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T H E C ATA L O G U E

> chemical micro process technology made by imm

5/09

P R E FA C E

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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 diversied, but also refocused offer of microstructured reactors and their processing plants. All ears on benet 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. IMMs micro process technology ever since is truly devoted to real-life applications in the eld 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 users 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 IMMs 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.

P R E FA C E

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Branch and whole tree Process intensication 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 ve 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 prolic soil on no mans 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 IMMs new research and development directions. Although not all of these have already been solidied 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 purication processes suited to continuous ow New heating concepts (microwave) and solventless/-free processing (ionic liquids; supercritical uids) 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 intensication 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 elephants 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 fr Mikrotechnik Mainz GmbH

CONTENTS
> superior products made by imm

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, Yellow 12 Hydrogenation of nitrobenzene Direct uorination of toluene with elemental uorine Sulphonation of toluene Direct hydrogen peroxide synthesis out of the elements [4+2] cycloaddition of singlet oxygen to cyclopentadiene to make cyclopentene-1.4-diol Side-chain photochlorination of toluene-2.4-di-isocyanate 02 Plants Contents Organic Synthesis Plant Impinging-Jet Microreactor Plant for Precipitation Reactions Cream and Emulsication 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

TESTING AND QUALITY CONTROL

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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. This catalogue makes the rst move to bring novel and highly innovative products for chemical micro process engineering to the customer. IMM regards such off-the-shelf delivery as indispensable to enable a technological break-through. The catalogue comprises both off-theshelf products and demonstrators that are ready for supply according to customers needs. IMM is aware that despite the novelty of the devices, they have to full the demands of industrial processing. For this reason, we do not only invest in scientic and technological promotion of our devices, but also in quality control, improvement of robustness, supplying proper uid connections, etc. First of all, our Quality Assurance policy is realised by a Quality Management System certied according to DIN EN ISO 9001. For reasons of transparency the following specic technical quality features are given additionally on the backside of each micro devices description in the catalogue: Specications Options Performance Data Applications & References tion channel platelets made of various materials, or incorporation of specialty functions (e.g. of an inspection window). For this reason, devices are regularly controlled by inhouse leakage rate tests. IMM thereby applies known and recommended procedures for leak testing of large-scale apparatus which are modied to the needs of microow devices. The setting of these tests orients on ASME and EU standards on leakage testing. If needed, leak tightness will be measured at elevated pressures and temperatures. The result will be expressed in the well-established way to classify leakage classes, e.g. as L0.01. In selected cases, more data are summed up in a graph in our assembly manual.

Delivery Time As we know, you do not have much time until you need to set work on your measurement or processing. 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.

Performance Data Performance Data include information on temperature and pressure stability, leakage rates, applicable ow rates, residence times and more, all based on experimental evidence. This enables you to judge whether the device meets basic requirements of the process or not. Said data are supplemented by geometric parameters comprising information on internal volumes or surfaces, in absolute terms or as specic properties. In addition to these basic, material- and construction-based parameters, more detailed information on processing is given, including description of hydrodynamics such as ow patterns or interfacial areas for selected parameter sets. Reaction engineering data such as conversions or space-time yields may be given as well. Any further information that is relevant and not included for reasons of limited space is referred in Applications & References. From all these contents of Performance Data, three presently important aspects are exemplarily discussed more in detail below.

Performance characterization IMM aims at disclosing the functioning of its devices largely as well as at showing their limits. Our devices can act as multi-purpose tools for a diversied range of applications. The information on these applications result from own or by partners practised chemistry as well as disclosed customer processes. Beyond multi-functionality, we identied application-unique uses for the micro devices and, vice versa, produce more and more custom-designed tools. Their functioning indeed can be thoroughly characterised and must be benchmarked to known apparatus and techniques. In this context, IMM runs several test set-ups, e.g. to characterise mixing, heat exchange, evaporation, and reaction processing. Besides such in-house testing, the rst basic versions of the devices were usually tested by partners or third parties being experts in the eld of the micro devices application. This particularly provides an independent assessment either from the industrial or scientic point of view concerning the performance of the devices. The results are documented in many peer-reviewed publications which are referred in the respective devices description.

Specications This is your guideline for your check on material compatibility and t into existing environment (e.g. by comparing outer dimensions). Relevant dimensions are listed here.

Options Since different customers have different demands on how a reactor might t best to their intended application, materials, internal dimensions or simply uidic peripherals may need to be changed. IMM tries to serve such demands on customized solutions. For instance, we typically offer a variety of, e.g. different uid connectors, reac-

Leakage rate tests Our devices meet the requirements of complex, detailed analyses and should not only be suited for making snapshots on feasibility. Here, leak tightness at the best possible rate is absolutely essential for correct balancing of all streams and avoiding contamination of the environment.

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

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are considered to comprise the essential information for the customer. In this context, we would like to point out that IMM was the rst to suggest an advanced mixing test procedure for ow-through devices (besides simple visual inspection of colouring/ neutralisation) by modication of an approach used for batch apparatus originally, developed by the Villermaux group in Nancy, France (Ind. Eng. Chem. Res. 38, 3 (1999) 1075-1082). IMM uses the chemical protocol described by S. Panic et al. (Chem. Eng. J. 101 (2004) 409-419). In the following the concentrations and preparation of the two solutions, pumped in the experiments at a volumetric ow rate ratio of 1:1 is given: Solution 1: A sulphuric acid solution with c(H2SO4) = 0.030 mol/L. Solution 2: A solution of KI, KIO3, NaOH, H3BO3. 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) = 0.0319 mol/L c(NaOH) = 0.0909 mol/L c(H3BO3) = 0.0909 mol/L Solution 2b: c(KIO3) = 0.00635 mol/L c(NaOH) = 0.0909 mol/L c(H3BO3) = 0.0909 mol/L

Experimental Determination of Mixing Performance of Microuidic Devices by the Villermaux/Dushmann method Mixing has a decisive impact on the overall performance of microreaction processes. A large number of micro mixers using different functional principles is available in the meantime. Therefore, there is an increased need for measuring and comparing mixing performance. IMM tests its micro mixers with regard to mixing performance experimentally using the so-called Villermaux/Dushmann method. The determination of mixing performance by the Villermaux/Dushman method is based on the competition of two parallel reactions. 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. Relevant chemical formulas: + H2BO3 + H H3BO3 (very fast) + 5 I- + IO3 + 6 H 3 I2 + 3 H2O (fast) I2 + I- I3(detectable by UV/Vis spectroscopy) In the experiments a buffered solution of KI/KIO3 is mixed with diluted sulphuric acid. In case of ideal mixing the acid is only consumed by the fast neutralisation. However, if mixing is less ideal iodine is formed by the comproportionation reaction. The formed iodine can be then detected as triiodide complex by UV-Vis spectroscopy with absorption band centred at 286 and 353 nm. The more iodine is detected the less ideal is the mixing perfomance.

Applications & References Information that is missing in the product sections might be found in the citations. You can be sure that the list of citations comprises the latest and most relevant information available on IMMs micro devices. Means, we limited this list to most relevant books and reviews.

PROCESSES

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CONTENTS
> processes made by imm

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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, Yellow 12 Hydrogenation of nitrobenzene Direct uorination of toluene with elemental uorine Sulphonation of toluene Direct hydrogen peroxide synthesis out of the elements [4+2] cycloaddition of singlet oxygen to cyclopentadiene to make cyclopentene-1.4-diol Side-chain photochlorination of toluene-2.4-di-isocyanate 23 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22

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KOLBE-SCHMITT SYNTHESIS

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Motivation and Results

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Low pressure operations under reux conditions are typically favored for laboratory asks and agitated tanks. Accordingly, the maximum temperature of many organic routes is often simply dened by the solvent boiling point. Micro reactor rigs on the other side allow a simple operation of liquid phases under high pressures and high temperatures. For instance, a system pressure of 50 bar is enough to maintain single-phase operation (i.e. no gas content and no boiling) even at temperatures up to 100C higher than boiling points of typical solvents. This has been termed high-p,T processing. The faster operation at higher temperatures typically is paid by more side and consecutive

reactions. Thus, efcient mixing and shortening of residence time to the kinetically limit become important drivers for process optimization. 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. This benet is counterbalanced by thermal degradation of the reactants and the products, in particular by decarboxylation of the 2,4-dihydroxy benzoic acid (see scheme below) and 2,4,6-trihydroxy benzoic acid.

Applied Process Parameters


Pressure: 40 80 bar Temperature: 100 220C Reaction time: 4 390 s

Benets through Process Intensication


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

MICHAEL ADDITION

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The merit of high-p,T processing (see initial chapter and under Kolbe-Schmitt synthesis for denition) was investigated for six Michael additions of two ,-unsaturated carbonyl compounds and three amines. 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). In addition, effects of higher temperature are given, since the reaction is carried out at much higher temperatures than the boiling points of the amines. For example, for the diethyl amine with a boiling point of -55C, best operation was at 100C, while the experiments were extended up to 200C. Reaction times and consequently space-time yields were reduced by order of magnitude in this way. Yields of up to 99% at about full selectivity were achieved.

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Applied Process Parameters


Pressure: 3 20 bar Temperature: 20 90C Reaction time: 2 30 min

Benets through Process Intensication


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

S O LV E N T- F R E E T H I O P H E N E B R O M I N AT I O N

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Motivation and Results

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In batch processing aggressive reactants typically are diluted to prevent thermal overshooting and runaway. Even then they often are added slowly drop by drop to allow heat transfer to be adjusted to heat release. In some cases, this may take a long time, up to hours. 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). On the contrary, microstructured reactors with their efcient heat and mass transfer have the potential to contact the full reactant load all-at-once. In addition, micro reactors can cope with concentrated solutions or even pure liquid reactants. There are several examples known that such all-at-once or solvent-free procedures are feasible in micro reactors with reasonable selectivity, whereas the same contacting led to vigorous reactions and even explosions (when done under special safety precautions with miniature volumes).

The bromination of thiophene investigated used pure thiophene and pure bromine ows at temperatures from -10C to room temperature. The micro reactor operation led to yields of 2,5-dibromothiophene up to 86%, at nearly complete conversion, which is better than for home-made (77% yield) and literature (50% yield) batch processing. Using the pure feeds and higher temperature, the reaction time was decreased from about two hours (for batch) to less than one second (for micro mixer reactor). Correspondingly, the space-time yields were by order of magnitude higher for the continuous micro reactor process. Due to the easiness to change reactant ratios and temperatures in the micro reactor rig, a fast parametric study could be done for nding optimal operating conditions.

Applied Process Parameters


Pressure: 1 bar Temperature: -10 0C Reaction time: A few ms

Benets through Process Intensication


Continuous process with exible output at constant selectivity of 80% Use of pure bromine, decomposed at the spot Simple control over substitution degree

SYNTHESIS OF AN IMIDAZOLE-TYPE IONIC LIQUID

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PROCESSES

Motivation and Results


A variant of the novel chemistry concept is to use solventfree processes with aggressive reactants which exhibit heattransfer sensitivity. The exothermic synthesis of an ionic liquid was carried out in this way in a micro reactor rig, and addresses especially the need for temperature control during the reaction, 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 challenge is further increased by favourably working without any solvents which is expected to result in temperature increase. The chemistry cannot be disclosed due to intellectual properties rights of the industrial user. Even under the advanced thermal control of a microstructured reactor, one can observe for a thermostat temperature of 50C an increasing yellow colouring of the product, i.e. the formation of unwanted side products. This nding, however, can be explained by looking at the determined temperature proles. Obviously, the reactor or the selected dimensions are not capable of removing reaction heat in a sufcient manner. In order to improve heat removal for the higher ow rates, an approach was to use ner structures, e.g. 1/16 tubes instead of 1/8 tubes. The smaller tubes, however, impose an increase of pressure drop which may become a limiting operational parameter. Therefore, the determination of temperature proles 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. As can be seen from the temperature proles, the heat removal capacity of the 1/8 tubes is sufcient in large parts of the reactor, e.g. for a total ow rate of 3.48 ml/min beginning at a reactor volume of 15%. In the following, therefore the rst two reactor sections where exchanged by 1/16 tubes with same internal volume as the replaced 1/8 tubes. Exemplarily, the obtained temperature proles with such a set-up for a total ow rate of 3.48 ml/min are given in Figure 7 with the corresponding prole of the set-up with all 1/8 tube sections as comparison. The maximum temperature rise above thermostat temperature was reduced from 50C to 10C with this reactor modication, yielding a clearer product. For the highest ow rate (6.96 ml/min) the modication did not prevent hot spot formation, since a good portion of the reaction is occurring after the rst two tube sections and therewith not affected by smaller dimensions in the rst two tubes. With regard to production purposes based on these experimental results an adapted reactor concept for higher ow rates was derived. The micro reactor consists of a stack of platelets and heat removal is improved by integration of microstructured heat exchangers. The testing is now in preparation. Furthermore, 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.

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Applied Process Parameters


Pressure: 1 bar Temperature: 50 60C Reaction time: 1 4 min

Benets through Process Intensication


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 exibility 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

PHENYL BORONIC ACID SYNTHESIS

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Motivation and Results

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Mixing sensitivity is particularly pronounced for the class of organometallic reactions. Often these reactions are carried out under cryogenic conditions to get acceptable yields. This can be changed when using microstructured reactors. In this way, the phenyl boronic acid synthesis from phenyl magnesium bromide could be performed at high selectivity

even at room temperature. The yield was raised by about 25% as compared to the industrial batch production process. Energy savings are both given by shifting the former cryogenic process to room temperature and by achieving a highly pure crude product, thereby rendering the former energy-consumptive distillation step unnecessary. Thus, having higher selectivity did not only affect the reaction itself, but also downstream purication.

Applied Process Parameters


Pressure: 1 bar Temperature: 50 60C Reaction time: 6 120 s

Benets through Process Intensication


Increase of yield of pure product by 25% Decrease of impurity level of crude product by factor 5, from 5% to 1% Process simplication: Eliminating the distillation step Favourable room temperature operation instead of cryogenic one Better costing of micro reactor process: Less invest (no distillation column), less energy consumption, less waste disposal

(S)-2-ACETYL TETRAHYDROFURAN SYNTHESIS

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PROCESSES

Motivation and Results


In the (S)-2-acetyl tetrahydrofuran (ATHF) synthesis, the Grignard reagent MeMgCl is very reactive and not easy to handle in large scale. The Grignard reaction can not only cause safety and hazardous problems at industrial scale, but there are also issues of chirality conservation. The -hydrogen of the starting material is unstable under basic conditions, and consequently, racemization may occur. The optical purity of the micro reactor product was 98.4% as compared to 97.9% at batch level. Further, there are selectivity issues, i.e. an over-alkylation to tertiary alcohol must be avoided. Also, the individual impurity level must be less than 0.2%. The micro reactor impurity was 0.18% by minimization of back-mixing, while the batch impurity was 1.56%. Accordingly, with ne thermal and ow control, the productivity and economics of this process are increased.

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Individual impurity Batch MRT 1.56% 0.18%

Optical purity 97.7% 98.4%

Applied Process Parameters


Pressure, Temperature, Reaction time: Not disclosed

Benets through Process Intensication


With ne thermal and ow control, the productivity and economics are increased Minimizing back-mixing during reaction reduces impurities by factor 8, from 1.56% to 0.18% Chirality conserved during reaction

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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, including tube reactors, static mixers and a microstructured reactor, were tested for the synthesis of an intermediate to yield a quinolone antibiotic drug, named Gemioxacin (FACTIVETM). Among several types of reactors investigated, the microstructured reactor was successfully applied to the synthesis of a pharmaceutical intermediate via a fast exothermic Boc protecting reaction step. The reaction temperature was isothermally controlled at 15C. By using the microstructured reactor the heat of reaction was completely removed so that virtually no byproducts were produced during the reaction. Conversions as high as 96% were achieved. The micro reactor operation can be compared with other reactors, however, which need to be operated at 0C or -20C to avoid side reactions.

Applied Process Parameters


Pressure: 1 bar Temperature: 15C Reaction time: Not disclosed

Benets through Process Intensication


Micro reactor was the best out of 5 different reactor concepts, including conventional tube reactors and Kenics static mixers, with the gures of merit being maximal yield and temperature close to ambient 97% yield

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

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A continuous nitro glycerine pilot plant with microstructured mixer/multi-tube reactors was installed at Xian site in China and was operated at a production rate of 15 kg/h nitro glycerine meeting all specs. A rough calculation for annual throughput gives a production rate of nearly 130 metric tons per year. Taking all reactants, i.e. fuming nitric acid, oleum and glycerine into account the total annual throughput is in the range of 900 cubic meters. The main challenge for such kind of plant is to ensure safety for all, even worst operational conditions. Therefore, all reactants must be pre-cooled before entering the microstructured mixer. Also the mixer itself is actively cooled by means of an integrated heat exchanger as well as the multitubular reactor. Advanced simulations were made to solve the problems with equipartition volume ow through the multi-tube reactor and some new, specic micro-macro interconnects for uid-ow guidance were developed and integrated. The plant is comparably small and thus, the necessary space for the plant in a safe environment, e.g. a bunker, can be reduced. The manufactured nitro glycerine will be used as medicine for acute cardiac infarction. Therefore, the product quality must be on highest grade, and the test runs indeed revealed higher selectivity and purity. The plant could be operated safely; one of the next targets is to have it fully automated. As a second step, a plant for downstream purication by washing and drying the nitro glycerine, of notably larger size and complexity as the reactor plant, is going to be developed and currently under negotiation. Environmental pollution should be excluded by advanced waste water treatment. In a nal stage, the micro reactor nitro glycerine plant may also encompass formulation and packaging.

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Applied Process Parameters


Pressure: 1 bar Temperature: 30 40C Reaction time: Some min

Benets through Process Intensication


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

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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, high-pressure (high-p,T) side-chain bromination of alkylaromatics. The transformation from batch to continuous processing, the safe operation with bromine at temperatures over 170C and the decrease of reaction time, respectively increase of space-time yields, were drivers for the development here. Molar ratios of bromine to m-nitrotoluene ranging from 0.25 to 1.00 were applied. The reactants were contacted in an interdigital micro mixer followed by a capillary reactor. At temperatures of about 200C nearly complete conversion is achieved. The selectivity to the target product benzyl bromide is reasonably high (at best being 85%; at 200C and higher being 80%). The main sideproduct formed is the nitro-substituted benzal bromide, i.e. the two-fold brominated side-chain product.

Applied Process Parameters


Pressure: 15 bar Temperature: 170 230C Reaction time: 2.6 min

Benets through Process Intensication


Process simplication: 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,T operation Quenching of non-reacted bromine on-line and instantly after use

SYNTHESIS OF AN AZO PIGMENT DYE, YELLOW 12

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PROCESSES

Motivation and Results


By the use of microstructured mixers, pigment and other particle syntheses can be improved, since the well-dened and predictable mixing improves the preparation all the way from seed generation until particle agglomeration. In this way, ner particles with more uniform size distribution were yielded for the commercial azo pigment Yellow 12. 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, lower contents of the costly raw material in the commercial dye products can now be employed which increases the protability of the pigment manufacture.

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Applied Process Parameters


Pressure: 1 2 bar Temperature: 20C Reaction time: A few s

Benets through Process Intensication


Benets through process intensication Increase of glossiness by 73% and Increase of transparency by 66% Better costing, since less raw material has the same effect Easy scaling out of powder synthesis, which otherwise may be complex

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

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Motivation and Results

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The hydrogenations of nitro aromatics have high intrinsic reaction rates, 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 ). For this reason, the hydrogen supply is restricted, thereby controlling reaction rate. Otherwise, decomposition of the nitro aromatics or of partially hydrogenated intermediates can occur. The hydrogenations of nitro benzene over supported noble metal catalysts were investigated in a microstructured falling lm micro reactor. For nitrobenzene hydrogenation, the overall mass transfer coefcient kLa was conservatively estimated (based on the lm thickness in the middle of the channels) to be in the -1 range 3 8 s . As a comparison, for intensied gas liquid contactors kLa can reach 3 s-1, but for bubble columns and -1 agitated tanks it does not exceed 0.2 s . A wide variation of preparation procedures for the palladium catalyst was tested. A sputtered palladium catalyst exhibited low conversion and large deactivation of the catalyst (60C; 4 bar). The corresponding selectivity was also low. A slightly better performance was obtained after an oxidation / reduction cycle. Following a steep initial deactivation, the catalyst activity stabilised at 2 4% conversion and at about 60% selectivity. After reactivation, selectivity

approached initially 100%. As side products, all intermediates except phenylhydroxylamine were identied. For a UV-decomposed palladium catalyst, a conversion was found slightly higher than for the sputtered one. A similar spectrum of side products as for the sputtered catalyst was given. For an impregnated palladium catalyst, complete conversion was achieved and maintained for six hours. Selectivity decreased with time, but remained still at a high level. The best performance of all catalysts investigated was found for an incipient-wetness palladium catalyst. Having initially more than 90% conversion, a 75% conversion at selectivity of 80% was reached for long times on stream. The catalyst life-time or the four types of catalysts, prepared by different preparation routes, depends on the catalyst loading which is related to the preparation route. The larger the loading, the longer the catalysts could be used before reactivation. 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. In this way, initial activity was recovered, thus regaining complete conversion.

Applied Process Parameters


Pressure: 1 4 bar Temperature: 60C Reaction time: 5 20 s

Benets through Process Intensication


One of the rst g-l-s processes reported in microstructured reactors Process not benchmarked in detail to batch ones

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

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PROCESSES

Motivation and Results


One way of process simplication is to make molecular complex compounds out of much simpler building blocks (e.g. by multi-component one-pot syntheses like the Ugi reaction), at best directly out of the elements. Especially in the latter case, this is often quoted as dream reaction. Typically, such routes have been realised so far from hazardous elements, easily undergoing reaction, but lacking of selectivity. One example for this is the direct uorination starting from elemental uorine which was performed, e.g., with toluene. Since the heat release cannot be controlled with conventional reactors, the process is deliberately slowed down. While for this reason the direct uorination needs hours in a laboratory bubble column, it is completed within seconds or even milliseconds when using a miniature bubble column, operating close to the kinetic limit. Favourable electrophilic substitution is achieved, showing that unselective radical paths are largely absent. The overall selectivity of this non-optimised process amounts to about 25%, not far from the total selectivity of all the Balz-Schiemann steps to achieve the same result. Waste reduction is less since a single step synthesis is undergone. Productivity is much higher, as demonstrated by the order of magnitude larger space-time yields.

01

Applied Process Parameters


Pressure: 3 20 bar Temperature: 20 90C Reaction time: 2 30 min

Benets through Process Intensication


Reduction of reaction time up to ~ 1000 Increase in space-time yield by factor 10,000 Increase in productivity by factor 5 Single-step operation replaces tedious Balz-Schiemann route Less waste generation Less reactor investment and process simplication

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 40C using a microstructured heat exchanger while at the same time liquid sulphur trioxide is heated up to 60C in order to evaporate it. 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. Thus, a gas stream is allowed to ow through to a microstructured reactor where it reacts with the liquid toluene. As shown in reaction (1), sulphonic acid is produced here via the desired reaction step. At the same time, though, sul-phone (reaction (2)), a mixed anhydride and sulphonic acid anhydride are also formed by side reactions. Sulphone cannot be converted further but the mixed anhydride reacts in the residence time module with toluene and forms the desired product, sulphonic acid, as shown in reaction (3). To convert the sulphonic acid anhydride to sulphonic acid, a hydration step is required (reaction (4)). To achieve this, water is added to the reaction mixture after the residence time module. Up to date, the reaction has been carried out up until the residence-time module. The nal hydration step has not

taken place. Even so, rst results are encouraging. In order to evaluate reaction conditions, the mole ratio of the two reactants, sulfur trioxide and toluene, was varied and the selectivity of the desired product (sulfonic acid) and of the by-products (sulfon and the anhydride mixture) was determined. Evidently, with increasing SO3/toluene mole ratio, the selectivity of the undesired by-products decreases while the selectivity of sulfonic acid stays nearly constant. At a mole ratio of 13/100, 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 1.3%. The isomer selectivity was also determined to be 8.1% for the ortho-sulphonic acid, 1.5% for the meta-sulphonic acid and 90.4% for the para-sulphonic acid. From literature, at a SO3/toluene mole ratio of 13.4, the selectivity of the orthosulphonic acid was 17.6%, of the meta-sulphonic acid 1.2% and that of the para-sulphonic acid was 81.2%. Thus the improvement of the selectivity for the para-sulphonic acid can already be seen from these results. Very recently also the last hydration step was executed successfully.

Applied Process Parameters


Pressure: 1 bar Temperature: 40C Reaction time: 5 15 s

Benets through Process Intensication


One of the rst complex micro-ow process designs for a multi-step synthesis Better para-isomer selectivity

DIRECT HYDROGEN PEROXIDE SYNTHESIS OUT OF THE ELEMENTS

21
PROCESSES

Motivation and Results


Several examples were reported for conducting routes in the explosive regime. Among them and most prominent was the detonating-gas reaction, using pure hydrogen and oxygen mixtures. This stands for a direct route from the elements. With special catalysts hydrogen peroxide, and not water, is obtained as value product, avoiding the circuitous Anthraquinone process, used at industrial scale. Calculations of explosion limits clearly demonstrate that there is a considerable shift, when explosive reactions are carried out in micro channels. The safety is not only related to avoiding thermal runaway, but relates to mechanistic reasons by breaking the radical chain by enhanced wall collision in the small channels with their large specic interfaces. Using this direct route to hydrogen peroxide, basic engineering for a new site for the production in the order of about 150,000 t hydrogen peroxide per year was done by UOP. Pilot processing and economic calculation of the production process has been performed. Based on microstructured mixing units, the new process is realised by direct contacting of hydrogen and oxygen (without inert gas) in the presence of a heterogeneous catalyst. The key to a high selectivity is to have a noble-metal catalyst in a partially oxidised state. Otherwise, only water is formed or no reaction is achieved. Peroxide testing at IMM used such a hydrogen peroxide selective catalyst placed within a mini-trickle bed reactor equipped with a micro mixer. Using UOP process specs, a space-time yield of 2 g hydrogen peroxide per g catalyst was achieved which exceeds literature values. In addition, operation at only 20 bar, considerably lower than for the published processes, and usage of smaller oxygen/ hydrogen ratios, saving valuable raw materials, is given. It could be clearly shown that improved selectivity and conversion is given at explosive oxygen/hydrogen ratios. 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. A selectivity as high as 85% at 90% conversion was achieved so far (oxygen/hydrogen ratio of 1.5 3).

01

Applied Process Parameters


Pressure: 30 bar Temperature: 50C Reaction time: A few s

Benets through Process Intensication


Reduction of system pressure by factor 4, from 120 to 30 bar Increase in space-time yield by 25%, from 1.5 to 2.0 g h/gcat Favourable decrease in oxygen to hydrogen ratio by factor ~ 4, from 6.8 to 1.5 (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

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-1.4-DIOL


Motivation and Results
This reaction of industrial interest utilises singlet oxygen generated by irradiation in the presence of Rose Bengal. An endoperoxide is formed as intermediate which is converted to 2-cyclopentene-1.4-diol by reduction with thiourea. Due to the small length scales in micro reactors, e.g. 50 m, high concentrations of a sensitizer may be used. As these materials typically have high costs, recycle loops with low inventory can be employed to consume only a low overall amount of sensitizer. The sensitizer absorption, despite the large molar extinction coefcient, is not over the tolerable limit since only small optical paths are employed. It is assumed that molecules in thin liquid layers face a broadly similar photon ux, unlike macro-scale photo processing. Low-intensity light sources should give efcient irradiation of thin liquid layers. Sample heating is reduced and so is radical recombination. In addition, oxygen-enrichment of solutions before and after micro reactor passage can be handled differently and is no longer a major safety problem. For the oxidation of cyclopentadiene by singlet oxygen to 2-cyclopentene-1.4-diol a yield of 19.5% was found. The feasibility of safely carrying out the oxidation of cyclopentadiene by singlet oxygen to 2-cyclopentene-1.4-diol was demonstrated. The explosive intermediate endoperoxide was generated and without isolation used on-site for a subsequent hydration reaction.

Applied Process Parameters


Pressure: 1 bar Temperature: 0 15C Reaction time: 5 20 s

Benets through Process Intensication


High quantum efciency 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

S I D E - 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 - 2 . 4 - D I - I S O C YA N AT E

23
Side-chain photochlorination of toluene isocyanates yield important industrial intermediates for polyurethane synthesis, one of the most important classes of polymers. The motivation for micro channel processing stems mainly from enhancing the performance of the photo process. Illuminated thin liquid layers should have much higher photon efciency (quantum yield) than given for conventional processsing. In turn, this may lead to the use of low-intensity light sources and considerably decrease the energy consumption for a photolytic process. Due to the planar layer structure of most micro reactors a uniform illumination is yielded in addition, which can be kept when increasing throughput by numbering-up. Here, the individual reaction units are assembled in parallel again on a plane, only a larger one. By using a nickel plate, space-time yields up to 401 mol/(l h) were achieved in the Falling Film Micro Reactor. Control experiments in a batch reactor at 30 min reaction time resulted in a space-time yield of only 1.3 mol/(l h), hence are by orders of magnitude smaller. By using an iron plate, spacetime yields up to 346 mol/(l h) were achieved in the Falling Film Micro Reactor. Conversions from 30% to 81% at selectivities from 79% to 67%, respectively yields from 24% to 54%, were found when using a Falling Film Micro Reactor (4.8 13.7 s; 130C). 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 having a selectivity which is higher by about a factor of 2.

01

Applied Process Parameters


Pressure: 1 bar Temperature: 130C Reaction time: 5 15 s

Benets through Process Intensication


High quantum efciency Increased selectivity, 79% instead of 45% for batch Increased conversion, 81% instead of 65% for batch Increased space-time yield by two orders of magnitude, 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

PLANTS

24 02

CONTENTS
> plants made by imm

25

Plants Organic Synthesis Plant OSBP Impinging-Jet Microreactor Plant for Precipitation Reactions IJMP Cream and Emulsication 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

ORGANIC SYNTHESIS PLANT


O SB P

26 02

OSBP for 2-step reaction

Principle
In micro reactor literature, 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. It is based on the reliable hybrid concept of IMM, utilizing innovative micro reactor components in connection with well-proven conventional small-uidic equipment. IMM has gained huge experience with carrying out organic reactions e.g. ethoxy silylations, metal-organic syntheses, and epoxidations in such micro mixer/tube reactor bench-scale units. As a result this unit concept was developed and tested to yield the bench-scale unit actually offered now. It comprises two pre-heating loops (as option: microstructured heat exchangers), a micro mixer, a 5/2-way valve, 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. On demand, the general bench-scale unit concept can be modied towards more complex design. The concept is amenable to supercritical processing as well.

OSBP for single-step reaction (top view)

OSBP for single-step reaction (inside view)

27

Typical ow 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 0.05 2.5 for mixer SIMM-V2 2.5 30 for mixer CPMM-V1.2-R600/12 4 changeable delay loops have a different length of approx. 1%, 5%, 20% and 100% (the absolute lengths will be adjusted to the applied mixer to yield reasonable residence times) L0.1

Further Applications
Based on the IMM knowledge on general demands for a chemical synthesis plant, this basic set-up was designed. Though it should be directly applicable for many typical (organic) syntheses i.e. for gas/liquid or liquid/liquid mixing homogenuously or dispersing (emulsions, foams), even catalyst slurries might be processed. If the standard version is not sufcient, it might be differentiated and/or extended where needed, e.g. for multi-step processing. Insofar, this set-up represents a versatile tool to directly enter into micro chemical process engineering.

02

Leakage Class

Specication 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, 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 ts into a heating bath

Options
Temperature and pressure measurement unit Pumping units Process control unit, programmed in LabView Other materials on request

Pilot-scale plant for nitro glycerine production

PLANTS

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 ow 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. The delay loop was removed and the remaining blocking sensitive part, the mixer, substituted by the simplest nonfouling component for continuous mixing-processing, the Impinging-Jet Micromixer IJMM. Educt streams are tempered via two microstructured heat exchangers HX204 before entering the mixer, enabling a fast and efcient temperature control. The overall pressure and temperature stability is mainly limited by the windows and gasket of the mixing chamber. The position of the IJMM in the mixing chamber can be adjusted in the vertical direction which allows best tting connection of an outleaving (reaction) tube downstream, in case the mixing section tends to spraying causing contamination of the mixing chamber. Additional (inert) gas ushing is integrated. Another option is to use the Separation Layer Interdigital Micromixer SLIMM instead of IJMM to carry out precipitations.

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 ows the exact mass ow regulation with gear pumps and balances as well as measuring and controlling their inlet temperature into the mixing chamber. Besides complete data acquisition including system pressure this LabView-based system can run given programs (e.g. overnight experiments) easily compiled with the integrated program editor. The collected data are as ASCII-les easily importable e.g. into Excel for further use.

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 (m) Options Impinging-Jet Microreactor Plant IJMP main part depicted left: approx. W 50 cm x H 80 cm x D 30 cm 1/4 / 1/4 Housing, mixer: 1.4571 Glass depending on used mixer, typically for IJMM: 350 m diameter Other materials like Hastelloy, Monell or Titan on request

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) -200 C to + 250 C @ 1 bar 0 - 40 bar @ 25 C depending on used mixer, for IJMM-350 e.g. 1.4 3.0 l/h watery ow

The LabView-based process control system for the IJMP

PLANTS

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, placed in a ask or vessel and then vigorously stirred or homogenised with high energy consumption. Micromixers insofar proved in literature to reduce energy input by factor 10. Besides, 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. Further taking the advantage of small hold-ups despite the pilot-scale productivity, a versatile tool concept is offered herewith enabling even a fast change of cream recipes within less than a minute. Respectively, a multitude of different pastes, creams, lotions within short time can be produced as samples or in larger amounts. The CSBP-Demonstrator is based on the reliable hybrid concept of IMM, utilizing innovative microreactor components in connection with wellproven conventional small-uidic equipment. Respectively, small gear ring pumps for max. to 1 15 l/h depending on type and 140C 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. The 4 solid components can be fed via temperature-controlled heated funnels into tempered ask whereof being pumped, enabling a full continuous processing even in case of production need. The liquids are heated up with simple heating loops, bath-fed or electrically driven heat exchangers depending on total ow rate need. The general bench-scale unit concept can be modied towards more complex design. The concept is amenable to unusual processing as well.

Cream Plant positioned on a holder for easy maintenance, cleaning and device exchange

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 2.5 60 L0.1

Specication 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 ts into a heating bath

02

Options
Temperature and pressure measurement unit Process control unit, programmed in LabView Other materials on request

Array of 3 CPMM to mix 4 components nearly at once, 4CCPM, ca. 3-60 l/h

Seven CPMM structures to mix 8 components, of PMMA, 8CCPM

Special StarLaminator10, to mix 3 components at once, ca. 5-80 l/h

PLANTS

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 benet from the outstanding properties of microstructured devices, especially concerning heat transfer and mixing. Mainly for ne 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, angeable 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 sufcient 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.

Conguration 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 conguration 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()

3.5 3.0 2.5

F ()

2.0 1.5
E()

0.4 0.2 0.0 0.0 0.5 1.0 1.5 2.0

1.0 0.5 0.0

=t/[-]

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

E()

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 ow controller for the gas ow, a cryostat, a supply- and a withdraw-pump for the liquid ow. 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 modied towards more complex design. Operation in the Falling Film Microreactor device can be performed up to 300C 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 ow 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 ow rate by using isopropanol and a channel size of 1200 m x 600 m 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

Specication 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 borooat 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 (m) Options

Options
Mass ow controllers Temperature and pressure measurement unit Process control system

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

Residence time (s) Liquid lm thickness (m) 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 ow velocity, and gas composition. The bench-scale unit comprises commercial mass-ow controllers for control of the gas feed, ame arresters to stop ame 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 900C 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 conned 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 modications can be arranged.

37
In conjunction with bench-scale unit construction, IMM services include provision of a manual which contains, besides general information, detailed documentation on experiences gained with operation of this bench-scale unit. Exemplarily, operational modes are given so facilitating the rst experimental steps when starting bench-scale unit operation. In case of further questions and desires, an IMM contact person can be consulted by mail or phone. By special request, a process parameter monitoring program based on the LabView software can be supplied that allows automatic acquisition of temperature and pressure data. The bench-scale unit was in detail investigated not only for numerous steam reforming and partial oxidation reactions of alcohol and hydrocarbon fuels, but also for CO clean-up such as water-gas shift, preferential oxidation and methanation. Besides constructional changes in the set-up, this requires the coating of another catalyst. 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. 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 modications of the bench-scale unit construction. Here, information on the exact process desired is required from the customer and a special offer will be prepared by IMM. The performance of the reforming bench-scale unit was demonstrated in detail for propane steam-reforming, methanol and ethanol steam-reforming, partial oxidation of propane, water-gas shift at high and low temperature, preferential oxidation of carbon monoxide, and for the methanation of carbon monoxide.

Specication of the Basic System


Mass ow controllers for hydrogen, nitrogen, hydrocarbons, carbon monoxide, carbon dioxide, air and water (choice of selection optional) Stainless steel vessels for water and organic liquids Evaporator Valves, manometers, ame 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-ow controllers (e.g. for air, oxygen) Additional periphery heating (pipes) Additional liquid storage tanks (required for long term operation) Additional temperature sensors

PLANTS

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. The unit is designed for tests of startup, steady-state and transient reactor behaviour and for long-term tests. Process optimization studies may be performed, if serial combinations of several reactors (e.g. reforming, water-gas shift and preferential oxidation reactors) are integrated into the unit. Fast serial variation of process parameters such as temperature, pressure, gas ow velocity, and gas composition are possible. The test bench comprises commercial mass-ow controllers for control of the gas feed, ame arrestors to stop ame propagation, and various evaporator types (evaporation power between 10 s of watts up to kilowatts). The evaporator, which is fed by a liquid tank, produces steam or organic vapour. All devices are mounted onto a metallic frame. Steam and gas feed are mixed and enter the reactor, which may be a microstructured device or a conventional reactor type (metallic monolith or xed bed reactor). Operation in the microstructured reactors may be performed up to 900C at pressures of up to 5 bars, for maximum temperature of 500C at pressures up to 100 bars, 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. By-pass lines are introduced, thus allowing for switching off the individual reactors under test. The catalyst is usually introduced into the micro channels prior to the sealing procedure (normally laser-welding), e.g. by the wash-coat route and subsequent impregnation. By laser-welding the thermal treatment is spatially conned so that the catalyst is not destroyed during interconnection.

39
Please contact IMM prior to the construction of the test bench so that the modications required can be arranged. In conjunction with test bench construction, IMM services include provision of a manual which contains, besides general information, detailed documentation on experiences gained with operation of this bench-scale unit. Exemplarily, operational modes are given so facilitating the rst experimental steps when starting bench-scale unit operation. In case of further questions and requests, an IMM contact person can be consulted by mail or phone. By special request, a process parameter monitoring program based on the LabView software can be supplied that allows automatic data acquisition of temperature and pressure. The bench-scale unit was in detail investigated for steamreforming and autothermal reforming of fossil fuels, for water-gas shift and for the preferential oxidation of carbon monoxide, all up to the 10 kW range (lower heating value of the hydrogen produced/processed), however it may on special customer request be modied to allow for investigations of other types of heterogeneous gas-phase reactions. Here, information on the exact process desired is required from the customer and a special offer will be prepared by IMM.

Operating Conditions
Max. pressure (bar) Max. reservoir of water or organic liquid for one continious run (l) Max. owrate (gas) approx. (Nl/min) Max. owrate (liquid) approx. (g/h) Max. evaporator temperature (C) 10 20 about 500 about 5000 200

02

Specication of the Basic System


Mass ow controllers for hydrogen, nitrogen, hydrocarbons, carbon monoxide, carbon dioxide, air and water (choice of selection optional) Stainless steel tanks for water and organic liquids Evaporators Temperature controllers Pressure controller (optional) Valves, manometers, ame arresters All above devices mounted on a metal plate Available Reactors

Options
Additional massow controllers (e.g. for air, oxygen) Additional periphery heatings Additional liquid storage tanks Additional temperature and pressure sensors

PLANTS

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, IMM has developed a matching Continuous Work-Up Plant. 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. A biphasic reaction mixture (e.g. organic phase and aqueous phase) is separated by an initial, gravity driven mini-settler. In the next step, the organic phase is contacted with an aqueous washing phase via a Caterpillar Micromixer and separated subsequently in a second settler. In the third step, the same procedure is repeated. One settler-unit is composed of a glass tube, attached with special ttings on both ends. The ow of the organic phase in the two washing steps is automatically regulated by gear pumps based on the measurement by special lling level sensors. The water level in a settler is adjusted by a exible tube siphon. 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. Based on this the ow rate of the aqueous phase is adjusted automatically.

CWUP; separation of an incoming biphasic system and subsequent 2-step washing with micromixer-settler-siphon system.

Operating Conditions
Total ow rate Operating pressure Temperature up to 150 ml/min atmospheric up to 80C

Specication of the Basic System


Three settlers (glass tube and siphons) Two Caterpillar Micromixers Two + two gear pumps Four lling level sensors Filling level-ow rate controller Lab hood-like housing with transparent doors

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 ow chart for the Mixer-Settler Continuous Work-Up Plant

1. settler

pump

2x sensor

3x siphon system

Detail view on settling process (above); overview on plant components for a double washing unit (left).

mixer

2. settler

pump

2x sensor

mixer

3. settler

pH-sensor

Main components of the CWUP

PLANTS

COMPONENTS

42 03

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-V1.2 group class-R150, -R300, -R600, -R1200, -R2400 46 Star Laminator StarLam group class -30, -300, -3000, -30000 Slit Interdigital Micromixer SIMM group class SIMM-V2, HPIMM, SIMHEX, 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

OVERVIEW

44 03

> applications

Applications Liquid/liquid and gas/liquid reactions

Type of Standard Mixers and Reactors SIMM, CPMM, StarLam, 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 Gemioxacin (FACTIVETM) Isomerisation of allyl alcohols H-transfer reduction of citraconic acid ester Aromatic nitrations Aliphatic nitrations Direct uorination of toluene Sulfonation of aromatics Hydrogenation of nitrobenzene Hydrogenation of cinnamic acid esters

Special gas/liquid reactions

FFMR, MBC, SIMM, 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 olenes Photochemical chlorination of alkylaromatics Hydrogenation of C=C double bonds

Dispersion and emulsion formation Mixing of liquids differing in viscosity Photochemical reactions

SIMM, CPMM, StarLam SFIMM-V2, SIMM, StarLam Produced with window: SFIMM-V2, FFMR, MBR

Reactions with catalytic suspensions Particle and pigment synthesis Inorganic particles

CPMM

SSIMM, CPMM, IJMM, SLIMM

Titanates (precipitation) CaCO3 (precip.) Au (GNP), Pt/C (reduction) {N-doped TiO2 (hydrothermal process)}

Organic particles Pigments Polymer particles Microcapsules Amphiphilic particles

SSIMM, CPMM, IJMM, SLIMM SSIMM, CPMM HPIMM, SSIMM, CPMM SSIMM, CPMM SSIMM

Bipyridine (precipitation) Starch (dispersion + solidication) Azopigment Yellow 12 (precipitation) Azopigment Clariant (precipitation) Polystyrene (dispersion + solidication) Model prot. PSA-in-LGPA (disp. + solid.) Nanocomp. - Steroids (disp. + solid.) Stearate/phenobrate (self-assembly) Amphiphilic vesicles (self-assembly) Block copolymer vesicles (self-as.)

> 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 (0,1l/h - 1,0l/h)

COMPONENTS

C AT E R P I L L A R M I C R O M I X E R
CP M M - V 1 . 2 G R O U P C L A S S -R 1 5 0 , - R300, - R600, - R1200, - R2400

46 03

CPMM group class

Principle
The Caterpillar Micromixers are particularly suitable for applications where fast mixing at higher throughput is desired, providing highest performance for l/l-mixing as well as for g/l- or l/ldispersing. As they consist of a structured single channel, these devices may also be used successfully if precipitation occurs during the reaction or if ne slurries shall be processed. The higher owrates enable production scales of a few up to about 100 tons per year with all the advantages of our micro mixers, such as mixing quality, availability of different housing materials and safety gains. The Caterpillar Micromixer has internal bas-relief structures which induce recirculation ows transverse to the ow direction which result in efcient chaotic mixing. At very low Re numbers, e.g. for viscous ows at low ow rates, the mixing mechanism may change and a near-multilamellae type ow pattern arises which uses diffusion mixing in thin layers, in a split-and-recombine fashion.

Simulated real ow proles at high ow rates in Caterpillar Micromixers

47
Single Caterpillar Micromixers

CPMM sizes, from left: R150, R300, R600, R1200, R2400

03
Caterpillar Micromixer Arrays & Stacks
Research Topics at IMM In the context of IMMs 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. They combine the unique properties of the Caterpillar Micromixers and their less clogging-sensitive structures with the aim to process higher throughputs. 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. 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. Development here has been accompanied by modelling works to learn and understand uidic behaviour, mixing, and uid equidistribution when numbering up.

COMPONENTS

C AT E R P I L L A R M I C R O M I X E R
CP M M - V 1 . 2 G R O U P C L A S S -R 1 5 0 , - R300, - R600, - R1200, - 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 ne slurries shall be processed. Due to the construction principle only 30 bar system pressure can be applied, nonetheless enabling production of slurries containing up to some 100 kg per year of ne powders. These mixers consist of a single structured mixer channel with an adapted outlet.

CPMM with a straight outlet made of PP As the emerging reaction uid is not forced to leave the mixer via the 90 elbow ow conguration and in addition the rectan-gular mixer geometry is smoothly adapted to the round shape outlet tube, eddies can be prevented in this region and therefore fouling is diminished or even prevented. This effect can further be promoted by the application of suitable special housing materials as e.g. PTFE.

Technical Data
Name Caterpillar Micromixer R300 CPMM-V1.2R300 Caterpillar Micromixer R600 CPMM-V1.2R600 Caterpillar Micromixer R1200 CPMM-V1.2R1200 Caterpillar Micromixer R2400 CPMM-V1.2R2400 Caterpillar Micromixer R300straight outlet CPMM-V1.2R300-so Caterpillar Micromixer R600straight outlet CPMM-V1.2R600-so Caterpillar Micromixer R1200straight outlet CPMM-V1.2R1200-so Caterpillar Micromixer R2400straight outlet CPMM-V1.2R2400-so

Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (m) Standard material Options

all: bas-relief, recirculation ow (chaotic) 60 x 45 x 20 1/16 / 1/8 300 x 300 1.4435 60 x 45 x 30 1/8 / 1/8 600 x 600 1.4435 60 x 45 x 30 1/8 / 1/4 1200 x 1200 1.4435 79 x 45 x 30 1/4 / 3/8 2400 x 2400 1.4435 51 x 45 x 20 1/16 / 1/16 300 x 300 1.4435 51 x 45 x 30 1/8 / 1/8 600 x 600 1.4435 51 x 45 x 30 1/8 / 1/8 1200 x 1200 1.4435 70 x 45 x 30 1/4 / 1/4 2400 x 2400 1.4435

Heat exchanger function is possible; other materials like Hastelloy, Monell, Titan, PTFE or other plastics on request

Operating Conditions
Order number Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (l) Max Viscosity (mPas) Leakage Class CPMM-V1.2R300 -40 220 100 0.5 4 3.6 72 10 100 < L0.001 CPMM-V1.2R600 -40 220 100 2 40 2.25 45 25 100 < L0.001 CPMM-V1.2R1200 -40 220 100 4 80 3.15 70.2 78 100 < L0.001 CPMM-V1.2R2400 -40 220 100 15 250 3.6 60 250 100 < L0.001 CPMM-V1.2R300-so -40 220 30 0.5 4 5.4 108 15 100 < L0.01 CPMM-V1.2R600-so -40 220 30 2 40 2.7 54 30 100 < L0.01 CPMM-V1.2R1200-so -40 220 30 4 80 4.05 81 90 100 < L0.01 CPMM-V1.2R2400-so -40 220 30 15 250 4.32 72 300 100 < L0.01

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, where no residence time/delay loop is needed, the Caterpillar Micromixers may be combined to arrays thus enabling a nearby simultaneous mixing of more than 2 uids at once. With such arrays e.g. multi-component creams can easily be generated.

4CCPM-R952/8.2-R1200/8.1-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.g. heat exchanger delay loop) thus extending the application range to more exothermic reaction or application of molten materials. Of course, this heat exchange version may also be combined with the straight

outlet and its housing can be produced in nearby any material desired. Meanwhile, the Caterpillar Micromixers with heat ex-changer function are, notwithstanding the above photo of a gasketed one, typically brazed, turning the two heat exchange passages into service free units and enabling even for the gasketed center mixing section high system pressures and temperatures.

S TA R L A M I N AT O R
STAR L A M G ROUP C LA S S -3 0 , -300, - 3000, - 30000

50 03

The StarLam family

Principle
The Star Laminators are the rst real production tools of IMM for mixing purposes. They create an alternate, interdigital-type feeding array which is generated by stacking thin foils with star-like through-holes. In this way, a nely-dispersed injection of two uid streams is achieved. The foil stack is inserted into the recess of a housing where it is tightened by applying compression. The novel Star Laminators are largecapacity microstructured mixers reaching volume ows up to the m3/h domain. The apparatuses yield at higher ow rates a mixing efciency which compares the high performance of todays low-capacity (l/h) micromixers. Therefore, continuity from the real micromixers over the herein described high-throughput tools to conventionally manufactured static mixers with even higher ow rates is given. A classication of the mixing efciency versus the power input conrms this continuity as well. For the Star Laminator StarLam 3000 e.g. a 3 throughput of about 3 m /h at a pressure loss of 0.7 bar was determined for watery sys-tems. In this way, the StarLam series expands the range of operation from pilot-scale microstructured mixers of the Caterpillar series into production applications.

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: 1.4571 Foils: 1.4401 Star Laminator 300 StarLam 300 Multi-Lamination 40 x 40 x 64 8 mm/10 mm 100 Body: 1.4571 Foils: 1.4401 Star Laminator 30 StarLam 30 Multi-Lamination 40 x 40 x 64 8 mm/10 mm 50 Body: 1.4571 Foils: 1.4401

Standard mixing channels (m) 250 Standard material Options Body: 1.4571 Foils: 1.4401

Other materials like Hastelloy, Other materials like Hastelloy, Other materials like Hastelloy, Other materials like Hastelloy, 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: - 2 0 t o + 2 2 0 ; f o r FFKM: -20 to +315; for graphite: -100 to +500 (old S tarLam versions ) 100 5000 30000 180-1100 1500 (623 mix section) 10000 < L0.001 100 600 8000 72 960 160 10000 < L0.001 100 80 1000 1.7 220 5 10000 < L0.001 100 12 150 24 840 2.8 10000 < L0.001

03

COMPONENTS

S TA R L A M I N AT O R
STAR L A M G ROUP C LA S S -3 0 , -300, - 3000, - 30000

52 03
A B A Mixing channel A B

The feed plates of the StarLam series (here StarLam 3000), which are alternately stacked. A star-like plate serves for uid injection; another plate with circular conduit serves for forming the mixing channel and separation of the plates. The plates of each layer are turned by 30 so that separate feeds result.

StarLam 3000 foils during assembly on the assembly rods

StarLam 3000

StarLam 30 StarLam 30/300 disassembled

StarLam 300

Feed plates of StarLam 30, 300 and StarLam 3000

Concerning the high ow rates used for practical applications, mixing occurs by turbulence. As to be expected, the StarLam apparatus cannot be used at very low ow rates, as simulations and reaction-type mixing experiments conrm. In this ow regime, a segregation of uid layers is given so that mixing is here not effective enough. On the contrary, at high ow rates experimental characterization of mixing efciency 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, supplied by IMM. When plotting mixing efciency versus pressure drop it becomes evident that a continuity is given to the Caterpillar series, i.e. at the same pressure drop an equal mixing efciency is yielded independent which microstructured mixer is chosen as to be expected for a turbulent mixing scheme. As for any microstructured mixer, the feeding section is most sensitive to particles and fouling. However, owing to their simple reversible assembly, which is a mounted foil

stack, the StarLam series can be cleaned in a straightforward manner, e.g. if fouling was noted. The circular outlet channel has macroscopic dimensions so that also here particles will not be detrimental. The foils of the Star Laminators are fabricated by laser cutting; the housing is made by precision machining. Due to the geometry of the StarLam a multicomponent mixing can be easily realised by re-allocating the 12 single holes, e.g. 2 educts via 2x6 holes (standard), 3 educts via 3x4 holes or 6 + 2x3 holes (cf. p. 53 detail in photo top left), 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. Despite the fact that such a 3-, 4- component housing can be easily rebuild as 2 component housing, the feeding of the educts can also be adjusted by the mixing foil thickness as to enable mixing ratios of up to 1:100. Finally, the housing of StarLam30 and StarLam300 are identical and those mixers vary only in height and inner geometry of the mixer foil stack.

53

StarLam for mixing 3 components at once, 3CSL

StarLam 30/300/3000 connected in a multi-testing pilot plant

03

COMPONENTS

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, HPIMM, SIMHEX, 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. It has been used by a large number of customers, is cited multiple times in literature, and is indeed one of our best sellers. They combine the regular ow pattern created by multi-lamination with geometric focussing which speeds up liquid mixing. Due to this double-step mixing, the slit mixers are amenable to wide variety of processes such as mixing, emulsication, single-phase and multiphase organic synthesis. Extensive knowledge on hydrodynamics, mixing performance and reaction engineering for diverse applications of these mixers has been documented worldwide.

Interdigital ow 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. The pictures here show our latest efforts for a 10-fold scaled-up version of the SIMM-V2 mixer (ARRAY-10x-Slit Interdigital Micromixer), combining the unique properties of the interdigital mixers and their small structures with the wish to process larger throughputs.

Ten mixing elements are operated in parallel using common feed structures. Two kinds of upper housings have been realised: One collecting all ten single outlet streams in one and one with ten separated outlets. The latter allows systematic equidistribution measurements. The device has been developed for a liquid/liquid dispersion step.

55
SIMM-V2 HPIMM

Individual parts of the SIMM-V2 device

Individual parts of the HPIMM

Principle
This version has all the benets of mixing using multi-lamination and focusing only. Deliberately avoiding volume expansion, the inner volume could be decreased to only 8 l, coming along with improved uidic connections, e. g. to pumps and tube reactors, as it employs HPLC connectors. Compared to the connectors of the standard version SSIMM, the HPLC joint to steel tubing improves leak tightness and higher pressure operation can be achieved.

Principle
This micromixer was optimized using a metal sealing for tightening the two parts of the housing. As a consequence, the limits of pressure and temperature during operation are much higher than for at-seal tightened devices. The mixer also comprises expansion-free outlet channel geometry, i.e. renounces on jet mixing, 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 (m) Standard material Options SIMM-V2 Multi-lamination 30 x 40 x 30 1/16 / 1/16 HPLC 45 x 200 Body: 1.4571 Inlay: 1.4435 Other materials like Hastelloy, Monell or Titan on request

Technical Data
Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (m) Standard material Options HPIMM Multi-lamination 25 x 21 x 37 1/16 / 1/16 HPLC approx. 45 m x 200 m Body: 1.4571 Inlay: 1.4401 Other materials like Hastelloy, Monell or Titan on request

03

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (l) Max Viscosity (mPas) Leakage Class -40 220 100 0.04 2.5 14.4 720 8 10000 < L0.001

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (l) Max Viscosity (mPas) Leakage Class -40 500 600 0.04 2.5 27 1350 15 10000 < L0.001

COMPONENTS

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, HPIMM, SIMHEX, 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, using a graphite sealing for tightening the two parts of the housing. As a consequence, the limits of pressure and temperature during operation are limited but conveniently provide the possibility of heating or cooling the device. The mixer also comprises expansionfree outlet channel geometry, i.e. renounces on jet mixing, but relies on multi-lamination and geometric focusing only.

Principle
This micromixer is the classic one amongst all IMM chemical micro processing products. It combines the regular ow pattern created by multi-lamination with geometric focussing and subsequent volume expansion, which speeds up liquid mixing of the multi-lamellae and leads to jet mixing. Due to the volume expansion the mixer contains an inner volume of 40 l and is only offered with non-stainless soft tube connectors.

Technical Data
Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (m) Standard material Options SIMHEX Multi-lamination 25 x 25 x 20 1/16 / 1/16 HPLC 40 x 300 Body: 1.4571 Inlay: 1.4401 Other materials like Hastelloy, Monell or Titan on request; incl. heat exchanger function

Technical Data
Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard mixing channels (m) Standard material Options SSIMM Multi-lamination 19 x 30 x 16.5 1/16 / 1/16 soft tube 45 x 200 Body: 1.4571 Inlay: 1.4435 Other materials like Hastelloy, Monell or Titan on request

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (l) Max Viscosity (mPas) Leakage Class -100 500 50 0.04 2.0 18 900 10 10000 < L0.001

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (l) Max Viscosity (mPas) Leakage Class -20 +100 3 0.04 1.5 72 3600 40 10000 < L0.001

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 ts the standard mixer as well as the version 2. For both versions the inlays have a size of 11.0 mm x 7.5 mm and ~ 3.6 mm thickness with different possible channel sizes and depths. The following inlays are available: Laser-ablation (channel width 45 m, 200 m channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request, order number SMI-Lasab45200 LIGA technology (channel width 25 m or 40 m) made from silver or nickel on copper with 300 m channel depth, order numbers SMI-Ni25, SMI-Ni40, SMI-Ag25 or SMI-Ag40 ASE (thermally oxidised silicon, channel width 30 m or 50 m) with 100 m channel depth, order numbers SMI-Si30 or SMI-Si50. As these inlays are only 0.6 mm thick, extra bases of 3.0 mm thickness are needed

This inlay ts the slit interdigital mixer heat exchange exclusively. The size of SMHXI inlays: 20 mm x 6 mm The following inlays are available: Laser-cutted inlays (channel width 45 m, 250 m channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request, order number SMHXI-45250

This inlay ts the high-pressure slit mixer exclusively. The size of HPMI inlays: 8.0 mm in diameter and 250 m in thickness The following inlays are available: Laser-cutted inlays (channel width 45 m, 250 m channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request, order number HPMILas45250

03

COMPONENTS

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. It comprises two microstructured plates with integrated micro mixer and micro heat exchanger. Insofar, it is particularly designed for reactions that benet from excellent heat transfer as well as fast mass transfer. The heat transfer is provided by specic surfaces of 10,000 m2/m3 in micro channels of a width of 200 m at an aspect ratio of 6, whilst the fast mass transfer derives from the meanwhile incorporated interdigital micromixer, known from the SIMM series. The LLMR-MIX can be offered of different materials on request besides the standard stainless steel. Flow rates

Detail of the internal mixing section

from 50 ml/h up to 2 l/h are feasible, with residence times in the 0,3 18 s range. The reactor can be used up to 50 bar and 180C (Viton, Chemraz gasket) or higher if graphite is applied. The laser-cut inlay of the LLMR-MIX

59

LLMR-MIX-HC276 disassembled

LLMR-MIX explosion drawing

LLMR-MIX made of Hastelloy

LLMR-SY; 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 (m) Liquid/Liquid Microreactor LLMR-Mix Multi-lamination 45 x 120 x 26 1/16 / 1/16 for chemicals 1/4 / 1/4 for cooling uid 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 0.05 2 0.3 18 1000 < L0.01

Standard cooling channels (m) 200 x 1200 Standard material Housing, reaction and cooling plate: 1.4571 or 1.4539 Inlay: 1.4404 Other materials like Hastelloy, Monell, Titan or plastics on request

Options

COMPONENTS

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 - 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. Physically speaking, this means having a nozzle feed array, a triangular-type focusing chamber and a thin mixing channel. The SuperFocus Mixer Version 2 (SFIMMV2) bases upon the simulation, design and characterisation of the former version SFIMM. Development target was to achieve even higher throughputs, to have a robust steel design, e.g. for high-pressure operation and to use a still higher focusing ratio, e.g. to reduce the sensitivity towards blockage. The SuperFocus mixer thus combines both high throughput, which is e.g. characteristic of the StarLam series and uniform ow patterns, which is e.g. characteristic for the SIMM components. Compared to the predecessor design more nozzles enable uid feed. The nozzle width was enlarged, thus being less particle sensitive, albeit the nal focused lamellae width of about 4 m was kept, i.e. the focusing ratio was increased from 40 formerly to now 178 (and can be set higher on demand). To arrange as many as 138 nozzles, a large circular arc was chosen for the feed array. The mixing channel width and length compares to the former design so that the semianalytical and experimental reaction type based ndings on the mixing time can be largely transferred to the new design. Although steel is employed as construction material, an optional inspection window may allow the monitoring of the ow patterns and of the mixing course. For the SuperFocus SFIMM-V2 throughput of about 350 l/h at a pressure loss of 3.5 bar was determined for watery systems. The formation of ow patterns is very uniform, i.e. a multi-lamellae ow is found all over the focusing chamber until the mixing channel is reached. The known deviations from ideal given for any multi-lamellae ow are found as well, e.g. that lamellae are thicker at the wall (boundary) than in the interior of the ow. In particular this deviation should be less here compared to other systems, as the ratio of outer to inner lamellae is 136:2.

Disassembled SFIMM-V2-300

The mixing time achievable is 4 ms according to calculation and experiments made with the former design, albeit excluding the time needed for owing through the focusing chamber. The latter is dependent on the volume ow. Specialty designs with notably reduced focusing time are possible. The same holds for integrated mixing-heating element congurations, allowing one to perform fast temperature switches for starting and ending reactions in a very short, dened time frame, as e.g. done in quench-ow analysis.

61

Multi-lamellae ow 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 (m) 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 m x 5 mm 138 260 178 1.4435 Other materials like Hastelloy, Monell or Titan on request; heat exchanger function is possible

The SFIMM is meanwhile also produced as smaller device for about one tenth of the original throughput, 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 < L0.001

03
Mixing structure of SFIMM-V2-30

SFIMM-V2-30 with straight outlet for high viscosity emulsions

COMPONENTS

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, e.g. by plugging the whole system. As a matter of fact, most organic processes are associated with more or less precipitation during the course of reactions. Particle generation is simply not possible in the vast majority of todays micro devices. For this reason, a specialty mixer was developed that performs mixing in a wall-free environment, i.e. by two pump-driven, falling jets merging into one in a Y-shaped conguration. It was shown that the smaller the jet diameter, the better the mixing quality. Intense knowledge on jet conguration as a function of ow rate and jet diameter has been documented, in addition to mixing quality judgement. As a result, the nozzles of the jet mixer have tiny, only 350 m 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. The aminolysis of acetyl chloride with n-triethylamine in THF leads to instantaneous heavy precipitation. This reaction hardly can be handled in any other micro device. It is an extreme representative of many other organic reactions that suffer more or less from fouling, e.g. like quaternizations.

3 different ow patterns: Y-type jet of IJMM (top) Fan-shaped jet (middle) Fanned-out jet (down)

63
Fluid A Fluid B

IJMM in a special funnel-like housing for particle production

Geometric parameters determine the mixing performance, beside ow parameters

Technical Data
Name Order number Mixing principles Size (L x B x H) Connectors (Inlet/Outlet) Standard boring-/noozle diameter d (m) Orientation angles (d) Standard material Options Impinging-Jet Micromixer IJMM Jet collision 10 x 35 x 10 1/8 / 1/8 Clamp screw 350, 500, 1000 45, 60, 90 1.4571 Other materials like Hastelloy, Monell or Titan on request

03

Impinging-Jet micromixer Plant, IJMP, cf. plant section, including heat exchangers, pumps, process control system

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (ms) Inner volume (l) Max Viscosity (mPas) Leakage Class -40 220 10 0.5 3 0 0 100 < L0.001

IJMM in adequate housing as used for IJMP

COMPONENTS

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 lms that move by gravity force for a typical residence time of seconds up to about one minute. Its unique properties are the good temperature control by an integrated heat exchanger and the specic interface of 20,000 m2/m3. Such high mass and heat transfer were e.g. exploited when performing direct uorination of toluene with elemental uorine in the original version of IMMs 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. Due to the high raised interest for such a kind of device, 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. The several types of Falling Film Microreactors including the new ones are introduced in the following.

65

Falling lm principle in a multichannel architecture

Thermographic monitoring: Initial wetting ow (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 modied by incorporation of additional grooves in order to improve via recirculation ows the liquid side mass transport. First tests based on CO2 absorption in aqueous sodium hydroxide have proven that signicant 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 1.4571 for housing and reaction plate Copper for cooling plate Borooat glass for inspection 300 x 100 (64 channels) 600 x 200 (32 channels) 1200 x 400 (16 channels) 7.6 5
3

Temperature (C) Pressure stability (bar) Flowrate (l/h)

180 (option: 300) 10 (without Borooat glass: 20) 0.05 for channel geometry 300 m 0.6 for channel geometry 600 m 1.5 for channel geometry 1200 m 0.8 20 25 100 up to 20000 L0.01

Residence time (s) Liquid lm thickness (m) Interfacial area (m /m ) Leakage Class
2 3

Standard reaction channels (m) Reaction channel length (cm) Gas chamber height (mm) volume of gas chamber (mm ) Standard cooling channels (mm) Options

13336 Width: 1.5 Depth: 0.5 Other materials like Hastelloy, Monell or Titan on request

COMPONENTS

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. In the FFMR-LARGE therefore the length and the number of channels have been increased by a factor of 100.5. From the general design FFMR-LARGE is quite similar to FFMR-STANDARD. FFMR-CYLINDRICAL follows another approach. The reaction channels are now engraved on the outside of a metallic tube. The cylindrical shape allows a quite compact design in this case. The number of the reaction channels has been increased by a factor of 7.5, the length of the channels has been elongated a bit to get a tenfold increase of structured surface area. The FFMR-CYLINDRICAL is of special interest for photochemistry applications. FFMR-CYLINDRICAL

FFMR-STANDARD and -LARGE

Technical Data
Name Order number Size (L x B x H) Connectors Material Standard reaction channels (m) 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 1.4571 for housing and reaction/cooling plate Quartz glass for inspection 1200 x 400 (50 channels) about 25 4,5 90000 Width: 0.2 Depth: 0.4 Other materials on request Falling Film Microreactor Cylindrical FFMR-CYLINDRICAL 80 x 130 1/8 and 1/4 (welded tubes) 1.4571 DURAN glass for inspection 1200 x 400 (120 channels) about 10 5 100000 Width: 1.2 Depth: 1.0 Other materials on request

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Liquid lm thickness (m) Interfacial area (m /m )
2 3

180 10 (without glass: 20) investigated range 0.24 - 1.20 calculated 23 - 8 calculated 60 - 100 about 9814 - 16780

180 5 investigated range 0.24 - 1.20 calculated 16 - 6 calculated 45 - 76 about 13140 - 22470

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 (m) 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 1.4571 + Ni screen printing braze 1200 x 400 (50 channels) about 25 5 4 7300 Width: 1.2 Depth: 0.4 On request STACK-1x-FFMR-LARGE 296 x 118 x 12 all 3/8 1.4571 + Ni screen printing braze 1200 x 400 (50 channels) about 25 50 4 73000 Width: 1.2 Depth: 0.4 On request STACK-10x-FFMR-LARGE 296 x 118 x 75 all 3/8 1.4571 + Ni screen printing braze 1200 x 400 (50 channels) about 25 500 4 730000 Width: 1.2 Depth: 0.4 On request

03

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Liquid lm thickness (m) Interfacial area (m2/m3) 180 10 about 0.02 - 0.12 about 23 - 8 about 60 - 100 about 9814 - 16780 up to 800 @ 1 bar up to 50 @ 25 C about 0.24 - 1.20 about 23 - 8 about 60 - 100 about 9814 - 16780 up to 800 @ 1 bar up to 50 @ 25 C about 2.4 - 12.0 about 23 - 8 about 60 - 100 about 9814 - 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. The STACK-1x-FFMR-LARGE thereby represents the equivalent to FFMR-LARGE and the basic functional element for following numbering-up. So STACK-10x-FFMRLARGE contains 10 functional elements. To round up the brazed reactor program also a new lab version has been developed (STACK-1x-FFMR-LAB). Compared to STACK-10x-FFMR-LARGE it should allow identical experimentation at a throughput of only 1/100 of the STACK-10x-FFMR-LARGE. Brazing technology opens the door for specically adopted reactors for high pressure applications.

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

Counter-ow principle

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 (m) Options Gas Phase Microreactor GPMR 70 x 70 x 55 1/8 1.4571 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) Specic inner surface per layer (m2/m3) Active inner volume per layer (mm ) Operation mode
3 2 3

GPMR integrated into a plant, here as simple heat exchanger (COMH) for education purpose
500 3 1 7 / 1 600 L0.1 18000 580 2900 32 Counter- or co-current ow

03

COMPONENTS

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- 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, each lled with one stack of microstructured platelets, which are connected via a conduit. Both stacks are connected to welded tubes, serving for feed and uid withdrawal. The rst stack comprises two types of mirror-imaged platelets with parallel feeding channels which are alternately arranged so that a multi-lamination ow conguration is created for gas mixing. In the conduit attached, forming a ow-through chamber, mixing is completed within short time due to the virtue of decreasing the diffusion path. Hence the mixed reactant gas volume (before reaction) is kept as small as possible. As a result, investigations in the explosive regime are safely amenable, as demonstrated by research with this and similar tools. The second stack comprises platelets with parallel channels of small depth so that very good heat transfer is provided. By this means, hot-spots are reduced and near-isothermal operation can be achieved. The platelet construction material itself may act as catalyst or, more preferably, the channels may be coated with a catalyst layer, e.g. wet chemically using the wash-coat route or by means of thin-lm deposition. A small total mass of the construction material, hence a compact arrangement of the functional units, and internal large-power heat supply guarantee fast heating up, typically in the range of a few minutes (ca. 100 K/min), even when approaching rela-tively large temperatures, e.g. up to 600C. Internal cooling typically of similar time scale is provided by convection ow of a gas stream at high ow rate in a channel which surrounds the functional units. The mixer-catalyst zone reactor has been extensively studied for its use for ethylene oxide synthesis. Among other results of the parametric study, safe operation in the ex regime (3 vol.-% ethylene, 50 vol.-% oxygen, balance nitrogen; 5 bar; 4 l/h; 277C), high space-time yields (up to 0.78 tons h-1 m-3), a maximum selectivity of 69% (6 vol.-% ethylene, 30 vol.-% oxygen, balance nitrogen; 5 bar; 0.124 s; 5 l/h; 290C), not far from the industrial benchmark, and higher conversions at comparable selectivity compared to xed-bed technology (20 vol.-% ethylene, 80 vol.-% oxygen; 0.3 MPa; 3.17 l/h; 230/250C) were demonstrated.

Schematic of the GPMR-Mix device and details of the functional principle

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 (m) Number of catalayst plates Size of catalyst plate (mm) Channel geometry of the catalyst plates (m) Gas Phase Microreactor with Mixer and Internal Heating GPMR-MIX 40 x 40 x 30 1/4

10 7.5 x 7.5 180 490 x ~ 100 10 9.5 x 9.5 460 x 125

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) Residence time (s) Leakage Class Specic surface area (m /m ) Total inner surface per reaction layer (mm ) Specic inner surface per reaction layer (m2/m3) Active inner volume per layer (mm )
3 2 2 3

03
600 50 5 0.025 2 < L0.1 12700 54 3840 2.5

COMPONENTS

Inconell 600 (2.4816) for housing and top plate 1.4571 for mixing and catalyst plates

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. The plates are easily exchangeable and the assembly of the reactor is simple. On demand, 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, however, it may be as well applied as a testing reactor for all kind of heterogeneous gas phase reactions at ow-rates exceeding the range of small-scale laboratory devices. 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. Full conversion of 32 g/h methanol was achieved with a conventional Pt-catalyst at 130C reaction temperature. No other products than carbon dioxide and water were found above the detection limit. Thus absence of bypass effects could be proven.

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 (m) 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 0.10 1 < L0.1

COMPONENTS

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. On demand, the micro structured plates can be coated with various carrier/catalyst systems. They are easily exchangeable using an included mounting tool and relatively inexpensive due to mass fabrication by wet-chemical etching. By simple exchange of the end caps a decision can be made whether to operate the microreactor in serial or in parallel mode. Parallel operation (1 in, 10 out): Using a diffuser-type end cap, the microstructured plates are fed simultaneously by the one common inlet stream. The sub-streams leave then through the ten separate outlets that can be analyzed accordingly. 10 levels with different catalysts but same feed gas. Screening of catalysts.
Parallel operation (10 in, 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. 10 levels with different catalysts and/ or different gases. Screening or numbering-up of catalysts. Serial operation (1 in, 1 out): Using two other end caps similar in shape, the one inlet stream ows serially in a zigzag manner from one plate to the other, being turned around and guided to the next level and so on, nally resulting in a path of ten times length compared to the single plate length, respectively ten times the residence time. Up to 10 plates with identical catalyst may be installed. Variation of the reactor length. Two end caps for parallel operation Stack of cartridges with coated microstructured plates

75

Special version for 800C 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 1.4841 for housing 1.4742 for catalyst plates 20 50 x 14 Other materials on request

Operating Conditions
Temperature (C) Pressure stability (bar) Standard ow velocity (m/s) Residence time (ms) Leakage Class 800 20 (100 bar at 400C) 0.4 40 0.025 2000 < L0.1

03

Options
Catalyst plates can be delivered with various channel geometries: Channel geometry (width m x depth m): 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

L A S E R - 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), WT-404, WT-304, WT-204 (from left to right)

Principle
The WT-series was developed as a heat exchanger for liquid/liquid, gas/ liquid or gas/gas applications and can also serve for evaporation or condensation. They comprise a laser welded stack of arranged microstructured plates enabling a counter- or co-current ow scheme. Being assembled with conventional 1/4 or 3/8 tubes, easy integration into the existing tubing system of pilot- or small-scale production plants is possible. The core elements are chemically etched microstructured plates, sealed by high-precision laser welding. These heat exchangers are normally designed for ow rates between 1 l/h up to 400 l/h; higher ow rates of up to 1000 l/h are possible at moderate pressure drops. The high efciency and heat transfer coefcients 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 specic surface. Additionally, the channels of plates can be coated with catalyst using the heat exchanger as reactor for heterogeneously catalysed reactions, typically gas-phase reactions, like e.g. steam reforming.
Single plates of the WT08-series

Single plates of the WT04-series

77
Technical Data
Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Dimensions of heating channels (m) 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, others on request 800 x 400, others on request WT 404 100 x 44 x 42 3/8 / 3/8

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (water, l/h) 0.5 50 up to 1000 @ 1 bar 5 @ 25 C (higher upon request, max. 20 bar) 2.5 250 6 600

03

Other examples of laser-welded micro heat exchangers

Special type HxA

Special Heat Exchanger, also for condensing

HCOMH

COMPONENTS

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); HX-204, HX-304 (top right), HX-404 (bottom right)

Principle
This novel HX-series was developed as a heat exchanger for liquid/liquid, gas/liquid or gas/gas applications at high pressure and temperature regimes. They comprise a brazed stack of aligned plates enabling a counter- or co-current ow scheme. The core elements are chemically etched microstructured plates, laminary joined applying brazing technology. These new heat exchangers are normally designed for ow rates between 1 l/h up to 400 l/h; higher ow rates of up to 1000 l/h are possible at moderate pressure drops. The high efciency and heat transfer coefcients 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 specic surface.

Single plates of the HX-304-series (left: blank, right: coated with screen printing paste)

79
Technical Data
Name Order number Size (L x B x H) Connectors (Inlet/Outlet) Material Dimensions of heating channels (m) HX 204 ca. 100 x 60 x 20 1/4 / 1/4 Brazed Micro Heat Exchanger Series HX 304 ca. 150 x 80 x 25 3/8 / 3/8 316 Ti, others on request 1000 x 600, others on request HX 404 ca. 200 x 120 x 40 1/2 / 1/2

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (water, l/h) 0.5 50 up to 800 @ 1 bar up to 500 @ 25 C 2.5 250 10 1000

Brazed (high pressure) Microreactors


Research Topics at IMM Brazing opens the possibility of interconnecting large-area reactor structures monolithically. Thereby large interior volumes are possible with high pressure strength at the same time. Further the brazing technique makes a multiplicity of new reactor geometries accessible. IMM extended strongly the application of the brazing technique as sealing technology for microreactors of different functionality. Besides the HX-series the technology has e.g. 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), which is tested for operation at 120 bar @ 250 C.

03

At IMM the microstructured reactor plates are coated with the brazing paste by using the screen printing machine Type THIEME 1010 E.

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.

COMPONENTS

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, designed for electrical heating of gases and liquids. The optimized size of this device allows a very fast heating up as well as fast changes of temperatures. Being offered in two sizes, the maximum power rate to be transferred can be up to 800 W with a thermal efciency > 90% (depending on operation conditions). Several options can be offered: THTMD solely THTMD plus suitable heat cartridge (if suitable electronic control unit is at hand) Full package, comprising THTMD plus heat cartridge, two thermocouples and electronic control unit In the latter case, 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. Operation conditions are tested for maximum 300C @ 1 bar or 45 bar @ 25C.
Technical detail of heat exchanger structure

THTMD in parts before laser-welding

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 (m) Options Tube Heat Transfer Micro Device THTMD 120 x 100 x 15 1/4 / 1/4 1.4571 60 400 Other materials like Hastelloy, Monell or Titan on request

Operating Conditions
Temperature (C) Pressure stability (bar) Flowrate (l/h) liquid Power rate (W) Thermal efcieny Leakage Class up to 500 45 1.0 20.0 800 > 90% L0.1

03

COMPONENTS

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 ow controller (upper box) and with integrated LV1 (lower box), front view (left) and backside view (right)

Principle
The Evaporator System is a nearly pulsation-free continuous evaporator without the supply of carrier gas. It comprises a pair of microstructured plates together with a control system for the liquid ow as well as the electrical heating and its temperatures to ensure the continuous use. Rapid preheating, evaporation and over-heating are realized in one single device. Two electrical heating cartridges supply the heat to the corresponding microstructured plates with large specic surfaces for excellent heat transfer. Up to 100 g/h water (without carrier gas) can be evaporated. A maximum temperature of 350C for the vapour or up to 6 bar system pressure are feasible.
LV1 Laboratory evaporator for 100 g/h

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 1.4301

Operating Conditions
Temperature (C) Pressure stability (bar) Temperature (C) of Vapor Flowrate (g/h) Power rate (W) 400 6 up to 350 10.0 100.0 400

03

COMPONENTS

84 04

GENERAL TERMS AND CONDITIONS OF DELIVERY AND SALE

1.

General Provisions

1.1 The terms and conditions set forth herein apply to deliveries and sales to entrepreneurs, public legal persons and public special funds according to 310 section 1 BGB (German Civil Code) (Purchaser) exclusively. 1.2 These terms and conditions apply to all our agreements and quotations, even to prospective agreements and quotations, and apply exclusively. 1.3 Purchasers conditions which are contradictory to or diverging from our terms and conditions do not apply unless their validity is expressly agreed in written form. 1.4 These terms and conditions also apply in case we supply even though contradiction or divergence of Purchasers conditions from our terms and conditions is known to us. 1.5 All agreements between us and Purchaser for the purpose of performance of the contract at hand require written form. This also applies to the waiver of the written form itself. 2. Offers and Prices

3.8 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, as well as compliance with agreed conditions of payment and other obligations by Purchaser. If these requirement are not timely fullled, respite of delivery will be adequately prolonged, unless we are responsible for the delay. 3.9 Delivery time will be extended adequately in case of force majeure, strike, lockout, breakdown, delay of external suppliers and other unexpected circumstances. In such cases we reserve the right to withdraw from the contract taking into account Purchasers interests. 3.10 If Purchaser defaults in payment in the context of other present contractual relationships between Purchaser and us, we are entitled to detain delivery under this contract for the duration of default of payment, prior notice to Purchaser provided. This shall not apply in case of minor outstanding payment. 3.11 In case of application to open insolvency proceedings as well as of afdavit 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. Furthermore, 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. 4. Payment Terms

2.1 Our offers are not binding until our written order conrmation is submitted. Oral offers are not valid unless a written conrmation is submitted. 2.2 Our prices are effective ex factory plus value added tax and costs of delivery and packaging. 2.3 Unless a xed price agreement is reached, we reserve the right to adequately adjust the price due to changed costs for wages, material and distribution of deliveries, which are carried out three months after conclusion of the contract or later on. 3. Extent of Delivery and Performance

4.1 Invoices are payable net within 30 days as of invoice date. 4.2 Unless otherwise agreed, ordering amounts of more than 10.000,-- EURO will be invoiced in two rates of 50% of the order value each. If so and unless otherwise agreed, delivery will not be performed until receipt of the rst rate. The second rate is due after delivery. 4.3 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. In the event of such agreed submission of bills of exchange or cheques, payment shall only be deemed to have been made upon encashment, due payment provided. 4.4 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). We reserve the right to claim a higher damage as a result of default. 4.5 Purchaser will be entitled to set off with counterclaims only, if said claims are undisputed or legally conrmed. Purchaser is entitled to lay a lien on his payment only as far as the counterclaim is based on the same contractual relationship. In case of reasonable partial delivery Purchaser is not entitled to lay a lien on his payment for reasons of outstanding parts of delivery. 5. Retention of Title

3.1 The order conrmation discloses the whole extent of the delivery and performance owed. 3.2 Purchaser bears the costs and risks of delivery. 3.3 In case we owe a separable performance, partial delivery is permitted for relevant reasons to a reasonable extent. We are entitled to invoice partial delivery separately. 3.4 Specications as to time of delivery are not binding unless a binding time of delivery is expressly agreed. If we do not meet a binding time of delivery, Purchaser will be entitled to withdraw from the contract, if we do not deliver within an adequate additional respite granted by Purchaser. Upon our request Purchaser is obliged to declare within an adequate respite, whether he withdraws from the contract because of the delay of the delivery or demands delivery. 3.5 If the Parties agree that our performance will not be initiated until down payment or advance payment has been made, delivery time will not begin unless the according amount has been credited to our business account subject to a separate agreement. 3.6 If we exceed time of delivery, Purchaser in case Purchaser credibly shows, that resulting from this he suffered damage will be entitled to demand indemnication amounting to 0.5 % of the delivery value for each completed week of delay, but not exceeding a total of 5 % of the delivery value. 3.7 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. 6 are excluded in all cases of delayed delivery, even after expiry of an additional respite of delivery. This shall not affect the cases where IMMs liability is mandatory by law in cases of intent, gross negligence or damage to life, body or health. The foregoing regulation does not stipulate a reversal of the burden of proof for Purchaser.

5.1 We reserve the right of property in the delivery items until Purchaser completely satises our claims arising from the contract at hand. 5.2 As long as property is not transferred to Purchaser, Purchaser is obliged to treat the delivery item with care. Particularly Purchaser is obliged to insure the delivery item sufciently according to its replacement value and at Purchasers own expenses against damage caused by theft, re and water. 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; we hereby accept assignment. Notwithstanding the assignment, Purchaser is authorised to assert and collect claims in his own name, by legal proceeding if necessary. Our entitlement to collection of debts remains unaffected by Purchasers authorisation. Necessary maintenance or inspections are to be performed by Purchaser at Purchasers own expenses in due time.

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5.3 In case of breach of contract, particularly of default of payment or breach of these terms and conditions, we reserve the right to withdraw from the contract at hand and to reclaim property. 5.4 In case of garnishment, requisition or other disposals or interventions of third parties, Purchaser is obliged to notify us forthwith. Purchaser shall be liable for our detriment, 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). 5.5 Purchaser is entitled to resale delivery items under reserved property in regular course of business. Purchaser herewith assigns to us all claims against Purchasers customers arising from said resale at the nal amount of the invoice (incl. value added taxes). This assignment is valid irrespective of whether the delivery items under reserved property were resold without or after product processing. Even after cession Purchaser remains authorised to collect outstanding claims. This shall not inuence our right to collect the debt. However, we will not collect the debt as long as Purchaser fulls his obligation of payment, Purchaser is not in default of payment, no application for opening insolvency proceedings is led and payment has not been stopped. 5.6 If the delivery items under reserved property are worked, processed or modied by Purchaser, such working, processing and modication shall always be deemed to be performed on our behalf. In this case the remainder of Purchaser in the delivery item is continued in the worked, processed or modied item. Shall the delivery item under reserved property be processed or modied together with other objects not belonging to us, 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. Relevant value will be that at the time of working, processing or modication. The same shall apply in case of commingling, mixture or combination. Should the resulting merchandise consist of Purchasers objects forming the main part, 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. For securing our claims against the Purchaser Purchaser herewith assigns to us all claims, which accrue to him from connection of the delivery items under reserved property with immovable property; we hereby accept assignment. 5.7 We hereby covenant to gradually release at Purchasers demand the securities obtained by retention of title in so far as the propertys value exceeds the debts to be secured by more than 20 %. 6. Transfer of Risk of the delivery items in connection with special chemicals. If Purchaser or third parties carry out inappropriate maintenance or changes, no claims because of fault emerging from such inappropriate maintenance or changes will accrue. 7.3 We do not accept liability for our product being apt for a special intention. All information, irrespective of being oral or written, relating to possible elds of application of our products, is served to the best of our knowledge. It is based on our experience and therefore is not guaranteed. Purchaser is responsible to inspect the suitability of our products for the intended elds of application. 7.4 We do not warrant freedom from third parties rights in the delivery items. 7.5 Purchaser will examine the consignment immediately after receipt for damages. If any defect becomes apparent during such inspection or is later detected, Purchaser has to give written notice thereof including description of the fault to us immediately, but not later than ve (5) working days after delivery and discovery respectively. 7.6 If despite all applied diligence delivery items show a fault, which already existed at the time of transfer of risk, we will be entitled, subject to notice of defect in due time by Purchaser, to subsequent performance which may be carried out as elimination of defect or delivery of items free of defects, as our choice may be. Within an adequate respite we are entitled to subsequent performances done twice. Claims for recourse remain unaffected by foregoing regulations without restrictions. 7.7 In case subsequent delivery fails, Purchaser is entitled claims for damages remain unaffected to withdraw from the contract or demand price reduction. 7.8 Should complaints turn out to be unjustied and should we not have given reasons therefore, Purchaser has to reimburse any and all of our costs in connection with the putative subsequent performance which we could reasonably deem appropriate. 7.9 Claims of Purchaser because of expenditures for the purpose of subsequent performance, particularly expenses for delivery, infrastructure, wages and material, will be excluded, if additional expenses are caused by subsequent transfer of the delivery items to a place other than Recipients site unless transfer corresponds to the delivery items conventional use. 7.10 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, which exceed the warranty, which is mandatory by law. Concerning the extent of the claims for recourse of Purchaser against us no. 9 shall apply mutatis mutandis. 7.11 Damages claims of Purchaser because of material defects or defects as to the quality are excluded. This does not apply in case of fraudulent concealment of the defect, noncompliance of guarantee of condition, in case of harm of life, body, health or liberty nor in case of intended or grossly negligent violation of duty. The foregoing regulation does not stipulate a reversal of the burden of proof for Purchaser. Claims of Purchaser because of material defects or defects as to the quality exceeding or differing from this clause VII. are excluded. 8. 7. Liability for Faulty Goods 8.1 All other damages claims of Purchaser are excluded no matter what legal ground they are based on, particularly in case of violation of duty of the contractual relationship and of tort. 8.2 This shall not affect the cases where our liability is mandatory by law, like e.g. according to Produkthaftungsgesetz (German Code of Liability for Faulty Products), in case of intent, gross negligence, damage to life, body or health, and in case of breach of cardinal contractual obligations. The liability of IMM in case of breach of cardinal contractual obligations shall be limited to the foreseeable, typically occurring damages. This shall not apply in case of intent, gross negligence, and damage to life, body or health. The Other Damages Claims

6.1 If the delivery items are sent to Purchaser at Purchasers demand, 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. This applies irrespective of whether dispatch is initiated from place of performance and irrespective of who bears the costs of delivery. 6.2 If dispatch, service, execution of setting up or assembly, taking over for operation, or trial operation are delayed for reasons attributable to Purchaser or Purchaser is in default of acceptance for other reasons, risk will be transferred to Purchaser.

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7.1 Period of warranty shall expire twelve (12) months after time of delivery. 7.2 Claims because of fault are excluded in case of negligible deviation, deviation being customary in trade and technically unavoidable deviation from the agreed condition, in case of negligible impairment of serviceability, in case of fair wear and tear and damages, which accrue after transfer of risk because of careless or faulty treatment, immoderate stress, use of unapt equipment or because of special exterior inuences, which are not subject to the contract at hand. Claims because of fault are excluded in case of corrosion damage unless Purchaser pointed out the intended use

ANNEX

GENERAL TERMS AND CONDITIONS OF SALE

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foregoing regulation does not stipulate a reversal of the burden of proof for Purchaser.

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9.

Title and Copyright

9.1 We reserve all copyright and rights of ownership concerning all samples, illustrations, drawings, calculations or other documents and information given to Purchaser. 9.2 Purchaser is obliged to keep secret all samples, illustrations, drawings, calculations or other documents and information received. They shall not be made accessible to third parties without our explicit consent. 9.3 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, illustrations, drawings, calculations or other documents and information has become common knowledge. 9.4 Purchaser is not allowed to disassemble the delivery items, samples etc., and/or to analyse or to examine or to have analysed delivery items, samples etc. composition, functioning, working or similar, or to manipulate delivered items, samples etc. in any other way. 10. Intellectual Property Rights 10.1 Purchaser warrants that production of items according to Purchasers instructions does not infringe third parties rights. 10.2 Should infringement of said rights be substantiated to us by a third party, we are entitled to stop any further activity being in opposition to said rights. If so, Purchaser will indemnify us from third parties claims on rst demand. 10.3 Purchasers obligation of release from liability comprises any expenditure we necessarily incur in the context of third parties claims. 10.4 Our claims for damages remain unaffected. 10.5 Statute of limitation concerning said claims expires ten (10) years as of conclusion of the respective contract. 11. Applicable Law 11.1 The Laws of the Federal Republic of Germany shall apply exclusively to this contract. 12. Place of Performance Place of Jurisdiction 12.1 Place of performance for all contractual duties shall be our place of business. 12.2 Any action concerning disputes arising from this contractual relationship shall be taken at the court, which is competent for our place of business. 13. Severability Clause Should one or several provisions of the contract be or become completely or partly void, regardless of the reasons thereof, or contain a loophole, validity of the other provisions shall not be affected thereby. Mainz, April 2009, Institut fr Mikrotechnik Mainz GmbH

REFERENCES

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Hessel, V., Renken, A., Schouten, J.C., Yoshida, J.-I.: Micro Process Engineering - A Comprehensive Handbook, three-volume edition, Wiley-VCH, Weinheim, 2009. Hessel, V., Lb, P., Lwe, H.; Volume 3, Part III, 9 Industrial Microreactor Process Development up to Production in: Micro Process Engineering A Comprehensive Handbook (eds.: Hessel, V., Renken, A., Schouten, J. C., Yoshida, J.-I.), 2009, pp. 185 247. Kralisch, D., Krtschil, U., Roberge, D. M., Hessel, V., Schmalz, D.; Volume 3, Part V, 13 The Economic Potential of Microreaction Technology in: Micro Process Engineering - A Comprehensive Handbook (eds.: Hessel, V., Renken, A., Schouten, J. C., Yoshida, J.-I.), 2009, pp. 281 296. Lb, P., Hessel, V., Simoncelli, A.; Microreactor Applications in the Consumer Goods Industry in Micro Process Engineering - A Comprehensive Handbook, Volume 2: Devices, Reactions and Applications, V. Hessel, A. Renken, J.C. Schouten, J.-I. Yoshida (Eds.), WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim, 2009. (Chapter 22 pp. 363-401). Hessel, V., Kolb, G., Brandner, J. J.; Microfabrication for Energy Generating Devices and Fuel Processors in: Microfabricated Power Generation Devices (eds.: Mitsos, A.; Barton, P. I.), Wiley-VCH, Weinheim, 2009, pp. 7 -37. Hessel, V., Lb, P., Lwe, H.; Industrial Microreactor Process Development up to Production in: Microreactors in Organic Chemistry and Catalysis (ed. Wirth, T.), Wiley-VCH, Weinheim, 2008, pp. 211-275. Schenk, R., Hessel, V., Jongen, N., Buscaglia, V., Guillemet-Fritsch, S., Jones, A. G.; Nanopowders produced using microreactors, Encyclopedia of NANOSCIENCE and NANOTECHNOLOGY, Vol. 7, 2003, pp. 287-296. Hessel, V., Lwe, H., Mller, A., Kolb, G.; Chemical Micro Process Engineering Processing and Plants, Wiley-VCH, Weinheim (2005). Hessel, V., Hardt, S., Lwe, H.; Chemical Micro Process Engineering Fundamentals, Modelling and Reactions, Wiley-VCH, Weinheim (2004). Ehrfeld, W., Hessel, V., Haverkamp, V.; Microreactors, in: Ullmanns Encyclopedia of Industrial Chemistry, Wiley-VCH, Weinheim (1999). V. Hessel, C. Serra, H. Lwe, G.Hadziioannou; Polymerisationen in mikro-strukturierten Reaktoren: Ein berblick, Chem. Ing. Tech. 77, 11 (2005) 39-59. Hessel, V., Angeli, P., Gavriilidis, A., Lwe, H.; Gas/liquid and gas/liquid/solid microstructured reactors contacting principles and applications, Ind. Eng. Chem. Res. 44, 25 (2005) 9750-9769. Hessel, V., Lb, P., Lwe, H.; Development of microstructured reactors to enable organic synthesis rather than subduing chemistry, Curr. Org. Chem. 9, 8 (2005) 765-787. Jhnisch, K., Hessel, V., Lwe, H., Baerns, M.; Chemistry in Microstructured Reactors, Angew. Chem. Int. Ed. 43, 4 (2004) 406-446. Kolb, G., Hessel, V.; Microstructured reactors for gas phase reactions: a review, Chem. Eng. J. 98, 1-2 (2004) 1-38. Pennemann, H., Watts, P., Haswell, S., Hessel, V., Lwe, H.; Benchmarking of microreactor applications, Org. Proc. Res. Dev. 8, 3 (2004) 422-439. Pennemann, P., Hessel, V., Lwe, H.; Chemical micro process technology from laboratory scale to production, Chem. Eng. Sci. 59, 22-23 (2005) 4789- 4794. Hessel, V., Lwe, H., Schnfeld, F.; Micro mixers a review on passive and active mixing priciples, Chem. Eng. Sci. 60 (2005) 2479-2501. Lb, P., Lwe, H., Hessel, V.; Fluorinations, chlorinations and brominations of organic compounds in micro structured reactors, J. Fluorine Chem. 125, 11 (2004) 1677-1694. Al-Rawashdeh, M., Hessel, V., Lb, P., Mevissen, K., Schnfeld, S.; Pseudo 3-D simulation of a falling lm microreactor based on realistic channel and lm proles, Chem. Eng. Sci. 63, 21 (2008) 51495159. V. Hessel, D. Kralisch, U. Krtschil; Sustainability through Green Processing Novel Process Windows intensify Micro and Milli Process Technologies, Energy Environ. Sci. 1, 4 (2008) 467- 478. Hessel, V., Knobloch, C., Lwe, H., Review on patents in microreactor and micro process engineering, Rec. Pat. Chem. Eng. 1 (2008) 1-16. Pennemann, H., Hessel, V., Kolb, G., Lwe, H., Zapf, R.; Partial oxidation of propane using a micro structured reactor, Chem. Eng. J. 135, 1 (2008) S66-S73. Rosenfeld, C.; Serra, C.; Brochon, C.; Hessel, V.; Hadziioannou, G.; Use of micromixers to control the molecular weight distribution in continuous two-stage nitroxide-mediated copolymerizations, Chem. Eng. J. 135, 1 (2008) S242-S246. Kolb, G., Cominos, V., Hofmann, C., Pennemann, H.; Schrer, J., Tiemann, D., Wichert, M., Zapf, R., Hessel, V., Lwe, H.; Integrated microstructured fuel processors for fuel cell applications, Chem. Eng. Res. Des. 83, 6 (2008) 626-633. Men, Y., Kolb, G., Zapf, R., Tiemann, D., Wichert, M., Hessel, V., Lwe, H.; A complete miniaturised microstructured methanol fuel processor / fuel cell system for low power applications, Int. J. Hydrogen Energy 33, 4 (2008) 1374-1382. Men, Y., Kolb, G., Zapf, R., Hessel, V., Lwe, H.; Ethanol steam reforming in a microchannel reactor, Trans. IChemE, Part B, Process Safety & Environmental Protection 85, B5 (2007) 1-6. Kolb, G., Schrer, J., Tiemann, D., Wichert, M., Zapf, R., Hessel, V., Lwe, H.; Fuel Processing in Integrated Microstructured Heat-Exchanger Reactors, J. Power Sources 171, 1 (2007) 198-204. Renken, A., Hessel, V. Lb, P., Miszczuk, R., Uerdingen, M.; Ionic liquid synthesis in a micro structured reactor for process intensication, Chem. Eng. Proc. (2007) Chem. Eng. Process 46, 9 (2007) 840-845. Lb, P., Hessel, V., Hensel, A., Simoncelli, A.; Micromixer based liquid/liquid-dispersion in the context of consumer good production with focus on surfactant vesicle formation, Chimica oggi Chemistry Today 25, 3 (2007) 26-29. Men, Y., Hessel, V., Lb, P., Lwe, H., Werner, B., Baier, T.; Determination of the segregation index to sense the mixing quality of scale-up concepts for pilot- and production-scale micro structured mixers, Trans. IChemE, Part A., Chem. Eng. Res. Dev. 85, A5 (2006) 1-8. Hardt, S., Schilder, B., Tiemann, D., Kolb, G., Hessel, V., Stephan, P.; Analysis of ow patterns emerging during evaporation in parallel microchannels, J. Intern. Heat & Mass Transfer 50, 1-2 (2007) 226-239. Lb, P., Pennemann, H., Hessel, V., Men, Y.; Impact of uid path geometry and operating parameters on l/l-dispersion in interdigital micromixers, Chemical Engineering Science 61 (2006) 2959-2967. Krtschil, U., Hessel, V., Kralisch, D., Kreisel, G., Kpper, M., Schenk, R.; Cost analysis of a commercial manufacturing process of a ne chemical using micro process engineering, Chimia 60, 9 (2006) 611-617. Zapf, R., Kolb, G., Pennemann, H., Hessel, V.; Basic study of the adhesion of several aluminabased washcoats deposited onto stainless steel microchannels, Chem. Eng. Technol. 29, 12 (2006) 1509-1512. Hessel, V., Serra, C., Lwe, H., Hadziioannou, G.; Polymerisationen in mikro strukturierten Reaktoren: Ein berblick , Chem. Ing. Tech. 77, 11 (2005) 39-59. Hessel, V., Lb, P., Lwe, H.; Direct uorination of aromatics with elemental uorine in microstructured reactors, Chimica oggi Chemistry Today 5 (2004) 10-15. Hessel, V., Hofmann, C., Lb, P., Lhndorf, J., Lwe, H., Ziogas, A.; Organic Process Research & Development, 9, 4 (2005) 479-489. Pennemann, H., Hessel, V., Lwe, H.; Chemical Engineering Science, 59, 22-23 (2004) 4789-4794. Lb, P., Hessel, V., Klefenz, H., Lwe, H., Mazanek, K.; Letters of Organic Chemistry, 2, 8 (2005) 767779. Pennemann, H., Forster, S., Kinkel, J., Hessel, V., Lwe, H., Wu, L., Org. Proc. Res. Dev., 9, 2 (2005) 188-192. Jhnisch, K., Dingerdissen, U.; Chemical Engineering and Technology, 28, 4 (2005) 426-427. Mller, A., Cominos, V., Horn, B., Ziogas, A., Jhnisch, K., Grosser, V., Hillmann, V., Jam, K. A., Bazzanella, A., Rinke, G., Kraut, M.; Chemical Engineering Journal, 107, 1-3 (2005) 205-214.

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ANNEX

Published by Institut fr Mikrotechnik Mainz GmbH Carl-Zeiss Str. 18-20 55129 Mainz, Germany www.imm-mainz.de catalogue@imm-mainz.de

For further questions please do not hesitate to contact us:

Institut fr Mikrotechnik Mainz GmbH Carl-Zeiss-Strae 18-20 55129 Mainz Phone: +49 61 31 / 990 - 0 Fax: +49 61 31 / 990 - 205 catalogue@imm-mainz.de www.imm-mainz.de

Status 05/2009