This reaction hardly can be handled in any other micro device. a specialty mixer was developed that performs mixing in a ”wall-free” environment. For this reason. As a matter of fact. Particle generation is simply not possible in the vast majority of today’s micro devices. most organic processes are associated with more or less precipitation during the course of reactions. falling jets merging into one in a Y-shaped configuration. only 350 µm wide nozzles. The mixer has been tested for inorganic reaction processing such as calcium carbonate precipitation and organic reaction that are associated by strong fouling. in addition to mixing quality judgement. e. the nozzles of the jet mixer have tiny.IMPINGING-JET MICROMIXER IJMM 62 03 Impinging-Jet Micromixer Principle Deliberately slow mixing is an issue when fast mixing would have deleterious effects on processing. The aminolysis of acetyl chloride with n-triethylamine in THF leads to instantaneous heavy precipitation. i. like quaternizations. the better the mixing quality. Intense knowledge on jet configuration as a function of flow rate and jet diameter has been documented. by plugging the whole system.e.g. 3 different flow patterns: • Y-type jet of IJMM (top) • Fan-shaped jet (middle) • Fanned-out jet (down) . It is an extreme representative of many other organic reactions that suffer more or less from fouling.g. As a result. It was shown that the smaller the jet diameter. e.

60°. IJMP. including heat exchangers.4571 Other materials like Hastelloy. plant section.001 IJMM in adequate housing as used for IJMP COMPONENTS . Monell or Titan on request 03 Impinging-Jet micromixer Plant. pumps.63 Fluid A Fluid B IJMM in a special funnel-like housing for particle production Geometric parameters determine the mixing performance. beside flow parameters Technical Data Name Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard boring-/noozle diameter d (µm) Orientation angles (d) Standard material Options Impinging-Jet Micromixer IJMM Jet collision 10 x 35 x 10 1/8˝ / 1/8˝ Clamp screw 350.5 – 3 0 0 100 < L0. cf. 1000 45°. 90° 1. 500. process control system Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (µl) Max Viscosity (mPas) Leakage Class -40 – 220 10 0.

g.FA L L I N G F I L M M I C R O R E A C T O R FFMR GROUP 64 03 Members of the extended Falling Film Microreactor family Principle The Falling Film Microreactor utilizes a multitude of thin falling films that move by gravity force for a typical residence time of seconds up to about one minute. starting from the FFMR-STANDARD in recent years the concept has faced several extensions and even more important has been brought from lab scale to pilot and production scale. Its unique properties are the good temperature control by an integrated heat exchanger and the specific interface of 20. exploited when performing direct fluorination of toluene with elemental fluorine in the original version of IMM´s Falling Film Microreactor (FFMR-STANDARD). This so far uncontrollable and highly explosive reaction could be managed under safe conditions and with control over the reaction mechanism and therewith selectivity.000 m2/m3. . Such high mass and heat transfer were e. Due to the high raised interest for such a kind of device. The several types of Falling Film Microreactors including the new ones are introduced in the following.

First tests based on CO2 absorption in aqueous sodium hydroxide have proven that significant performance improvements can be achieved. 03 Operating Conditions Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Falling Film Microreactor (Standard) FFMR-STANDARD 120 x 76 x 40 all 1/4˝ 1.5 Other materials like Hastelloy.8 – 20 25 – 100 up to 20000 L0.5 for channel geometry 1200 µm 0.6 for channel geometry 600 µm 1.05 for channel geometry 300 µm 0.6 5 3 Temperature (°C) Pressure stability (bar) Flowrate (l/h) 180 (option: 300) 10 (without Borofloat glass: 20) 0.4571 for housing and reaction plate Copper for cooling plate Borofloat glass for inspection 300 x 100 (64 channels) 600 x 200 (32 channels) 1200 x 400 (16 channels) 7. Monell or Titan on request COMPONENTS .5 Depth: 0.65 Falling film principle in a multichannel architecture Thermographic monitoring: Initial wetting flow (FFMR-STANDARD) FFMR Standard Reactor assembled Reactor disassembled Reaction plates Research Topics at IMM IMM is exploring the potential of further structuring the straight reaction channels in the Falling Film Microreactor. So IMM realised recently a reaction plate in which each of the channels have been modified by incorporation of additional grooves in order to improve via recirculation flows the liquid side mass transport.01 Residence time (s) Liquid film thickness (µm) Interfacial area (m /m ) Leakage Class 2 3 Standard reaction channels (µm) Reaction channel length (cm) Gas chamber height (mm) volume of gas chamber (mm ) Standard cooling channels (mm) Options 13336 Width: 1.

FFMR GROUP 66 FFMR-LARGE & FFMR-CYLINDRICAL 03 Reaction plates for FFMR-STANDARD and -LARGE Starting from FFMR-STANDARD two new reactor types have been developed targeting at a tenfold increase of the structured surface area on the reaction plate. The number of the reaction channels has been increased by a factor of 7.100 about 9814 .0 Other materials on request Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Liquid film thickness (µm) Interfacial area (m /m ) 2 3 180 10 (without glass: 20) investigated range 0. FFMR-CYLINDRICAL follows another approach. FFMR-CYLINDRICAL FFMR-STANDARD and -LARGE Technical Data Name Order number Size (L x B x H) Connectors Material Standard reaction channels (µm) Reaction channel length (cm) Gas chamber height (mm) Volume of gas chamber (mm3) Standard cooling channels (mm) Options Falling Film Microreactor Large FFMR-LARGE 320 x 156 x 40 all 1/4´´ 1.5 90000 Width: 0.20 calculated 16 .24 . The reaction channels are now engraved on the outside of a metallic tube. the length of the channels has been elongated a bit to get a tenfold increase of structured surface area.8 calculated 60 .20 calculated 23 .1. The cylindrical shape allows a quite compact design in this case.2 Depth: 0. In the FFMR-LARGE therefore the length and the number of channels have been increased by a factor of 100.22470 .5.24 . From the general design FFMR-LARGE is quite similar to FFMR-STANDARD.2 Depth: 1.6 calculated 45 . The FFMR-CYLINDRICAL is of special interest for photochemistry applications.4571 for housing and reaction/cooling plate Quartz glass for inspection 1200 x 400 (50 channels) about 25 4.16780 180 5 investigated range 0.4 Other materials on request Falling Film Microreactor Cylindrical FFMR-CYLINDRICAL 80 x 130 1/8´´ and 1/4´´ (welded tubes) 1.76 about 13140 .5.4571 DURAN® glass for inspection 1200 x 400 (120 channels) about 10 5 100000 Width: 1.1.

8 about 60 .4571 + Ni screen printing braze 1200 x 400 (50 channels) about 25 500 4 730000 Width: 1.4 .12.67 Brazed Falling Film Microreactors (STACK-FFMR) STACK-1x-FFMR-LAB STACK-1x-FFMR-LARGE (open/closed) STACK-10x-FFMR-LARGE Outlook for even larger reactors: test reaction plate for FFMR-XXL Technical Data Name / Order number Size (L x B x H) Connectors Material Standard reaction channels (µm) Reaction channel length (cm) Reaction channels number Gas chamber height (mm) Volume of gas chamber (mm3) Standard cooling channels (mm) Options STACK-1x-FFMR-LAB 294 x 28 x 19 all 1/8´´ 1.16780 COMPONENTS The reactor concept of FFMR-STANDARD and -LARGE has been transferred to a pure plate design to which brazing as joining technology can be applied. Compared to STACK-10x-FFMR-LARGE it should allow identical experimentation at a throughput of only 1/100 of the STACK-10x-FFMR-LARGE.4 On request STACK-10x-FFMR-LARGE 296 x 118 x 75 all 3/8´´ 1.2 Depth: 0.12 about 23 . So STACK-10x-FFMRLARGE contains 10 functional elements.4 On request STACK-1x-FFMR-LARGE 296 x 118 x 12 all 3/8´´ 1. Brazing technology opens the door for specifically adopted reactors for high pressure applications.24 .20 about 23 .100 about 9814 .2 Depth: 0.4571 + Ni screen printing braze 1200 x 400 (50 channels) about 25 50 4 73000 Width: 1.16780 up to 800 @ 1 bar up to 50 @ 25 °C about 0.100 about 9814 .100 about 9814 .4571 + Ni screen printing braze 1200 x 400 (50 channels) about 25 5 4 7300 Width: 1. To round up the brazed reactor program also a new lab version has been developed (STACK-1x-FFMR-LAB).16780 up to 800 @ 1 bar up to 50 @ 25 °C about 2.2 Depth: 0.0.02 .8 about 60 .0 about 23 . .1.8 about 60 . The STACK-1x-FFMR-LARGE thereby represents the equivalent to FFMR-LARGE and the basic functional element for following numbering-up.4 On request 03 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Liquid film thickness (µm) Interfacial area (m2/m3) 180 10 about 0.

Coprecipitation and sol-gel techniques were applied as well for catalyst deposition. one passage solely with electrical heating: No insulation plates. Most commonly. The plates can be coated with catalyst. either with or without internal heat transfer. Intense studies on periodic reactions were made with this reactor by three well-known European research groups. and subsequent catalyst impregnation are applied. The device can also be used as a gasphase and/or liquid-phase micro heat exchanger. of various aluminas. On request. catalyst deposition in the micro channels can be offered as well. concerning the oxidation of propane. Counter-flow principle . so that the assembled device can be operated as gas-phase reactor.GAS PHASE MICROREACTOR G PM R 68 03 Gas Phase Microreactor Principle The Gas Phase Microreactor comprises a stack of several microstructured plates (generally 10 + 10 plates) that are arranged for counter-flow or co-current flow practice. wash coating of different carriers. the dehydration of isopropanol. e. and the selective oxidation of isoprene to citraconic anhydride.g. Each plate consists of 34 parallel micro channels of 300 µm width and 200 µm depth.g. The GPMR is a modular system which can also be customized (e. special designed end caps with integrated heat cartridges). The plate stack is encompassed by two ® ceramic Macor plates. for thermal insulation to the environment and the two steel end caps.

69 Gas phase reactor installed in bench-scale plant Plate coated with catalyst Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Standard material Number of catalayst plates Size of catalyst plate (mm) Channel geometry of the catalyst plates (µm) Options Gas Phase Microreactor GPMR 70 x 70 x 55 1/8˝ 1. here as simple heat exchanger (COMH) for education purpose 500 3 1 – 7 / 1 – 600 L0.1 18000 580 2900 32 Counter.4571 for housing and catalyst carrier Glass ceramics MACOR for insulation layer 20 40 x 40 300 x 200 GPMR is also usable as a single heat exchanger. end caps for heating cartridges Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) liquid/gas Leakage Class Heat transfer area (m /m ) Total inner surface per layer (mm2) Specific inner surface per layer (m2/m3) Active inner volume per layer (mm ) Operation mode 3 2 3 GPMR integrated into a plant.or co-current flow 03 COMPONENTS .

5 l/h. By this means. 0. each filled with one stack of microstructured platelets. 4 l/h. As a result. investigations in the explosive regime are safely amenable. A small total mass of the construction material. safe operation in the ex regime (3 vol. 0. 80 vol. even when approaching rela-tively large temperatures. The mixer-catalyst zone reactor has been extensively studied for its use for ethylene oxide synthesis. 277°C). e.g. hot-spots are reduced and near-isothermal operation can be achieved. 290°C). up to 600°C. balance nitrogen.17 l/h. serving for feed and fluid withdrawal. e. which are connected via a conduit. hence a compact arrangement of the functional units.M I X Gas Phase Microreactor with Mixer and Internal Heating/ Cooling Top housing plate of reactor with mixer and reactor stack Principle The Gas Phase Microreactor with Mixer and Internal Heating/Cooling GPMR-MIX contains two recesses.3 MPa. The platelet construction material itself may act as catalyst or. forming a flow-through chamber.124 s. the channels may be coated with a catalyst layer.-% ethylene. 5 bar. a maximum selectivity of 69% (6 vol. The first stack comprises two types of mirror-imaged platelets with parallel feeding channels which are alternately arranged so that a multi-lamination flow configuration is created for gas mixing. wet chemically using the wash-coat route or by means of thin-film deposition. mixing is completed within short time due to the virtue of decreasing the diffusion path. Both stacks are connected to welded tubes.g.-% ethylene. In the conduit attached. as demonstrated by research with this and similar tools.-% ethylene. and higher conversions at comparable selectivity compared to fixed-bed technology (20 vol. more preferably. 50 vol. Hence the mixed reactant gas volume (before reaction) is kept as small as possible.-% oxygen. 230/250°C) were demonstrated. Schematic of the GPMR-Mix device and details of the functional principle .-% oxygen.70 03 GAS PHASE MICROREACTOR WITH MIXER A N D I N T E R N A L H E AT I N G / C O O L I N G G PM R. 100 K/min). balance nitrogen. Internal cooling typically of similar time scale is provided by convection flow of a gas stream at high flow rate in a channel which surrounds the functional units.78 tons h-1 m-3). high space-time yields (up to 0. typically in the range of a few minutes (ca.-% oxygen. 5 bar. not far from the industrial benchmark. Among other results of the parametric study. and internal large-power heat supply guarantee fast heating up. 3. 30 vol. The second stack comprises platelets with parallel channels of small depth so that very good heat transfer is provided.

5 180 – 490 x ~ 100 10 9.5 COMPONENTS Inconell 600 (2.4816) for housing and top plate 1.5 460 x 125 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Leakage Class Specific surface area (m /m ) Total inner surface per reaction layer (mm ) Specific inner surface per reaction layer (m2/m3) Active inner volume per layer (mm ) 3 2 2 3 03 600 50 5 0.5 x 7.5 x 9.1 12700 54 3840 2.71 Individual parts of GMPR-Mix Mixer and reaction platelet Laser-cut mixer platelets Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Standard material Number of mixing plates Size of mixing plates (mm) Channel geometry of mixing plates (µm) Number of catalayst plates Size of catalyst plate (mm) Channel geometry of the catalyst plates (µm) Gas Phase Microreactor with Mixer and Internal Heating GPMR-MIX 40 x 40 x 30 1/4˝ 10 7.025 – 2 < L0.4571 for mixing and catalyst plates .

The plates are easily exchangeable and the assembly of the reactor is simple. Thus absence of bypass effects could be proven. it may be as well applied as a testing reactor for all kind of heterogeneous gas phase reactions at flow-rates exceeding the range of small-scale laboratory devices. however. the reactor plates can be coated with various carrier/catalyst systems. . The CMBR was designed for testing the catalysed burning of fuels with different catalysts. Heating of the reactor is realised by heating cartridges with temperature determination feasible at two positions inside the reactor. The Catalyst Micro Burner Reactor is designed for a power generation in the range of several hundreds of Watts by burning various fuels. On demand.C ATA LY S T M I C R O B U R N E R R E A C T O R CM BR 72 03 Catalyst Micro Burner Reactor Principle The Catalyst Micro Burner Reactor is a testing reactor composed of a housing which can take in a stack of up to 16 microstructured plates. No other products than carbon dioxide and water were found above the detection limit. Full conversion of 32 g/h methanol was achieved with a conventional Pt-catalyst at 130°C reaction temperature.

1 COMPONENTS .10 – 1 < L0.73 Single parts of the Catalyst Micro Burner Reactor Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Standard material Number of catalayst plates Size of catalyst plate (mm) Channel geometry of the catalyst plates (µm) Micro channel surface area per platelet (mm2) Options Catalyst Micro Burner Reactor CMBR 160 x 120 x 50 1/4˝ 1.4571 1 – 16 50 x 50 600 x 400 588 Other materials on request 03 Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Leakage Class 550 5 10 – 150 0.

Variation of the reactor length. the one inlet stream flows serially in a zigzag manner from one plate to the other. Serial operation (1 in. being turned around and guided to the next level and so on. the micro structured plates can be coated with various carrier/catalyst systems. Screening or numbering-up of catalysts. 10 out): Even testing ten different catalysts using ten different gases (at similar pressure) can be applied by assembling the reactor with two end caps for parallel operation. On demand. Two end caps for parallel operation Stack of cartridges with coated microstructured plates . By simple exchange of the end caps a decision can be made whether to operate the microreactor in serial or in parallel mode. 1 out): Using two other end caps similar in shape. finally resulting in a path of ten times length compared to the single plate length. The sub-streams leave then through the ten separate outlets that can be analyzed accordingly. respectively ten times the residence time. Screening of catalysts. 10 levels with different catalysts and/ or different gases. They are easily exchangeable using an included mounting tool and relatively inexpensive due to mass fabrication by wet-chemical etching. 10 out): Using a diffuser-type end cap.C ATA LY S T T E S T I N G M I C R O R E A C T O R CT M R 74 03 Catalyst Testing Microreactor with end caps for parallel operation Principle The Catalyst Testing Microreactor consists of a housing comprising twenty micro structured plates positioned pairwise face to face resulting in ten levels of parallel microchannels. 10 levels with different catalysts but same feed gas. the microstructured plates are fed simultaneously by the one common inlet stream. Parallel operation (10 in. Parallel operation (1 in. Up to 10 plates with identical catalyst may be installed.

1 03 Options Catalyst plates can be delivered with various channel geometries: Channel geometry (width µm x depth µm): 2900 x 300 2000 x 300 1000 x 300 1000 x 100 750 x 300 750 x 100 500 x 300 500 x 100 Number of channels: 3 4 7 7 9 9 12 12 COMPONENTS .75 Special version for 800°C and 20 bar operation Standard version disassembled Alternative heating option with one heat jacket instead of 10 heat cartridges Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Standard material Number of catalayst plates Size of catalyst plate (mm) Options Catalyst Testing Microreactor CTMR 100 x 100 x 108 1/4˝ / 1/16˝ for parallel operation 1/8˝ / 1/8˝ for serial operation 1.025 – 2000 < L0.4 – 40 0.4841 for housing 1.4742 for catalyst plates 20 50 x 14 Other materials on request Operating Conditions Temperature (°C) Pressure stability (bar) Standard flow velocity (m/s) Residence time (ms) Leakage Class 800 20 (100 bar at 400°C) 0.

typically gas-phase reactions.g. The core elements are chemically etched microstructured plates.W E L D E D M I C R O H E AT E X C H A N G E R W T-S E RI E S 76 03 Laser-welded micro heat exchanger group class (WT-series). The high efficiency and heat transfer coefficients of the micro channels are even more enhanced compared to conventional heat exchangers due to the low material thickness (low heat resistance) and high inner specific surface. WT-404. the channels of plates can be coated with catalyst using the heat exchanger as reactor for heterogeneously catalysed reactions.L A S E R . These heat exchangers are normally designed for flow rates between 1 l/h up to 400 l/h.or small-scale production plants is possible. gas/ liquid or gas/gas applications and can also serve for evaporation or condensation. Being assembled with conventional 1/4” or 3/8” tubes. They comprise a laser welded stack of arranged microstructured plates enabling a counter. easy integration into the existing tubing system of pilot. sealed by high-precision laser welding.or co-current flow scheme. higher flow rates of up to 1000 l/h are possible at moderate pressure drops. like e. steam reforming. WT-204 (from left to right) Principle The WT-series was developed as a heat exchanger for liquid/liquid. Additionally. WT-304. Single plates of the WT…08-series Single plates of the WT…04-series .

max. also for condensing HCOMH COMPONENTS . 20 bar) 2.5 – 50 up to 1000 @ 1 bar 5 @ 25 °C (higher upon request. others on request WT 404 100 x 44 x 42 3/8˝ / 3/8˝ Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (water. others on request 800 x 400.77 Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Dimensions of heating channels (µm) WT 204 60 x 24 x 23 1/4˝ / 1/4˝ Laser-Welded Micro Heat Exchanger Series WT 304 80 x 34 x 32 3/8˝ / 3/8˝ 316 Ti. l/h) 0.5 – 250 6 – 600 03 Other examples of laser-welded micro heat exchangers Special type HxA Special Heat Exchanger.

The high efficiency and heat transfer coefficients of the micro channels are even more enhanced compared to conventional heat exchangers due to the low material thickness (low heat resistance) and high inner specific surface. HX-304 (top right).or co-current flow scheme. Single plates of the HX-304-series (left: blank. They comprise a brazed stack of aligned plates enabling a counter. HX-404 (bottom right) Principle This novel HX-series was developed as a heat exchanger for liquid/liquid. laminary joined applying brazing technology. HX-204. These new heat exchangers are normally designed for flow rates between 1 l/h up to 400 l/h. gas/liquid or gas/gas applications at high pressure and temperature regimes. The core elements are chemically etched microstructured plates. higher flow rates of up to 1000 l/h are possible at moderate pressure drops. right: coated with screen printing paste) .B R A Z E D M I C R O H E AT E X C H A N G E R S HX-SERIES 78 03 Brazed micro heat exchanger group class (HX-series).

IMM extended strongly the application of the brazing technique as sealing technology for microreactors of different functionality. 150 x 80 x 25 3/8˝ / 3/8˝ 316 Ti. which is tested for operation at 120 bar @ 250 °C.5 – 50 up to 800 @ 1 bar up to 500 @ 25 °C 2. Further the brazing technique makes a multiplicity of new reactor geometries accessible. also been applied for realising the prototype of a high pressure microreactor with two temperature zones with a reactor interior volume on the reaction side of 90 ml (HPMR-2TZ-V2-90ml). Besides the HX-series the technology has e. Thereby large interior volumes are possible with high pressure strength at the same time. High Pressure Microreactor with two temperature zones (Type HPMR-2TZ-V2-90ml)) Section view of two brazed plates aligned face to face Complex feed structures are feasible: The picture shows the feeding structure for a SuperFocus like micromixer with nozzle like outlets for an inner liquid phase surrounded from top and bottom from chains of rectangular feed structures for the outer liquid phase.5 – 250 10 – 1000 Brazed (high pressure) Microreactors Research Topics at IMM Brazing opens the possibility of interconnecting large-area reactor structures monolithically. l/h) 0. 200 x 120 x 40 1/2´´ / 1/2´´ Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (water. COMPONENTS . others on request HX 404 ca.79 Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Dimensions of heating channels (µm) HX 204 ca. 100 x 60 x 20 1/4˝ / 1/4˝ Brazed Micro Heat Exchanger Series HX 304 ca. others on request 1000 x 600. 03 At IMM the microstructured reactor plates are coated with the brazing paste by using the screen printing machine Type THIEME 1010 E.g.

Operation conditions are tested for maximum 300°C @ 1 bar or 45 bar @ 25°C. comprising THTMD plus heat cartridge. two thermocouples and electronic control unit In the latter case. The optimized size of this device allows a very fast heating up as well as fast changes of temperatures.T U B E H E AT T R A N S F E R M I C R O D E V I C E THT M D 80 03 Tube Heat Transfer Micro Device Principle The Tubular Heat Transfer Micro Device is a microstructured heat exchanger. Being offered in two sizes. the temperature of the heating process is basically controlled by a thermocouple in the THTMD-outlet as well as an additional thermocouple to avoid overheating is integrated within the heating cartridge itself. Several options can be offered: • THTMD solely • THTMD plus suitable heat cartridge (if suitable electronic control unit is at hand) • Full package. designed for electrical heating of gases and liquids. Technical detail of heat exchanger structure THTMD in parts before laser-welding . the maximum power rate to be transferred can be up to 800 W with a thermal efficiency > 90% (depending on operation conditions).

0 800 > 90% L0.81 Explosion drawing of THTMD Heat control system for THTMD Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Number of heating channels Width of heating channels (µm) Options Tube Heat Transfer Micro Device THTMD 120 x 100 x 15 1/4˝ / 1/4˝ 1. Monell or Titan on request Operating Conditions Temperature (°C) Pressure stability (bar) Flowrate (l/h) liquid Power rate (W) Thermal efficieny Leakage Class up to 500 45 1.0 – 20.1 03 COMPONENTS .4571 60 400 Other materials like Hastelloy.

front view (left) and backside view (right) Principle The Evaporator System is a nearly pulsation-free continuous evaporator without the supply of carrier gas. Rapid preheating. evaporation and over-heating are realized in one single device. Up to 100 g/h water (without carrier gas) can be evaporated. LV1 – Laboratory evaporator for 100 g/h . It comprises a pair of microstructured plates together with a control system for the liquid flow as well as the electrical heating and its temperatures to ensure the continuous use. A maximum temperature of 350°C for the vapour or up to 6 bar system pressure are feasible. Two electrical heating cartridges supply the heat to the corresponding microstructured plates with large specific surfaces for excellent heat transfer.L A B O R AT O R Y E VA P O R AT O R 82 03 Temperature control unit with integrated mass flow controller (upper box) and with integrated LV1 (lower box).

4301 Operating Conditions Temperature (°C) Pressure stability (bar) Temperature (°C) of Vapor Flowrate (g/h) Power rate (W) 400 6 up to 350 10.0 400 03 COMPONENTS .83 LV1 – with open heating housing LV1 – disassembled Technical Data Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Evaporator System LV1 300 x 300 x 360 1/8˝ / 1/8˝ 1.0 – 100.

Purchaser is obliged to treat the delivery item with care. 2.9 Delivery time will be extended adequately in case of force majeure.4 Specifications as to time of delivery are not binding unless a binding time of delivery is expressly agreed. The foregoing regulation does not stipulate a reversal of the burden of proof for Purchaser. 4. even to prospective agreements and quotations. 5. lockout. 4. 3.5 If the Parties agree that our performance will not be initiated until down payment or advance payment has been made. Upon our request Purchaser is obliged to declare within an adequate respite. gross negligence or damage to life. 3. 3. but not exceeding a total of 5 % of the delivery value.4 On default of payment Purchaser has to pay interest at 8 percentage points above the current base rate according to § 247 BGB (German Civil Code). 2. as well as compliance with agreed conditions of payment and other obligations by Purchaser.5 % of the delivery value for each completed week of delay.2 As long as property is not transferred to Purchaser.000. Notwithstanding the assignment. Our entitlement to collection of debts remains unaffected by Purchaser‘s authorisation. 1. 1. 3. we reserve the right to adequately adjust the price due to changed costs for wages. General Provisions 1. Extent of Delivery and Performance 4. Retention of Title 3. even after expiry of an additional respite of delivery. whether he withdraws from the contract because of the delay of the delivery or demands delivery.2 These terms and conditions apply to all our agreements and quotations.4 These terms and conditions also apply in case we supply even though contradiction or divergence of Purchaser’s conditions from our terms and conditions is known to us.7 Damages claims of Purchaser resulting from delay of delivery as well as damages claims in place of delivery exceeding the limits set by foregoing no. that resulting from this he suffered damage – will be entitled to demand indemnification amounting to 0. 1. if we do not deliver within an adequate additional respite granted by Purchaser. we are entitled to detain delivery under this contract for the duration of default of payment. public legal persons and public special funds according to § 310 section 1 BGB (German Civil Code) (“Purchaser”) exclusively. We are entitled to invoice partial delivery separately.1 Invoices are payable net within 30 days as of invoice date. If we do not meet a binding time of delivery. Payment Terms 2. we hereby accept assignment. 3. If so and unless otherwise agreed. delivery time will not begin unless the according amount has been credited to our business account subject to a separate agreement. In the event of such agreed submission of bills of exchange or cheques. In case of reasonable partial delivery Purchaser is not entitled to lay a lien on his payment for reasons of outstanding parts of delivery. unless we are responsible for the delay. In such cases we reserve the right to withdraw from the contract taking into account Purchaser’s interests.3 Bills of exchange and cheques are only accepted on explicit agreement and only on account of performance and they shall not be deemed to constitute payment until honoured. if said claims are undisputed or legally confirmed. ordering amounts of more than 10. 4.3 Purchaser’s conditions which are contradictory to or diverging from our terms and conditions do not apply unless their validity is expressly agreed in written form. prior notice to Purchaser provided. . 3. fire and water. and apply exclusively. This shall not apply in case of minor outstanding payment.3 In case we owe a separable performance. 1. 3.1 The terms and conditions set forth herein apply to deliveries and sales to entrepreneurs. Purchaser will be entitled to withdraw from the contract.11 In case of application to open insolvency proceedings as well as of affidavit of means according to § 807 ZPO (German Code of Civil Procedure) we are entitled to detain delivery until consideration has been executed or until Purchaser furnishes appropriate security.5 Purchaser will be entitled to set off with counterclaims only. partial delivery is permitted for relevant reasons to a reasonable extent. delay of external suppliers and other unexpected circumstances. 3. by legal proceeding if necessary.-. 5. Purchaser is authorised to assert and collect claims in his own name. Oral offers are not valid unless a written confirmation is submitted.1 We reserve the right of property in the delivery items until Purchaser completely satisfies our claims arising from the contract at hand. breakdown. The second rate is due after delivery. Claims arising from said insurances as well as everything possibly acquired as a substitute according to § 285 BGB (German Civil Code) are herewith assigned from Purchaser to us. 6 are excluded in all cases of delayed delivery. due payment provided. strike. 5. material and distribution of deliveries. 2.84 04 GENERAL TERMS AND CONDITIONS OF DELIVERY AND SALE 1.3 Unless a fixed price agreement is reached. Purchaser is entitled to lay a lien on his payment only as far as the counterclaim is based on the same contractual relationship.10 If Purchaser defaults in payment in the context of other present contractual relationships between Purchaser and us. We reserve the right to claim a higher damage as a result of default.2 Our prices are effective “ex factory” plus value added tax and costs of delivery and packaging. 3. respite of delivery will be adequately prolonged.1 Our offers are not binding until our written order confirmation is submitted. Particularly Purchaser is obliged to insure the delivery item sufficiently according to its replacement value and at Purchaser‘s own expenses against damage caused by theft. Furthermore. Purchaser – in case Purchaser credibly shows.6 If we exceed time of delivery. If these requirement are not timely fulfilled. body or health.EURO will be invoiced in two rates of 50% of the order value each. 4. 4.2 Purchaser bears the costs and risks of delivery. we are entitled to claim full payment and – after futile expiration of a reasonable additional respite – to withdraw from the contract unless Purchaser furnishes adequate security on our demand. This shall not affect the cases where IMM’s liability is mandatory by law in cases of intent.1 The order confirmation discloses the whole extent of the delivery and performance owed.8 Meeting respites of delivery requires timely receipt of all documents as well as required permissions and clearances and particularly of plans to be delivered by Purchaser. payment shall only be deemed to have been made upon encashment. which are carried out three months after conclusion of the contract or later on. Necessary maintenance or inspections are to be performed by Purchaser at Purchaser‘s own expenses in due time. Offers and Prices 3.2 Unless otherwise agreed. This also applies to the waiver of the written form itself. 3. delivery will not be performed until receipt of the first rate.5 All agreements between us and Purchaser for the purpose of performance of the contract at hand require written form.

in case of fair wear and tear and damages. Even after cession Purchaser remains authorised to collect outstanding claims. we will not collect the debt as long as Purchaser fulfils his obligation of payment. 7. 9 shall apply mutatis mutandis. 7.8 Should complaints turn out to be unjustified and should we not have given reasons therefore. taking over for operation. gross negligence. gross negligence. particularly expenses for delivery. we will be entitled. However. Purchaser herewith undertakes to assign proportionate co-ownership to us according to our contribution and keeps the ownership or co-ownership by us in safe custody. and in case of breach of cardinal contractual obligations. subject to notice of defect in due time by Purchaser. If any defect becomes apparent during such inspection or is later detected. particularly of default of payment or breach of these terms and conditions. if and to the extent to which third parties are not able to refund costs arising in or out of court for actions taken in accordance with § 771 ZPO (German Code of Civil Procedure). 5. service. If Purchaser or third parties carry out inappropriate maintenance or changes. 04 7.4 In case of garnishment. Relevant value will be that at the time of working. we reserve the right to withdraw from the contract at hand and to reclaim property.1 All other damages claims of Purchaser are excluded no matter what legal ground they are based on.7 We hereby covenant to gradually release at Purchaser‘s demand the securities obtained by retention of title in so far as the property’s value exceeds the debts to be secured by more than 20 %. 7. which accrue after transfer of risk because of careless or faulty treatment. This shall not influence our right to collect the debt. processed or modified item. which already existed at the time of transfer of risk. 7. Purchaser is responsible to inspect the suitability of our products for the intended fields of application. Purchaser is entitled – claims for damages remain unaffected – to withdraw from the contract or demand price reduction. execution of setting up or assembly. Purchaser has to reimburse any and all of our costs in connection with the putative subsequent performance which we could reasonably deem appropriate.g. Shall the delivery item under reserved property be processed or modified together with other objects not belonging to us. such working. 8. Purchaser bears the risk of accidental destruction or deterioration of the delivery items from the time of dispatch and at the latest from the time the delivery items leave the works/storage. which is mandatory by law. are excluded. as our choice may be. The Other Damages Claims 6.1 Period of warranty shall expire twelve (12) months after time of delivery. damage to life. Purchaser is obliged to notify us forthwith. wages and material.5 Purchaser will examine the consignment immediately after receipt for damages. This shall not apply in case of intent. use of unapt equipment or because of special exterior influences. In this case the remainder of Purchaser in the delivery item is continued in the worked. Purchaser has to give written notice thereof including description of the fault to us immediately. 7. 7. The liability of IMM in case of breach of cardinal contractual obligations shall be limited to the foreseeable. 6. 7. irrespective of being oral or written. if additional expenses are caused by subsequent transfer of the delivery items to a place other than Recipient‘s site unless transfer corresponds to the delivery item‘s conventional use. 6. but not later than five (5) working days after delivery and discovery respectively. processing and modification shall always be deemed to be performed on our behalf. 7. Liability for Faulty Goods 8. 5. deviation being customary in trade and technically unavoidable deviation from the agreed condition.4 We do not warrant freedom from third parties‘ rights in the delivery items. This assignment is valid irrespective of whether the delivery items under reserved property were resold without or after product processing. 5.2 If dispatch. which accrue to him from connection of the delivery items under reserved property with immovable property. noncompliance of guarantee of condition. All information. typically occurring damages. like e. Claims of Purchaser because of material defects or defects as to the quality exceeding or differing from this clause VII.2 Claims because of fault are excluded in case of negligible deviation.5 Purchaser is entitled to resale delivery items under reserved property in regular course of business. Claims for recourse remain unaffected by foregoing regulations without restrictions. we acquire co-ownership in the resulting merchandise at an interest depending on the ratio of delivery items‘ objective value to the other objects‘ value which do not belong to us.6 If the delivery items under reserved property are worked. will be excluded. Purchaser is not in default of payment. Purchaser shall be liable for our detriment. Purchaser herewith assigns to us all claims against Purchaser‘s customers arising from said resale at the final amount of the invoice (incl. which exceed the warranty. according to Produkthaftungsgesetz (German Code of Liability for Faulty Products). and damage to life. which are not subject to the contract at hand. Should the resulting merchandise consist of Purchaser‘s objects forming the main part.11 Damages claims of Purchaser because of material defects or defects as to the quality are excluded. Concerning the extent of the claims for recourse of Purchaser against us no. 7.3 In case of breach of contract. in case of negligible impairment of serviceability.7 In case subsequent delivery fails.10 Claims for recourse of Purchaser against us only accrue insofar as Purchaser has not agreed with his customer on terms regarding claims for faulty delivery.6 If despite all applied diligence delivery items show a fault. The foregoing regulation does not stipulate a reversal of the burden of proof for Purchaser. This does not apply in case of fraudulent concealment of the defect. to subsequent performance which may be carried out as elimination of defect or delivery of items free of defects. is served to the best of our knowledge. value added taxes). relating to possible fields of application of our products. 7. 7. The same shall apply in case of commingling. immoderate stress. or trial operation are delayed for reasons attributable to Purchaser or Purchaser is in default of acceptance for other reasons. It is based on our experience and therefore is not guaranteed. Claims because of fault are excluded in case of corrosion damage unless Purchaser pointed out the intended use ANNEX . processing or modification. body or health. we hereby accept assignment. health or liberty nor in case of intended or grossly negligent violation of duty. body. in case of harm of life. 8. infrastructure. Within an adequate respite we are entitled to subsequent performances done twice. no application for opening insolvency proceedings is filed and payment has not been stopped. requisition or other disposals or interventions of third parties.9 Claims of Purchaser because of expenditures for the purpose of subsequent performance.85 5.3 We do not accept liability for our product being apt for a special intention. For securing our claims against the Purchaser Purchaser herewith assigns to us all claims. This applies irrespective of whether dispatch is initiated from place of performance and irrespective of who bears the costs of delivery. mixture or combination.2 This shall not affect the cases where our liability is mandatory by law. risk will be transferred to Purchaser. processed or modified by Purchaser. body or health. in case of intent. Transfer of Risk of the delivery items in connection with special chemicals. 5.1 If the delivery items are sent to Purchaser at Purchaser’s demand. no claims because of fault emerging from such inappropriate maintenance or changes will accrue. particularly in case of violation of duty of the contractual relationship and of tort.

illustrations. 10. regardless of the reasons thereof. 9. illustrations. validity of the other provisions shall not be affected thereby.3 The above duty of secrecy shall survive performance of the contract at hand but shall lapse if and in so far as the information included in the entrusted samples. we are entitled to stop any further activity being in opposition to said rights.2 Any action concerning disputes arising from this contractual relationship shall be taken at the court. Place of Performance – Place of Jurisdiction 12. 10. 11.2 Should infringement of said rights be substantiated to us by a third party. composition. 10. Purchaser will indemnify us from third parties‘ claims on first demand. April 2009. samples etc. 10.1 The Laws of the Federal Republic of Germany shall apply exclusively to this contract.3 Purchaser‘s obligation of release from liability comprises any expenditure we necessarily incur in the context of third parties‘ claims. Title and Copyright 9. Applicable Law 11. or to manipulate delivered items. Severability Clause Should one or several provisions of the contract be or become completely or partly void. or contain a loophole. drawings. in any other way.5 Statute of limitation concerning said claims expires ten (10) years as of conclusion of the respective contract. Mainz. functioning. samples etc. which is competent for our place of business. calculations or other documents and information received. 04 9. calculations or other documents and information has become common knowledge. 9. They shall not be made accessible to third parties without our explicit consent. working or similar.1 Purchaser warrants that production of items according to Purchaser‘s instructions does not infringe third parties‘ rights. illustrations.2 Purchaser is obliged to keep secret all samples. 13.4 Purchaser is not allowed to disassemble the delivery items.1 Place of performance for all contractual duties shall be our place of business. If so. Institut für Mikrotechnik Mainz GmbH . 12. 12. and/or to analyse or to examine or to have analysed delivery items‘.GENERAL TERMS AND CONDITIONS OF SALE 86 foregoing regulation does not stipulate a reversal of the burden of proof for Purchaser. drawings. 9.4 Our claims for damages remain unaffected.. 10. Intellectual Property Rights 10.1 We reserve all copyright and rights of ownership concerning all samples. samples‘ etc. drawings. calculations or other documents and information given to Purchaser.

Hessel. V. Hessel. Löwe. V. „Cost analysis of a commercial manufacturing process of a fine chemical using micro process engineering“. Hessel. Hardt.. V.. Hessel. Hessel.REFERENCES 87 Hessel. 9 (2007) 840-845. Part V. “Microreactor Applications in the Consumer Goods Industry” in „Micro Process Engineering . 22-23 (2005) 4789. Löwe. Eng. C. Chimia 60. „Industrial Microreactor Process Development up to Production“ in: “Microreactors in Organic Chemistry and Catalysis” (ed. Yoshida.. Hessel. 7 -37. A.. Men. Löwe. R. V. D. Grosser. V. Ing. V. S. Renken. Men. Kolb. Schouten. Löb. Schenk. J.. M.. Chem.. Schouten.. V. Yoshida (Eds. 43. V... V. Simoncelli. Sci. J. V. pp.“. 3 (2004) 422-439. Hessel.. Rinke. Serra. C. Hardt. „Determination of the segregation index to sense the mixing quality of scale-up concepts for pilot. Y.. Hessel.. Watts.. Hessel. „Fuel Processing in Integrated Microstructured Heat-Exchanger Reactors“. Hessel. Zapf. G.. Chem. Löb. 4 (2008) 467. Löb. J. Tech. Löwe. J. J. Schürer. Hessel. WILEY-VCH Verlag GmbH & Co. 211-275. Tiemann.. M.. G.... „Nanopowders produced using microreactors“.. G. Chemical Engineering Science 61 (2006) 2959-2967... Vol. J. Schenk.). Kolb. V.. Hessel. Hessel.. Hessel.. Zapf. 2009.. V... Wichert... Jähnisch.. pp. Chemical Micro Process Engineering – Processing and Plants. Hessel. H. H.: Mitsos.-I. H. Löwe... U. P. 44. Eng. N... P. Kinkel. D... H. 77.. Chem. Chimica oggi – Chemistry Today 5 (2004) 10-15.. V. Löwe. 60 (2005) 2479-2501. Hessel. A. H. D. H.. „Volume 3.).C. Jones. V. V. D. Knobloch.. J. Pennemann. Res. Wichert. P. G.. “Chemical Engineering Journal”.. V. Hillmann.. Hessel. Stephan. Tiemann. Pennemann. S. Simoncelli. G. H. Hessel. Energy Environ.. R. T. C.. Chemical Micro Process Engineering – Fundamentals. B. P. Löwe. „Integrated microstructured fuel processors for fuel cell applications“..: Hessel. 2 (2005) 188-192.. H. „Partial oxidation of propane using a micro structured reactor“. J. Hofmann. pp. Schönfeld. Kraut. Löb. 11 (2005) 39-59.. H. Löwe. G. Eng. Eng.. V. Cominos. Hessel.. Löwe. Eng.. Wiley-VCH. Dev. Angew. F. 11 (2004) 1677-1694. J. V. 9. V. Uerdingen. in: Ullmann’s Encyclopedia of Industrial Chemistry. Sci. Ing. 2003. „Review on patents in microreactor and micro process engineering“.. Yoshida. 25 (2005) 9750-9769.... H. Renken... Wiley-VCH.. “Chemical micro process technology – from laboratory scale to production”.. V. P. P. H. Kralisch. M. Res... “Fluorinations.. Jongen. 107. Yoshida. A. V. G. Löb. 1-3 (2005) 205-214.. Tiemann. Weinheim (2004). 22-23 (2004) 4789-4794. C.. 9 “Industrial Microreactor Process Development up to Production“ in: „Micro Process Engineering – A Comprehensive Handbook“ (eds. A. Krtschil. C. H. P. Y. Löb.. Löb. 2009.. V...A Comprehensive Handbook.. 8 (2005) 765-787. H. 2.478. “Ionic liquid synthesis in a micro structured reactor for process intensification”. K. A. Chem. pp. Schmalz. Hessel. H.. U... Guillemet-Fritsch. Ziogas. Löb. J. 98. H. “Chemical Engineering Science”. “Micro mixers – a review on passive and active mixing priciples”.. S. U.. Jähnisch. Chem. Org... Hessel. 85. Hessel. Pennemann. A.. Löwe. Baier. A5 (2006) 1-8. Löb. Löwe.. „Sustainability through Green Processing – Novel Process Windows intensify Micro and Milli Process Technologies“.. V.. Rosenfeld. Löhndorf. 13 The Economic Potential of Microreaction Technology“ in: „Micro Process Engineering . Horn.... K. (2007) Chem. Part III. D.. “Microreactors”.). Bazzanella. J. Müller. Zapf. Proc. V. R. Müller. A. W. Weinheim. Technol.. R. Pennemann. 21 (2008) 51495159... Mazanek. “Org. Hydrogen Energy 33.. 4 (2005) 426-427. J.. Miszczuk.C.. Kralisch. 04 ANNEX . 1 (2007) 198-204. Process 46. 77. Kolb.. V. “Analysis of flow patterns emerging during evaporation in parallel microchannels”. Renken. Hessel. „Microfabrication for Energy Generating Devices and Fuel Processors“ in: „Microfabricated Power Generation Devices“ (eds. V. Proc. P. “Development of microstructured reactors to enable organic synthesis rather than subduing chemistry”.. “Chemical Engineering and Technology”.. Chem.. Weinheim. V. 1-2 (2004) 1-38.. Baerns. V... S. H. Tech. R... 2008. Hessel. Löb.. Y. Löb.. K. S. J.. Modelling and Reactions. Trans.. M.. Zapf. Löwe. V.. Serra. 1 (2008) S242-S246. A. 4 (2004) 406-446. Int. V. Schouten. R. Renken.. B. Cominos. G. Löwe. P. M... Chem.. Ziogas.. Wiley-VCH. Gavriilidis.. C.. K. D. C. Ed. P... Eng. Werner. 135. Encyclopedia of NANOSCIENCE and NANOTECHNOLOGY. Pat. V. P.. V.. G.. J. Pennemann. Chimica oggi – Chemistry Today 25. A. Heat & Mass Transfer 50... Kolb.. KGaA.. M. „Micromixer based liquid/liquid-dispersion in the context of consumer good production with focus on surfactant vesicle formation“. Löwe. „Ethanol steam reforming in a microchannel reactor“. Schilder. 28. D. A. Schouten. Angeli.. “Gas/liquid and gas/liquid/solid microstructured reactors – contacting principles and applications”..A Comprehensive Handbook“ (eds. L.. Hessel. 12 (2006) 1509-1512. Löwe. Int.. Wirth. 9 (2006) 611-617. Intern. Barton. Eng. J. Hensel.. „Impact of fluid path geometry and operating parameters on l/l-dispersion in interdigital micromixers“. Weinheim (1999). H. Haverkamp.. A. Zapf. B5 (2007) 1-6. Al-Rawashdeh. Weinheim. V.. Kralisch. H. 9. Hessel. 6 (2008) 626-633. Kolb....-I. “Use of micromixers to control the molecular weight distribution in continuous two-stage nitroxide-mediated copolymerizations”. 281 – 296. C. “Letters of Organic Chemistry”. (Chapter 22 pp.. M. Schönfeld. 8. H. Hessel.).and production-scale micro structured mixers“.. A. Wiley-VCH. H. Process Safety & Environmental Protection 85.. 2009. Hessel. 287-296. “Direct fluorination of aromatics with elemental fluorine in microstructured reactors”.. „ Volume 3. Kolb. 4 (2005) 479-489. V. H. 1 (2008) 1-16. Pennemann.. chlorinations and brominations of organic compounds in micro structured reactors”.A Comprehensive Handbook”. three-volume edition. H... 9. Löwe.. Kolb. pp.. P.. Jam.. V. IChemE. 83... Sci. G. „Basic study of the adhesion of several aluminabased washcoats deposited onto stainless steel microchannels“.. 185 – 247. Trans. Zapf. K. A. Des. B. Hessel. G. Hessel.. Part B. Pennemann. Brandner. 3 (2007) 26-29. A. Forster. G. Men.. Jähnisch. H. Wiley-VCH. Roberge. Küpper. 1 (2008) S66-S73. J. 2009. Reactions and Applications“. Kolb. 11 (2005) 39-59. M.. Chem. A. V. 1-2 (2007) 226-239. R. J. P.. P. P.. P. Chem. J. Y. 59... 8 (2005) 767779. Wiley-VCH... „A complete miniaturised microstructured methanol fuel processor / fuel cell system for low power applications“.Hadziioannou.4794. H. Löwe. Hessel. V. “Benchmarking of microreactor applications”.-I. D.. V. Hadziioannou. H. Löwe. Rec. Chem. Res.. K. Hofmann. 125. H.).. V. Men. Löwe.. Brochon. “Polymerisationen in mikro-strukturierten Reaktoren: Ein Überblick“. Löwe. Chem. Ind.... H. “Pseudo 3-D simulation of a falling film microreactor based on realistic channel and film profiles“.. V. Hessel. “Microstructured reactors for gas phase reactions: a review”.. 59. M. Hessel. V. P. G.. U... Res. 63. Löwe. Dev. IChemE. Curr. V. Res.. Eng. Wichert. Renken.. 135. H. Tiemann. A. Löwe. Chem. R. Hessel. Chem.. Hessel. Löwe. V. Haswell.. Mevissen.... Power Sources 171. P. Serra. H. G. J. V. Pennemann. Org. Dev. Löb. V. G. Sci. T.-I..: „Micro Process Engineering . G. H. A. Hessel. “Chemistry in Microstructured Reactors”.. Buscaglia. C. S. Eng.. Hessel. Kolb... Eng. Wu. Eng. Hessel. 2009. Löwe.. Löb. C. V.. Dingerdissen. Ehrfeld. 363-401). Chem. 4 (2008) 1374-1382. Weinheim... I. “Organic Process Research & Development”. V. Chem. Chem. Weinheim (2005). Kolb. Part A. Eng. Hessel.. Proc. V. H. „Polymerisationen in mikro strukturierten Reaktoren: Ein Überblick“ . J. H. Schürer. V.. Hadziioannou.. Klefenz. 1.. Löwe.: Hessel. 7... H. J. Eng.. 29. Krtschil. Hessel. Krtschil. Fluorine Chem.. V. Kreisel. R. Volume 2: Devices. Hessel. D.

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imm-mainz.de Status 05/2009 .de www.205 catalogue@imm-mainz.0 Fax: +49 61 31 / 990 .For further questions please do not hesitate to contact us: Institut für Mikrotechnik Mainz GmbH Carl-Zeiss-Straße 18-20 55129 Mainz Phone: +49 61 31 / 990 .