Institut für Mainz GmbH - CeeInd · group in Nancy, France (Ind. Eng. Chem. Res. 38, 3 (1999)...

> p r o c e s s t e c h n o l o g y o f t o m o r r o w m a d e b y i m m

5/06T H E C ATA L O G U E

Institut fürMikrotechnikMainz GmbH

PREFACE

Today’s micro reaction technology contributes substantially to the fi elds of chemistry, chemical engineering, energy generation, and many more. The trend is from micro reactor design to micro reactor process design, de-manding respective engineering skills. More and more applications are faced in-depth, plant engineering becomes an issue, and cost calculations decide about profi tability. Thus, we see that the technology, while on a reaction level displaying many more facets concerning diverse applications, con-siders now downstream processing to move to industry’s pilot and even pro-duction processing. The availabilityof complete plants with microstructu-red reactors has steered commercial interest. The incorporation of micro-structured reactors in existing plants at industrial sites is one preferred way for commercial use. Finally, there are fi rst pilot and production devices withmicrostructured reactors for fi ne-chemical industry and reports about corresponding industrial uses are distributed.

The new catalogue 2006 is refl ecting this trend. New versions of plants at lab-scale format (table-top) are in-cluded, as well as lab-scale plants with completely new functions such as the Cream Manufacture Plant, which is part of the emulsion activities at IMM. Recently, the technology of building pilot plants with microstructured reac-tors was introduced at IMM. The most visible outcome of this new technolo-gy branch is the nitro glycerine pro-duction plant at Xi’an North Huian Chemical Industry Co., Ltd. in Xi’an,

central China, capable of producing 15 kg/h nitro glycerine at a total liquid fl ow of about 100 l/h. This posed the request for pilot and production type microstructured mixers which resultedin an expansion and optimization of the Caterpillar (CPMM) series and StarLaminator (StarLam) series, re-spectively. In this way, the idea is sup-ported of having grouped-class de-vices for step-wise scale-out and as a technology offer for modular plant engineering.

The catalogue was also supplemented by some off-the-shelf tools coming from the fuel processing development at IMM like catalytic reactors, heat exchangers, and evaporators. Besidesapplications in the fi eld of energy tech-nology, this opens up the whole range of heterogeneously catalysed reationsof gas-solid type and, with some modi-fi cations in reactor design, of gas-liquid-solid type.

Finally, besides providing tools for plant engineering, the catalogue offer includes process engineering services as exemplarily illustrated by some recent process development studies. This crosses over from off-the-shelf delivery to customised solutions with respective reactors and the proposi-tion of process fl ows, which refers to the Micro Reactor Process Design, the motto of this editorial. Albeit not quoted herein, fi rst cost analyses have been performed and give answers on the return-on-invest and amortisation of equipment to justify the expenses for the new technology.

Hopefully, the ancient motif “Pánta Rhei” (All Things Flow), which is (not entirely correctly) ascribed to the pre-socratic Greek philosopher Heraklit,may hold for a signifi cant part of futurechemical industry. The generally opti-mistic attitude of that era is, without any doubt, also helpful and demanded for implementing a new, emerging technology.

Volker Hessel

Institut für Mikrotechnik Mainz GmbH

From Micro Reactor Design to Micro

Reactor Process Design

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IMM SALES TEAM

Prof. Dr. Volker HesselDirector R&[email protected]

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Prof. Dr. Holger LöweDirector R&[email protected]

Dr. Bernd WernerProduct [email protected]

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CONTENTS> s u p e r i o r p r o d u c t s m a d e b y i m m

Preface 1

IMM sales team 2

Contents 3

Testing and quality control 4

01 Processes

Introduction 6

Contents 7

Kolbe-Schmitt synthesis 8

Michael Addition 9

Solvent-free thiophene bromination 10

Synthesis of an imidazole-type ionic liquid 11

Phenyl boronic acid synthesis 12

(S)-2-Acetyl tetrahydrofuran synthesis 13

Synthesis of intermediate for quinolone antibiotic drug 14

Nitro glycerine production plant 15

Brominations of aromatics and alkylaromatics 16

Synthesis of an azo pigment dye, Yellow 12 17

Hydrogenation of nitrobenzene 18

Direct fl uorination of toluene with elemental fl uorine 19

Sulphonation of toluene 20

Direct hydrogen peroxide synthesis out of the elements 21

[4+2] cycloaddition of singlet oxygen to cyclopentadiene 22

to make cyclopentene-1.4-diol Side-chain photochlorination of toluene-2.4-di-isocyanate 23

02 Plants

Introduction 24

Contents 25

Organic Synthesis Plant 26

Cream and Emulsifi cation Plant 28

Falling Film Micro Reactor Plant 30

Gas Phase Reactor Test Plant 32

Fuel Processor Demonstration Plant 34

03 Components

Introduction 36

Contents 37

Overview applications 38

Mixing Principles 39

Liquid/Liquid and Gas/Liquid Mixers or Reactors 40

Special Gas Liquid Reactors 58

Gas Phase Reactors 62

Heat Exchangers 70

04 Accessories Introduction 76

Contents 77

Spare parts 78

05 Anex

General terms and conditions of sale 80

References 83

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TESTING AND QUALITY CONTROL

Testing and quality control of IMM

micro reactor devices and plants

People often complain that innova-tions need too much time and con-sume too much money until they are available for industry and society. This catalogue makes the fi 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 technologi-cal break-through.

The catalogue comprises both off-the-shelf products and demonstrators that are ready for supply according to cus-tomers needs. IMM is aware that de-spite the novelty of the devices, they have to fulfi l the demands of industrial processing. For this reason, we do not only invest in scientifi c and technolog-ical promotion of our devices, but alsoin quality control, improvement of robustness, supplying proper fl uid connections, etc.

First of all, our Quality Assurance policy is realised by a Quality Manage-ment System certifi ed according toDIN EN ISO 9001. For reasons of trans-parency the following specifi c technicalquality features are given additionally on the backside of each micro device‘s description in the catalogue:• Specifi cations• Options• Performance Data• Applications & References

Specifi cations

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

Options

Since different customers have differ-ent demands on how a reactor might fi t best to their intended application, materials, internal dimensions or simp-ly fl uidic peripherals may need to bechanged. IMM tries to serve such de-mands on customized solutions. For instance, we typically offer a variety of, e.g. different fl uid connectors, reac-

tion channel platelets made of various materials, or incorporation of specialtyfunctions (e.g. of an inspection win-dow).

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 fl ow rates, residence times and more, all based on experimental evidence. This ena-bles you to judge whether the device meets basic requirements of the pro-cess or not. Said data are supplemen-ted by geometric parameters compris-ing information on internal volumes or surfaces, in absolute terms or as specifi c properties. In addition to thesebasic, material- and construction-basedparameters, more detailed informationon processing is given, including de-scription of hydrodynamics such as fl 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 „Appli-cations & References“.

From all these contents of PerformanceData, three presently important as-pects are exemplarily discussed more in detail below.

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 isabsolutely essential for correct ba-lancing of all streams and avoiding contamination of the environment.

For this reason, devices are regularly controlled by inhouse leakage rate tests. IMM thereby applies known and recommended procedures for leak test-ing of large-scale apparatus which are modifi ed to the needs of microfl ow de-vices. The setting of these tests orientson ASME and EU standards on leak-age testing. If needed, leak tightness will be measured at elevated pressuresand 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 assemblymanual.

Performance characterization

IMM aims at disclosing the functioningof its devices largely as well as at show-ing their limits. Our devices can act as multi-purpose tools for a diversifi edrange of applications. The informationon these applications result from own or by partners practised chemistry as well as disclosed customer processes.

Beyond multi-functionality, we identi-fi ed application-unique uses for the micro devices and, vice versa, producemore 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 reac-tion processing. Besides such in-housetesting, the fi rst basic versions of the devices were usually tested by part-ners or third parties being experts in the fi eld of the micro device‘s applica-tion. This particularly provides an in-dependent assessment – either from the industrial or scientifi c point of view – concerning the performance of the devices. The results are document-ed in many peer-reviewed publicationswhich are referred in the respective device‘s description.

Development of measuring techniques

IMM does not only use state-of-the-artmeasuring techniques for device per-formance characterisation but also actively develops new techniques that

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are considered to comprise the essen-tial information for the customer. In this context, we would like to point out that IMM was the fi rst to suggest an advanced mixing test procedure for fl ow-through devices (besides simple visual inspection of colouring/neutralisation) by modifi cation of an approach used for batch apparatus originally, developed by the Villermauxgroup in Nancy, France (Ind. Eng. Chem. Res. 38, 3 (1999) 1075-1082).

Experimental Determination of Mixing

Performance of Microfl uidic 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 prin-ciples is available in the meantime. Therefore, there is an increased need for measuring and comparing mixing performance. IMM tests its micro mix-ers with regard to mixing performance experimentally using the so-called “Villermaux/Dushmann method”.

The determination of mixing perfor-mance by the Villermaux/Dushman method is based on the competition of two parallel reactions. The acid-cata-lysed reaction of potassium iodide with potassium iodate to elemental iodine competes with the faster neu-tralisation 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 solu-tion 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 com-proportionation reaction. The formediodine can be then detected as triiodidecomplex 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.

IMM uses the chemical protocol de-scribed by S. Panic et al. (Chem. Eng. J. 101 (2004) 409-419). In the following the concentrations and preparation ofthe two solutions, pumped in the ex-periments at a volumetric fl 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 volumetricratio of 1:1:

Solution 2a: c(KI) = 0.0319 mol/Lc(NaOH) = 0.0909 mol/Lc(H3BO3) = 0.0909 mol/L

Solution 2b: c(KIO3) = 0.00635 mol/Lc(NaOH) = 0.0909 mol/Lc(H3BO3) = 0.0909 mol/L

Applications & References

Information that is missing in the pro-duct 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 IMM‘s micro devices. Means, we limited this list to most relevant books and reviews.

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PROCESSES

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CONTENTS> p r o c e s s e s m a d e b y i m m

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Processes

Kolbe-Schmitt synthesis 8

Michael Addition 9

Solvent-free thiophene bromination 10

Synthesis of an imidazole-type ionic liquid 11

Phenyl boronic acid synthesis 12

(S)-2-Acetyl tetrahydrofuran synthesis 13

Synthesis of intermediate for quinolone antibiotic drug 14

Nitro glycerine production plant 15

Brominations of aromatics and alkylaromatics 16

Synthesis of an azo pigment dye, Yellow 12 17

Hydrogenation of nitrobenzene 18

Direct fl uorination of toluene with elemental fl uorine 19

Sulphonation of toluene 20

Direct hydrogen peroxide synthesis out of the elements 21

[4+2] cycloaddition of singlet oxygen to cyclopentadiene 22

to make cyclopentene-1.4-diol

Side-chain photochlorination of toluene-2.4-di-isocyanate 23

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KOLBE-SCHMITT SYNTHESIS

01Motivation and Results

Low pressure operations under refl ux conditions are typi-cally favored for laboratory fl asks and agitated tanks. Ac-cordingly, the maximum temperature of many organic routes is often simply defi ned by the solvent boiling point. Micro reactor rigs on the other side allow a simple opera-tion of liquid phases under high pressures and high temper-atures. 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 100°C higher than boiling points of typical solvents. This has been termed high-p,T processing. The faster operation at higher temper-atures typically is paid by more side and consecutive reac-

tions. Thus, effi cient mixing and shortening of residencetime to the kinetically limit become important drivers for process optimization.

For the aqueous-based Kolbe-Schmitt synthesis with re-sorcinol and phloroglucinol shortenings in reaction time by orders of magnitude (up to a factor of 2000) were achieved in this way. This benefi t is counterbalanced by thermal de-gradation 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 – 220°C• Reaction time: 4 – 390 s

Benefi ts through Process Intensifi cation

• Increase in space-time yield by factor 440• Increase in productivity by factor 4• Possibly circumventing the more tedious original Kolbe- Schmitt route with autoclave operation and aggressive earth alkaline hydroxide bases

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MICHAEL ADDITION

Motivation and Results

The merit of high-p,T processing (see initial chapter and under Kolbe-Schmitt synthesis for defi nition) was investi-gated for six Michael additions of two α,β-unsaturated car-bonyl 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 batchprocessing times is here much larger than kinetically need-ed to avoid too large heat releases and therefore the reactantis 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 -55°C, best operation was at 100°C, while the experiments were extended up to 200°C.

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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• 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%


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

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SOLVENT-FREE THIOPHENE BROMINATION


In batch processing aggressive reactants typically are dilutedto 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 pro-longs 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 con-trary, microstructured reactors with their effi cient heat and mass transfer have the potential to contact the full reactantload “all-at-once“. In addition, micro reactors can cope withconcentrated solutions or even pure liquid reactants. There are several examples known that such “all-at-once“ or sol-vent-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 thio-phene and pure bromine fl ows at temperatures from -10°C to room temperature. The micro reactor operation led to yields of 2,5-dibromothiophene up to 86%, at nearly com-plete 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 re-actor rig, a fast parametric study could be done for fi nding optimal operating conditions.


• Pressure: 1 bar• Temperature: -10 – 0°C• Reaction time: a few ms


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

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SYNTHESIS OF AN IMIDAZOLE-TYPE IONIC L IQUID


A variant of the novel chemistry concept is to use solvent-free processes with aggressive reactants which exhibit heat-transfer sensitivity. The exothermic synthesis of an ionic liquid was carried out in this way in a micro reactor rig, andaddresses especially the need for temperature control dur-ing 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 isfurther increased by favourably working without any sol-vents which is expected to result in temperature increase.The chemistry cannot be disclosed due to intellectual prop-erties rights of the industrial user.

Even under the advanced thermal control of a microstruc-tured reactor, one can observe for a thermostat tempera-ture of 50°C an increasing yellow colouring of the product, i.e. the formation of unwanted side products. This fi nding, however, can be explained by looking at the determined temperature profi les. Obviously, the reactor or the selected dimensions are not capable of removing reaction heat in a suffi cient manner. In order to improve heat removal for thehigher fl ow rates, an approach was to use fi 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 profi les becomes so impor-tant by locating the reactor section where smaller tubes haveto be used and therewith to minimise the use of smaller tu-

bes to where necessary. As can be seen from the temper-ature profi les, the heat removal capacity of the 1/8˝ tubes is suffi cient in large parts of the reactor, e.g. for a total fl ow rate of 3.48 ml/min beginning at a reactor volume of 15%.

In the following, therefore the fi rst two reactor sections where exchanged by 1/16˝ tubes with same internal vol-ume as the replaced 1/8˝ tubes. Exemplarily, the obtained temperature profi les with such a set-up for a total fl ow rate of 3.48 ml/min are given in Figure 7 with the corre-sponding profi le of the set-up with all 1/8˝ tube sections as comparison. The maximum temperature rise above thermostat temperature was reduced from 50°C to 10°C with this reactor modifi cation, yielding a clearer product. For the highest fl ow rate (6.96 ml/min) the modifi cation did not prevent hot spot formation, since a good portion of the reaction is occurring after the fi rst two tube sections and therewith not affected by smaller dimensions in the fi rst two tubes. With regard to production purposes based on these experimental results an adapted reactor con-cept for higher fl ow rates was derived. The micro reactor consists of a stack of platelets and heat removal is impro-ved 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.


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


• 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 – fl 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 shut- down

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PHENYL BORONIC ACID SYNTHESIS


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 pro-cess. 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 purifi cation.


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


• Increase of yield of pure product by 25%• Decrease of impurity level of crude product by factor 5, from 5% to 1%• Process simplifi cation: 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

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(S ) -2 -ACETYL TETRAHYDROFURAN SYNTHESIS


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 α-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 al-cohol 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 im-purity was 1.56%. Accordingly, with fi ne thermal and fl ow control, the productivity and economics of this process are increased.


• Pressure, Temperature, Reaction time: Not disclosed


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

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Individual impurity Optical purity

Batch 1.56% 97.7%

MRT 0.18% 98.4%

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SYNTHESIS OF INTERMEDIATE FOR QUINOLONE ANTIBIOTIC DRUG


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 anti-biotic drug, named Gemifl oxacin (FACTIVETM).

Among several types of reactors investigated, the micro-structured reactor was successfully applied to the synthesis of a pharmaceutical intermediate via a fast exothermic Boc protecting reaction step.


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


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

The reaction temperature was isothermally controlled at 15°C. By using the microstructured reactor the heat of reac-tion was completely removed so that virtually no bypro-ducts 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 0°C or -20°C to avoid side reactions.

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NITRO GLYCERINE PRODUCTION PLANT


A continuous nitro glycerine pilot plant with microstructuredmixer/multi-tube reactors was installed at Xi’an site in Chinaand was operated at a production rate of 15 kg/h nitro glyc-erine meeting all specs. A rough calculation for annual throughput gives a production rate of nearly 130 metric tonsper 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 safe-ty for all, even worst operational conditions. Therefore, all reactants must be pre-cooled before entering the micro-structured mixer. Also the mixer itself is actively cooled bymeans of an integrated heat exchanger as well as the multi-tubular reactor. Advanced simulations were made to solve the problems with equipartition volume fl ow through the multi-tube reactor and some new, specifi c micro-macro

interconnects for fl uid-fl 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. There-fore, the product quality must be on highest grade, and thetest runs indeed revealed higher selectivity and purity. Theplant could be operated safely; one of the next targets is tohave it fully automated. As a second step, a plant for down-stream purifi cation by washing and drying the nitro glyc-erine, of notably larger size and complexity as the reactor plant, is going to be developed and currently under nego-tiation. Environmental pollution should be excluded by advanced waste water treatment. In a fi nal stage, the micro reactor nitro glycerine plant may also encompass formula-tion and packaging.


• Pressure: 1 bar• Temperature: 30 – 40°C• Reaction time: some min


• 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

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BROMINATIONS OF AROMATICS AND ALKYLAROMATICS

01 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 200°C nearly complete conver-sion is achieved. The selectivity to the target product benzylbromide is reasonably high (at best being 85%; at 200°C and higher being 80%). The main sideproduct formed is thenitro-substituted benzal bromide, i.e. the two-fold brominatedside-chain product.


The bromination of meta-nitrotoluene is an example for ahigh-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 170°Cand 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


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


• Process simplifi cation: 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

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SYNTHESIS OF AN AZO PIGMENT DYE, YELLOW 12


By the use of microstructured mixers, pigment and other particle syntheses can be improved, since the well-defi nedand predictable mixing improves the preparation all the way from seed generation until particle agglomeration. In this way, fi ner particles with more uniform size distributionwere yielded for the commercial azo pigment Yellow 12.

The particles formed in the microstructured mixer have


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


• Benefi ts through process intensifi cation• 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

better optical properties such as the glossiness or trans-parency 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 profi tability of the pigment manufacture.

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HYDROGENATION OF NITROBENZENE

01 approached initially 100%. As side products, all intermedi-ates except phenylhydroxylamine were identifi ed. 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 wasgiven. For an impregnated palladium catalyst, complete conversion was achieved and maintained for six hours. Se-lectivity decreased with time, but remained still at a highlevel. The best performance of all catalysts investigated wasfound 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, preparedby different preparation routes, depends on the catalyst loading which is related to the preparation route. The largerthe 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 acti-vity was recovered, thus regaining complete conversion.


The hydrogenations of nitro aromatics have high intrinsicreaction rates, which however cannot be exploited by con-ventional reactors as they are unable to cope with the largeheat releases due to the large reaction enthalpies (500 –550 kJ mol-1). For this reason, the hydrogen supply is re-stricted, thereby controlling reaction rate. Otherwise, de-composition of the nitro aromatics or of partially hydro-genated intermediates can occur. The hydrogenations of nitro benzene over supported noble metal catalysts were investigated in a microstructured falling fi lm micro reactor.

For nitrobenzene hydrogenation, the overall mass transfer coeffi cient kLa was conservatively estimated (based on the fi lm thickness in the middle of the channels) to be in the range 3 – 8 s-1. As a comparison, for intensifi ed gas liquid contactors kLa can reach 3 s-1, but for bubble columns and agitated tanks it does not exceed 0.2 s-1.

A wide variation of preparation procedures for the palladi-um catalyst was tested. A sputtered palladium catalyst ex-hibited low conversion and large deactivation of the cata-lyst (60°C; 4 bar). The corresponding selectivity was also low. A slightly better performance was obtained after an oxidation / reduction cycle. Following a steep initial deacti-vation, the catalyst activity stabilised at 2 – 4% conversion and at about 60% selectivity. After reactivation, selectivity


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


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

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DIRECT FLUORINATION OF TOLUENE WITH ELEMENTAL FLUORINE

While for this reason the direct fl uorination needs hours in a laboratory bubble column, it is completed within secondsor even milliseconds when using a miniature bubble col-umn, operating close to the kinetic limit. Favourable elec-trophilic 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.


One way of process simplifi cation is to make molecular com-plex compounds out of much simpler building blocks (e.g. by multi-component one-pot syntheses like the Ugi reac-tion), at best directly out of the elements. Especially in thelatter case, this is often quoted as “dream reaction“. Typi-cally, such routes have been realised so far from hazardouselements, easily undergoing reaction, but lacking of selec-tivity. One example for this is the direct fl uorination starting from elemental fl uorine which was performed, e.g., with toluene.

Since the heat release cannot be controlled with conven-tional reactors, the process is deliberately slowed down.


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


• 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 simplifi cation

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SULPHONATION OF TOLUENE


Toluene is heated up to 40°C using a microstructured heatexchanger while at the same time liquid sulphur trioxide isheated up to 60°C in order to evaporate it. Nitrogen is furtheradded 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 fl 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 can-not be converted further but the mixed anhydride reacts inthe residence time module with toluene and forms the de-sired 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 fi nal hydration step has not


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


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

taken place. Even so, fi 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 deter-mined. Evidently, with increasing SO3/toluene mole ratio, the selectivity of the undesired by-products decreases whilethe selectivity of sulfonic acid stays nearly constant. At amole ratio of 13/100, the selectivity of sulfonic acid is ap-proximately 80% while that of sulfone decreases to approx-imately 3% and that of the sulfonic acid anhydride to ap-proximately 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 ortho-sulphonic 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.

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DIRECT HYDROGEN PEROXIDE SYNTHESIS OUT OF THE ELEMENTS


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 circui-tous 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 rea-sons by breaking the radical chain by enhanced wall colli-sion in the small channels with their large specifi c interfaces.

Using this direct route to hydrogen peroxide, basic engineer-ing for a new site for the production in the order of about 150,000 t hydrogen peroxide per year was done by UOP. Pi-lot processing and economic calculation of the production process has been performed. Based on microstructured

mixing units, the new process is realised by direct contact-ing of hydrogen and oxygen (without inert gas) in the pres-ence of a heterogeneous catalyst. The key to a high selec-tivity is to have a noble-metal catalyst in a partially oxidisedstate. 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. Itcould be clearly shown that improved selectivity and con-version 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).


• 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


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

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[4+2] CYCLOADDITION OF SINGLET OXYGEN TO CYCLOPENTADIENE TO MAKE CYCLO-PENTENE-1.4 -DIOL

01 Low-intensity light sources should give effi cient 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 cyclopenta-diene by singlet oxygen to 2-cyclopentene-1.4-diol was de-monstrated. The explosive intermediate endoperoxide was generated and without isolation used on-site for a sub-sequent hydration reaction.


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 µm,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 coeffi cient, is not over the tolerablelimit since only small optical paths are employed. It is as-sumed that molecules in thin liquid layers face a broadly similar photon fl ux, unlike macro-scale photo processing.


• High quantum effi ciency• 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


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

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SIDE-CHAIN PHOTOCHLORINATION OFTOLUENE-2.4 -DI - ISOCYANATE


Side-chain photochlorination of toluene isocyanates yieldimportant industrial intermediates for polyurethane syn-thesis, one of the most important classes of polymers. The motivation for micro channel processing stems mainly fromenhancing the performance of the photo process. Illumi-nated thin liquid layers should have much higher photon effi ciency (quantum yield) than given for conventional pro-cesssing. In turn, this may lead to the use of low-intensity light sources and considerably decrease the energy con-sumption 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 ex-periments in a batch reactor at 30 min reaction time result-ed in a space-time yield of only 1.3 mol/(l h), hence are by orders of magnitude smaller. By using an iron plate, space-time yields up to 346 mol/(l h) were achieved in the Falling Film Micro Reactor.

Conversions from 30% to 81% at selectivities from 79% to67%, respectively yields from 24% to 54%, were found whenusing a Falling Film Micro Reactor (4.8 – 13.7 s; 130°C). Control experiments in a batch reactor (30 ml reaction vol-ume) 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.


• High quantum effi ciency• 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


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

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PLANTS

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CONTENTS> p l a n t s m a d e b y i m m

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Plants

Organic Synthesis Plant OSBP 26

Cream and Emulsifi cation Plant 28

Falling Film Micro Reactor Plant FFMR-BSP 30

Gas Phase Reactor Test Plant 32

Fuel Processor Demonstration Plant 34

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ORGANIC SYNTHESIS PLANTOSBP

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OSBP for 2-step reaction

Principle

In micro reactor literature, the most frequently used approach for organic synthesis is the micro mixer/tube reac-tor. The organic synthesis bench-scale unit relies on this concept and has inaddition control and measuring func-tions. It is based on the reliable hybrid concept of IMM, utilizing innovative micro reactor components in connec-tion with well-proven conventional small-fl uidic equipment. IMM has gain-ed huge experience with carrying outorganic reactions e.g. ethoxy silylations, metal-organic syntheses, and epoxida-tions 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 of-fered now. It comprises two pre-heat-ing loops (as option: microstructured heat exchangers), a micro mixer, a 5/2-way valve, and 4 delay loops ofdifferent length collected to one outletwhich allows to change the residence time for a given set of parameters dur-ing the reaction by simply switching the valve. On demand, the general bench-scale unit concept can be modi-fi ed towards more complex design.The concept is amenable to supercrit-ical processing as well.

OSBP for single-step reaction (top view)

OSBP for single-step reaction (inside view)

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Typical fl ow charts for Organic Synthesis Plant

Pilot-scale plant for nitro glycerine production

Operating Conditions

Temperature (°C) -50 – 180

Pressure stability (bar) 30 for stainless steel 3 for PTFE

Flowrate (l/h) 0.05 – 2.5 for mixer SIMM-V2 2.5 – 30 for mixer CPMM-V1.2-R600/12

Residence time (s) 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) Leakage Class L0.1

Specifi cation 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 fi ts into a heating bath

Options

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

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 suffi cient, 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 mic-ro chemical process engineering.

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CREAM AND EMULSIF ICATION PLANT

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Cream Synthesis Plant for 5 different chemicals

Prototype of a Cream Synthesis Plant

Principle

Generating emulsions is typically a process where all materials are being balanced or measured, placed in a fl askor vessel and then vigorously stirred or homogenised with high energy con-sumption. Micro mixers insofar proved in literature to reduce energy input byfactor 10. Besides, more narrow dro-plet size distribution can be achieved within a shorter time as conventionaltechniques 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 multi-tude of different pastes, creams, lotionswithin short time can be produced as samples or in larger amounts.

The CSµCE-Demonstrator is based on the reliable hybrid concept of IMM, uti-lizing innovative micro reactor compo-

nents in connection with well-proven conventional small-fl uidic equipment. Respectively, small gear ring pumps for max. to 1 – 15 l/h depending on typeand 140°C are used to convey up to 4 liquids and 4 solids being molten in the comprised heat bath into a mixer array as the 8 Component CaterpillarMicro Mixer (8CCPMM) directly yield-ing the hot emulsion. The 4 solid com-ponents can be fed via temperature-controlled heated funnels into tempe-red fl ask whereof being pumped, en-abling a full continuous processing even in case of production need. The liquids are heated up with simple heat-ing loops, bath-fed or electrically drivenheat exchangers depending on total fl ow rate need.

On demand, the general bench-scale unit concept can be modifi ed towards more complex design. The concept is amenable to unusual processing as well.

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Cream Synthesis Plant for 8 different chemicals and continous use (top view)

Cream Synthesis Plant for eight different chemicals and continous use (bottom view), not fully assembled

Three caterpillar mixer structures to mix 4 chemicals at once

Seven caterpillar mixer structures to mix 8 chemicals at once made of PMMA


Temperature (°C) 20 – 140

Pressure stability (bar) 20 for stainless steel 3 for PTFE

Flowrate (l/h) 2.5 – 60

Leakage Class L0.1


• 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 fi ts into a heating bath

Options

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

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FALLING F ILM MICRO REACTOR PLANTFFMR-BSP

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Falling Film Micro Reactor Plant

Operation in the Falling Film Micro Re-actor device can be performed up to 180°C at a pressure of max. 10 bar by using the standard version (upper housing with inspection glass) or max. 20 bar with the special upper housing without window. The suitable liquid fl ow rates depend on the channel ge-ometry of the corresponding reaction plate and the property of the reactant (e.g. viscosity). For example, the max. liquid fl ow rate by using isopropanol and a channel size of 1200 µm x 600 µmis 1.5 l/h.

Principle

The Falling Film Micro Reactor Bench-Scale Plant comprises besides the Fall-ing Film Micro Reactor, a mass fl ow controller for the gas fl ow, a cryostat, a supply- and a withdraw-pump for theliquid fl ow. The precise assortment of the peripheral equipment components basically depends on the different che-mical reactions which the customer wants to perform. This means, the gen-eral bench-scale unit concept can bemodifi ed towards more complex de-sign.

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Flow charts of a Falling Film Micro Reactor Plant


Temperature (°C) 180

Pressure stability (bar) 10 (without Borofl oat glass: 20) Flowrate (l/h) 0.05 for channel geometry 300 µm 0.6 for channel geometry 600 µm 1.5 for channel geometry 1200 µm

Residence time (s) 0.8 – 20

Liquid fi lm thickness (µm) 25 – 100

Leakage Class L0.01

Technical Data

Name Falling Film Micro Reactor Plant

Order number FFMR-BSP

Connectors (Inlet/Outlet) 1/4˝ / 1/4˝

Material of FFMR 1.4571 for housing and reaction plate copper for cooling plate borofl oat glass for inspection glass Standard mixing 300 x 300 (64 channels) channels of FFMR (µm) 600 x 600 (32 channels) 1200 x 1200 (16 channels) Options Other materials like Hastelloy, Monell or Titan on request

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• Mass fl ow controllers• Temperature and pressure measurement unit• Process control system


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

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GAS PHASE REACTOR TEST PLANT

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

Principle

This bench-scale unit serves for inves-tigations in heterogeneous catalysis with respect to fossil fuel and alcoholfuel processing, e.g. concerning thedetermination of the activity/selectivityand 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 fl ow velocity, and gas composition.The bench-scale unit comprises com-mercial mass-fl ow controllers for con-trol of the gas feed, fl ame arresters tostop fl ame propagation, and a micro-structured evaporator fed by a liquid

tank, which produces steam or organicvapours (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 to900°C at a pressure of 10 bars, using external resistance heating. The cata-lyst is usually introduced into the microchannels prior to interconnection, e.g. by the wash-coat route and subsequentimpregnation. By laser-welding the thermal treatment is spatially confi ned

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 other-source micro reactor can be integratedinto this bench-scale unit. In this case,please contact IMM prior to the con-struction of the bench-scale unit so that the required modifi cations can be arranged.

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In conjunction with bench-scale unit construction, IMM serv-ices include provision of a manual which contains, besides general information, detailed documentation on experiencesgained with operation of this bench-scale unit. Exemplarily, operational modes are given so facilitating the fi rst experi-mental steps when starting bench-scale unit operation. Incase of further questions and desires, an IMM contact per-son can be consulted by mail or phone.

By special request, a process parameter monitoring pro-gram 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 meth-

anation. Besides constructional changes in the set-up, this requires the coating of another catalyst. IMM has in partic-ular gained experience in building bench-scale units for allkind of fuel processing unit operations and in operating re-spective micro devices. An extension of the use of bench-scale units for other types of heterogeneous catalytic studiesis principally possible and requires in most cases only minormodifi cations 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, meth-anol and ethanol steam-reforming, partial oxidation of pro-pane, water-gas shift at high and low temperature, preferen-tial oxidation of carbon monoxide, and for the methanation of carbon monoxide.

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Options

• Additional mass-fl ow controllers (e.g. for air, oxygen)• Additional periphery heating (pipes)• Additional liquid storage tanks (required for long term operation)• Additional temperature sensors


• Mass fl ow controllers for hydrogen, nitrogen, hydro- carbons, carbon monoxide, carbon dioxide, air and water (choice of selection optional)• Stainless steel vessels for water and organic liquids• Evaporator• Valves, manometers, fl ame arresters• Temperature controllers• Pressure controller (optional) • All above devices mounted on a metal frame• Available IMM-reactors for testing catalyst performance

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FUEL PROCESSOR DEMONSTRATION PLANT

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Principle

This test bench serves for investiga-tions in reactor performance testing with focus on fuel processing applica-tions such as fossil and alcohol fuel reforming and catalytic CO-clean-up. The unit is designed for tests of start-up, 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, wa-ter-gas shift and preferential oxidation reactors) are integrated into the unit. Fast serial variation of process para-meters such as temperature, pressure,gas fl ow velocity, and gas compositionare possible.

Test bench for single reactors and multiple reactor arrangements

The test bench comprises commercialmass-fl ow controllers for control of thegas feed, fl ame arrestors to stop fl ame propagation, and various evaporator types (evaporation power between 10 s of watts up to kilowatts). The evapora-tor, which is fed by a liquid tank, pro-duces 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 conven-tional reactor type (metallic monolith or fi xed bed reactor). Operation in themicrostructured reactors may be per-formed up to 900°C at pressures of upto 5 bars, for maximum temperature

of 500°C at pressures up to 100 bars, using either external resistance heat-ing or integrated catalytic burners. Also internally cooled reactors (heat exchangers) and combinations of thesereactor types may be tested in the test bench. By-pass lines are introduced, thus allowing for switching off the in-dividual reactors under test. The cata-lyst is usually introduced into the microchannels prior to the sealing procedure(normally laser-welding), e.g. by the wash-coat route and subsequent im-pregnation. By laser-welding the ther-mal treatment is spatially confi ned so that the catalyst is not destroyed during interconnection.

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Please contact IMM prior to the construction of the test bench so that the modifi cations required can be arranged.

In conjunction with test bench construction, IMM servicesinclude provision of a manual which contains, besides gen-eral information, detailed documentation on experiences gained with operation of this bench-scale unit. Exemplarily, operational modes are given so facilitating the fi rst experi-mental steps when starting bench-scale unit operation. In case of further questions and requests, an IMM contact per-son can be consulted by mail or phone.

By special request, a process parameter monitoring program

based on the LabView software can be supplied that allowsautomatic data acquisition of temperature and pressure.

The bench-scale unit was in detail investigated for steam-reforming 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 modifi ed to allow for in-vestigations 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.


Max. pressure (bar) 10 Max. reservoir of water or organic 20 liquid for one continious run (l) Max. fl owrate (gas) approx. (Nl/min) about 500

Max. fl owrate (liquid) approx. (g/h) about 5000 Max. evaporator temperature (°C) 200

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


• Mass fl ow controllers for hydrogen, nitrogen, hydro- carbons, 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, fl ame arresters • All above devices mounted on a metal plate• Available Reactors

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COMPONENTS

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CONTENTS> c o m p o n e n t s m a d e b y i m m

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Components

Liquid/Liquid and Gas/Liquid Mixers or Reactors

Overview Applications 38

Mixing Principles 39

Caterpillar Split-Recombine Micro Mixer CPMM-V1.2 group class-R300, -R600, -R1200, -R2400 40

Star Laminator StarLam group class -30, -300, -3000, -30000 44

Slit Interdigital Micro Mixer SIMM group class SIMM-V2, HPIMM, SIMHEX, SSIMM 48

Liquid/Liquid Micro Reactor LLMR-MIX 52

SuperFocus Interdigital Micro Mixer SFIMM-V2 54

Impinging-Jet Micro Mixer IJMM 56

Special Gas Liquid Reactors

Falling Film Micro Reactor FFMR 58

Micro Bubble Column MBC 60

Gas Phase Reactors

Gas Phase Micro Reactor GPMR 62

Gas Phase Micro Reactor with Mixer and Internal Heating/Cooling GPMR-Mix 64

Catalyst Micro Burner Reactor CMBR 66

Catalyst Testing Micro Reactor CTMR 68

Heat Exchangers

Counter-fl ow Micro Heat Exchanger WT-series 70

Tube Heat Transfer Micro Device THTMD 72

Laboratory Evaporator 74

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03Applications Type of Standard Mixers and Reactors Application Examples Liquid/liquid and gas/liquid reactions SIMM, CPMM, StarLam, SFIMM-V2 • 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 Gemifl oxacin (FACTIVETM) • Isomerisation of allyl alcohols • H-transfer reduction of citraconic acid ester • Aromatic nitrations • Aliphatic nitrations

Special gas/liquid reactions FFMR, MBC, SIMM, CPMM and StarLam • Direct fl uorination of toluene • Sulfonation of aromatics • Hydrogenation of nitrobenzene • Hydrogenation of cinnamic acid esters

Reactions at high pressure HPIMM • Alkylation of aromatics with supercritical CO2

Dispersion and emulsion formation SIMM, CPMM, StarLam • Mixing of silicon oil and water • Mixing of diesel and water

Mixing of liquids differing in viscosity SFIMM-V2, SIMM, StarLam • Addition reaction with liquid ethylene oxide synthesis

Particle and pigment synthesis CPMM, StarLam, IJMM • Azobenzene type formation • Calcium carbonate, titanates and oxalates powders • Amide formation • Bisquarternization of amines (Menschutkin reaction)

Photochemical reactions Produced with window: • [2+2] Diels Alder photooxygenation SFIMM-V2, FFMR, MBR of olefi nes • Photochemical chlorination of alkylaromatics Reactions with catalytic suspensions Made of glass: TIMM, RIMM • Direct H2O2 synthesis CPMM • Hydrogenation of C=C double bonds

OVERVIEW> a p p l i c a t i o n s

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Triangular

Tilted jets

Split-recombine Multi-lamination Jet collision

Ramp-up/downInterdigital

disk array

Caterpillar

CPMMStar Laminator

StarLamImpinging-jet

IJMM

Triangular

Super-Focus (V2)

SFIMM

Slit

Standard

SSIMM

Version 2

SIMM-V 2

Heat Exchanger

SIMHEX

High-Pressure

HPIMM

Tilted jetsInterdigital channel array

> m i x i n g p r i n c i p l e s b y i m m

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Principle

The Caterpillar Micro Mixers are partic-ularly suitable for applications where fast mixing at higher throughput is de-sired, providing highest performance for l/l-mixing as well as for g/l- or l/l- dispersing. As they consist of a struc-tured single channel, these devices may also be used successfully if preci-pitation occurs during the reaction or if fi ne slurries shall be processed.

The higher fl owrates enable productionscales 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 materi-als and safety gains.

Caterpillar Micro Mixers use a different mixing principle, called “split-and re-combine”: Dividing the streams, fold-ing/guiding over each other and re-combining them per each mixing step, consisting of 8 to 12 such steps. This ideally ends up in 512 to 4096 fi ne la-mellae, each approximately 2.4 µm wide. Mixing fi nally occurs via diffu-sion within milliseconds, exclusive of residence time for the multi-step fl ow passage. Additionally, at higher fl ow-rates – as determined by simulations –turbulences add to this mixing effect, improving the total mixing quality further.

CPMM group class

Simulated “real“ fl ow profi les at high fl ow rates in caterpillar mixers

Split-and-recombine mixing principle shown for two of eight mixing steps

CATERPILLAR SPLIT-RECOMBINE MICRO MIXER CPMM-V1.2 GROUP CLASS-R300, -R600, -R1200, -R2400

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CPMM group class

CPMM-R1200/8 CPMM-R2400/10

CPMM-R300/12

This standard version 1.2 of the Caterpillar Micro Mixers isprovided with welded-in tubing or HPLC-connectors enab-ling 50 – 100 bar system pressure for l/l-mixing or for g/l-, l/l-dispersing. Operation temperatures are limited through the used gasket materials to -40 – +220°C but can be extended

by use of graphite gaskets to 500°C. Thus, as fi ne slurries can be processed, heterogeneously catalysed high-temper-ature and -pressure reactions are easily performed in small hold-up volumes.

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The Caterpillar Micro Mixers with straight outlet are partic-ularly suitable for applications where fast mixing is desired though precipitation occurs during the reaction or if fi ne slurries shall be processed. Due to the construction princip-le only 30 bar system pressure can be applied, nonetheless enabling production of slurries containing up to some 100 kg per year of fi ne powders. These mixers consist of a single structured mixer channel with an adapted outlet. As the

CPMM with a straight outlet CPMM with a straight outlet made of PP

emerging reaction fl uid is not forced to leave the mixer via the 90° elbow fl ow confi guration 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 suitab-le special housing materials as e.g. PTFE.

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CATERPILLAR SPLIT-RECOMBINE MICRO MIXER CPMM-V1.2 GROUP CLASS-R300, -R600, -R1200, -R2400

Technical Data

Name Caterpillar Caterpillar Caterpillar Caterpillar Caterpillar Caterpillar Caterpillar Caterpillar Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- bine Micro bine Micro bine Micro bine Micro bine Micro bine Micro bine Micro bine Micro Mixer R300 Mixer R600 Mixer R1200 Mixer R2400 Mixer R300- Mixer R600- Mixer R1200- Mixer R2400- straight outlet straight outlet straight outlet straight outlet

Order number CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- R300 R600 R1200 R2400 R300-so R600-so R1200-so R2400-so

Mixing principles Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- Split-Recom- bine bine bine bine bine bine bine bine

Size (L x B x H) 60 x 45 x 20 60 x 45 x 30 60 x 45 x 30 79 x 45 x 30 51 x 45 x 20 51 x 45 x 30 51 x 45 x 30 70 x 45 x 30

Connectors (Inlet/Outlet) 1/16˝ / 1/8˝ 1/8˝ / 1/8˝ 1/8˝ / 1/4˝ 1/4˝ / 3/8˝ 1/16˝ / 1/16˝ 1/8˝ / 1/8˝ 1/8˝ / 1/8˝ 1/4˝ / 1/4˝

Standard mixing 300 x 300 600 x 600 1200 x 1200 2400 x 2400 300 x 300 600 x 600 1200 x 1200 2400 x 2400 channels (µm)

Standard material 1.4435 1.4435 1.4435 1.4435 1.4435 1.4435 1.4435 1.4435

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


Order number CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- CPMM-V1.2- R300 R600 R1200 R2400 R300-so R600-so R1200-so R2400-so

Temperature (°C) -40 – 220 -40 – 220 -40 – 220 -40 – 220 -40 – 220 -40 – 220 -40 – 220 -40 – 220

Pressure stability (bar) 100 100 100 100 30 30 30 30 Flowrate (l/h) 0.5 – 4 2 – 40 4 – 80 15 – 250 0.5 – 4 2 – 40 4 – 80 15 – 250

Residence time (ms) 3.6 – 72 2.25 – 45 3.15 – 70.2 3.6 – 60 5.4 – 108 2.7 – 54 4.05 – 81 4.32 – 72 Inner volume (µl) 10 25 78 250 15 30 90 300

Max Viscosity (mPas) 100 100 100 100 100 100 100 100 Leakage Class < L0.001 < L0.001 < L0.001 < L0.001 < L0.01 < L0.01 < L0.01 < L0.01

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CPMM-R2400/10-HEX-ss-wt assembled and disassembled CPMM-R2400/10-HEX-SO-ss-wt assembled with straight outlet connector and integrated heat exchanger

8CCPMM-R1200/8.7-PMMA 4CCPMM-R952/8.2-R1200/8.1-ss-hplc

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

As an additional feature the Caterpillar Micro Mixers may be offered with an integrated heat exchange function partic-ularly suitable for applications where pre-heating/-coolingof the mixture is desired prior to the subsequent reactor (bymeans of e.g. heat exchanger delay loop) thus extending

the application range to more exothermic reaction or appli-cation 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.

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The StarLam family

capacity microstructured mixers reach-ing volume fl ows up to the m3/h do-main. The apparatuses yield at higher fl ow rates a mixing effi ciency which compares the high performance of today’s low-capacity (l/h) micro mixers. Therefore, continuity from the “real” micro mixers over the herein describedhigh-throughput tools to convention-ally manufactured static mixers with even higher fl ow rates is given. A classifi cation of the mixing effi ciency versus the power input confi rms this

Principle

The Star Laminators are the fi 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 fi nely-dispersed injection of two fl 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 large-

STAR LAMINATORSTARLAM GROUP CLASS-30, -300, -3000, -30000

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continuity as well. For the Star Lami-nator StarLam 3000 e.g. a throughput of about 3 m3/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.

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StarLam 30000 StarLam 3000 StarLam 300 StarLam 30

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Order number StarLam 3000 StarLam 300 StarLam 30 Temperature (°C) -40 – 220 -40 – 220 -40 – 220 Pressure stability (bar) 100 100 100 Flowrate (l/h) 600 – 8000 80 – 1000 12 – 150

Residence time (ms) 72 – 960 1.7 – 220 24 – 840 Inner volume (ml) 160 5 2.8

Max Viscosity (mPas) 10000 10000 10000

Leakage Class < L0.001 < L0.001 < L0.001

Technical Data

Name Star Laminator 3000 Star Laminator 300 Star Laminator 30 Order number StarLam 3000 StarLam 300 StarLam 30 Mixing principles Multi-Lamination Multi-Lamination Multi-Lamination

Size (L x B x H) 95 x 95 x 150 40 x 40 x 64 40 x 40 x 64

Connectors (Inlet/Outlet) DN 15/DN 25 8 mm/10 mm 8 mm/10 mm

Standard mixing channels (µm) 250 100 50 Standard material Body: 1.4571 Body: 1.4571 Body: 1.4571 Foils: 1.4401 Foils: 1.4401 Foils: 1.4401

Options 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

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The feed plates of the StarLam series (here StarLam 3000), which are alternately stacked. A star-like plate serves for fl 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.

mance of the Star Laminators is reached which then com-pares with the high quality of the smaller micro mixers, supplied by IMM. When plotting mixing effi ciency 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 effi ciency is yielded independent which micro-structured 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 straightfor-ward manner, e.g. if fouling was noted. The circular outlet channel has macroscopic dimensions so that also here par-ticles will not be detrimental.

The foils of the Star Laminators are fabricated by laser cut-ting; the housing is made by precision machining.

Principle

The Star Laminators are the fi rst real high-capacity produc-tion tools of IMM for mixing purposes. They create an alter-nate, interdigital-type feeding array which is generated by stacking thin foils with star-like through-holes. In this way, a fi nely-dispersed alternating injection of the two multi-splitted fl uid streams is achieved, resulting in the addition of fl uid ring per fl uid ring to the center fl ow in the mixing chamber superposed by turbulent fl ow regime. The foil stack is inserted into the recess of a housing where it is tightened by applying compression.

Concerning the high fl ow rates used for practical applica-tions, mixing occurs by turbulence. As to be expected, theStarLam apparatus cannot be used at very low fl ow rates, as simulations and reaction-type mixing experiments con-fi rm. In this fl ow regime, a segregation of fl uid layers is giv-en so that mixing is here not effective enough. On the con-trary, at high fl ow rates experimental characterization of mixing effi ciency by using competitive reactions shows thatby increased turbulent action an increasing mixing perfor-

StarLam 30/300 disassembled

StarLam 3000 foils during assembly on the assembly rods

Mixing channel

AB

A

B

A

Mixing channel

AB

A

B

A

Feed plates of StarLam 30, 300 and StarLam 3000

StarLam 3000

StarLam 30StarLam 300

StarLam 3000

StarLam 30StarLam 300

STAR LAMINATORSTARLAM GROUP CLASS-30, -300, -3000, -30000

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

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SIMM group class

SSIMM

SIMM-V2 HPIMM

SIMHEXSSIMM

SIMM-V2 HPIMM

SIMHEX

Interdigital mixing principle

Interdigital fl ow passes slit to create multi-lamellae

Principle

This group class of micro mixers is a classic amongst all IMM chemical mi-cro 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 fl ow pattern created by multi-lamination with geo-metric focussing which speeds up liquid mixing.

Due to this double-step mixing, the slit mixers are amenable to wide variety ofprocesses such as mixing, emulsifi ca-tion, single-phase and multiphase or-ganic synthesis. Extensive knowledgeon hydrodynamics, mixing perform-ance and reaction engineering for di-verse applications of these mixers has been documented worldwide.

SLIT INTERDIGITAL MICRO MIXER SIMM GROUP CLASS S IMM-V2, HPIMM, SIMHEX, SSIMM

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Temperature (°C) -40 – 220 Pressure stability (bar) 100 Flowrate (l/h) 0.04 – 2.5

Residence time (ms) 14.4 – 720 Inner volume (µl) 8

Max Viscosity (mPas) 10000

Leakage Class < L0.001

SIMM-V2 HPIMM


Temperature (°C) -40 – 500 Pressure stability (bar) 600

Flowrate (l/h) 0.04 – 2.5

Residence time (ms) 27 – 1350 Inner volume (µl) 15



Technical Data

Order number SIMM-V2 Mixing principles Multi-lamination

Size (L x B x H) 30 x 40 x 30

Connectors (Inlet/Outlet) 1/16˝ / 1/16˝ HPLC Standard mixing channels (µm) 45 x 200

Standard material Body: 1.4571 Inlay: 1.4435 Options Other materials like Hastelloy, Monell or Titan on request

Technical Data

Order number HPIMM Mixing principles Multi-lamination

Size (L x B x H) 25 x 21 x 37

Connectors (Inlet/Outlet) 1/16˝ / 1/16˝ HPLC Standard mixing channels (µm) 25 x 21 x 37


Principle

This version has all the benefi ts of mixing using multi-lami-nation and focusing only. Deliberately avoiding volume ex-pansion, the inner volume could be decreased to only 8 µl, coming along with improved fl 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 micro mixer 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 fl 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.

Individual parts of the SIMM-V2 device Individual parts of the HPIMM

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Principle

This micro mixer was optimized considering a heat exchangefunction within the mixer, using a graphite sealing for tight-ening 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 expansion-free outlet channel geometry, i.e. renounces on jet mixing, but relies on multi-lamination and geometric focusing only.

SLIT INTERDIGITAL MICRO MIXER SIMM GROUP CLASS SIMM-V2, HPIMM, SIMHEX, SSIMM

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Slit Interdigital Mixer Heat Exchanger (SIMHEX) Standard Slit Interdigital Micro Mixer (SSIMM)

SIMHEX SSIMM

Principle

This micro mixer is the classic one amongst all IMM chemi-cal micro processing products. It combines the regular fl owpattern created by multi-lamination with geometric focuss-ing 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 µl and is only offered with non-stainless soft tube connectors.

Technical Data

Order number SIMHEX Mixing principles Multi-lamination

Size (L x B x H) 25 x 25 x 20

Connectors (Inlet/Outlet) 1/16˝ / 1/16˝ HPLC Standard mixing channels (µm) 40 x 300

Standard material Body: 1.4571 Inlay: 1.4401

Options Other materials like Hastelloy, Monell or Titan on request; incl. heat exchanger function

Technical Data

Order number SSIMM Mixing principles Multi-lamination

Size (L x B x H) 19 x 30 x 16.5

Connectors (Inlet/Outlet) 1/16˝ / 1/16˝ soft tube Standard mixing channels (µm) 45 x 200





Residence time (ms) 18 – 900

Inner volume (µl) 10






Residence time (ms) 72 – 3600 Inner volume (µl) 40



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Laser-cut Inlay for HPIMMLaser-cut Inlay for SIMHEXLaser ablation Inlay for SIMM-V2 and SSIMM

This inlay fi ts the standard mixer as well as the version 2.

For both versions the inlays have a sizeof 11.0 mm x 7.5 mm and ~ 3.6 mm thickness with different possible chan-nel sizes and depths.

The following inlays are available:• Laser-ablation (channel width 45 µm, 200 µm channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request, order number SMI-Lasab45200• LIGA technology (channel width 25 µm or 40 µm) made from silver or nickel on copper with 300 µm channel depth, order numbers SMI-Ni25, SMI-Ni40, SMI-Ag25 or SMI-Ag40• ASE (thermally oxidised silicon, channel width 30 µm or 50 µm) with 100 µm 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 fi 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 µm, 250 µm channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request, order number SMHXI-45250

This inlay fi ts the high-pressure slit mixer exclusively.

The size of HPMI inlays: 8.0 mm in diameter and 250 µm in thickness

The following inlays are available:• Laser-cutted inlays (channel width 45 µm, 250 µm channel depth) made of stainless steel (SS 316L) as standard but other materials like Hastelloy etc. or other channel dimensions on request, order number HPMI- Las45250

Slit mixer inlays

SMI (for SIMM-V2 and SSIMM)

SIMHEX inlays

SMHXI

High pressure mixer inlays

HPMI

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Principle

The Liquid/Liquid Micro Reactor is mainly designed for highly exothermic reactions and can also be applied for contacting two immiscible liquids andperforming a reaction thereby. It com-prises two microstructured plates with integrated micro mixer and micro heat exchanger. Insofar, it is particularly designed for reactions that benefi t from excellent heat transfer as well as fast mass transfer. The heat trans-fer is provided by specifi c surfaces of 6.770 m2/m3 in micro channels of a width of 200 µm at an aspect ratio of 6, whilst the fast mass transfer derives from the meanwhile incorporated in-terdigital micro mixer, known from the SIMM series.

The LLMR-MIX can be offered of dif-ferent materials on request besides the standard stainless steel. Flow rates

Liquid/Liquid Micro Reactor with internal Mixer – LLMR-MIX

LIQUID/L IQUID MICRO MIXERLLMR-MIX

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from 50 ml/h up to 2 l/h are feasible, with residence times in the 0,3 – 12 s range. The reactor can be used up to50 bar and 180°C (Viton, Chemraz gasket) or higher if graphite is applied.

Detail of the internal mixing section

The laser-cut inlay of the LLMR-MIX

53

LLMR-MIX-HC276 disassembled LLMR-MIX explosion drawing

LLMR-MIX made of Hastelloy LLMR-SY; a reactor with internal arrangement of 4 LLMR-MIX including delay loop


Temperature (°C) -40 – 200 Pressure stability (bar) 50 Flowrate (l/h) 0.05 – 2

Residence time (s) 0.3 – 12 Max Viscosity (mPas) 1000


Technical Data

Name Liquid/Liquid Micro Reactor Order number LLMR-Mix Mixing principles Multi-lamination Size (L x B x H) 45 x 120 x 26

Connectors (Inlet/Outlet) 1/16˝ / 1/16˝ for chemicals 1/4˝ / 1/4˝ for cooling fl uid

Standard mixing channels (µm) 45 x 200 Standard cooling channels (µm) 200 x 1200 Standard material Housing, reaction and cooling plate: 1.4571 Inlay: 1.4401 Options Other materials like Hastelloy, Monell, Titan or plastics on request

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Principle

Focusing mixers perform a multi-laminating step and geo-metrically focus the streams (in a way similar to hydrody-namic focusing) to thin the lamellae and then mix by diffus-ion. Physically speaking, this means having a nozzle feed array, a triangular-type focusing chamber and a thin mixing channel. The novel SuperFocus Mixer Version 2 (SFIMM-V2)bases upon the simulation, design and characterisation of theformer 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 focus-ing ratio, e.g. to reduce the sensitivity towards blockage. Thenovel SuperFocus mixer thus combines both high through-put, which is e.g. characteristic of the StarLam series and uniform fl ow patterns, which is e.g. characteristic for the SIMM components.

Compared to the predecessor design more nozzles enable fl uid feed. The nozzle width was enlarged, thus being lessparticle sensitive, albeit the fi nal focused lamellae width of about 4 µm was kept, i.e. the focusing ratio was increased from 40 formerly to now 178 (and can be set higher on de-mand). To arrange as many as 138 nozzles, a large circular arc was chosen for the feed array. The mixing channel widthand length compares to the former design so that the semi-analytical and experimental reaction type based fi ndings onthe mixing time can be largely transferred to the new design. Although steel is employed as construction material, an op-tional inspection window may allow the monitoring of the fl ow patterns and of the mixing course.

For the new SuperFocus SFIMM-V2 throughput of about 350 l/h at a pressure loss of 3.5 bar was determined for wa-tery systems. The formation of fl ow patterns is very uniform,i.e. a multi-lamellae fl ow is found all over the focusing cham-ber until the mixing channel is reached. The known devia-tions from ideal given for any multi-lamellae fl ow are found as well, e.g. that lamellae are thicker at the wall (boundary) than in the interior of the fl ow. In particular this deviation should be less here compared to other systems, as the ratioof outer to inner lamellae is 136:2.

SuperFocus microstructured mixer SFIMM-V2 Central plate of the SFIMM-V2

The mixing time achievable is 4 ms according to calculationand experiments made with the former design, albeit ex-cluding the time needed for fl owing through the focusing chamber. The latter is dependent on the volume fl ow. Spe-cialty designs with notably reduced focusing time are pos-sible. The same holds for integrated mixing-heating elementconfi gurations, allowing one to perform fast temperature switches for starting and ending reactions in a very short, defi ned time frame, as e.g. done in quench-fl ow analysis.

Disassembled SFIMM-V2

SUPERFOCUS INTERDIGITAL MICRO MIXERSFIMM-V2

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Multi-lamellae fl ow in the SuperFocus microstructured mixer SFIMM-V2


Temperature (°C) -40 – 220 Pressure stability (bar) 100 Flowrate (l/h) 10 – 300 Max Viscosity (mPas) 10000 Leakage Class < L0.001

Technical Data

Name SuperFocus Interdigital Micro Mixer Version 2 Order number SFIMM-V2 Mixing principles Multi-lamination Size (L x B x H) 140 x 140 x 40


Standard mixing channels (µm) 500 µm x 5 mm Number of feeding channels 138 Width of feeding channel 260

Focusing ratio 178

Standard material 1.4435 Options Other materials like Hastelloy, Monell or Titan on request; heat exchanger function is possible

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

Impinging-Jet Micro Mixer

Principle

Deliberately slow mixing is an issuewhen fast mixing would have deleter-ious effects on processing, e.g. by plugging the whole system. As a mat-ter of fact, most organic processes areassociated with more or less precipita-tion during the course of reactions. Particle generation is simply not pos-sible in the vast majority of today’s 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 confi guration. It was shown that the smaller the jet dia-meter, the better the mixing quality. Intense knowledge on jet confi gura-tion as a function of fl ow rate and jet diameter has been documented, in addition to mixing quality judgement.

As a result, the nozzles of the jet mixerhave tiny, only 350 µm wide nozzles. The mixer has been tested for inor-ganic 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.

IMPINGING-JET MICRO MIXERIJMM

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Temperature (°C) -40 – 220

Pressure stability (bar) 10 Flowrate (l/h) 0.5 – 3

Residence time (ms) 0

Inner volume (µl) 0 Max Viscosity (mPas) 100 Leakage Class < L0.001

Technical Data

Name Impinging-Jet Micro Mixer Order number IJMM Mixing principles Jet collision Size (L x B x H) 10 x 35 x 10

Connectors (Inlet/Outlet) 1/8˝ / 1/8˝ Clamp screw

Standard boring-/noozle 350, 500, 1000 diameter d (µm)

Orientation angles (d) 45°, 60°, 90°

Standard material 1.4571 Options Other materials like Hastelloy, Monell or Titan on request

IJMM in a special funnel-like housing for particle production Geometric parameters determine the mixing performance, beside fl ow parameters

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FALLING F ILM MICRO REACTORFFMR

Falling Film Micro Reactor

Thermographic monitoring: Initial wetting fl ow

Principle

The Falling Film Micro Reactor utilizes a multitude of thin falling fi lms that move by gravity force for typical residencetimes of seconds up to about one minute. Its unique proper-ties are the specifi c interface of 20,000 m2/m3 and the good temperature control by an integrated heat exchanger. Such high mass and heat transfer were achieved performing di-rect fl uorination of toluene with elemental fl uorine in this device. This so far uncontrollable and highly explosive re-action could be managed under safe conditions and with control over the reaction mechanism. Via an electrophilic pathway, a yield of 20% of o- and p-mono-fl uorinated iso-mers was achieved.

Fundamental studies on mass transport were carried out using the carbon dioxide conversion in alkaline media. It turned out that higher space-time yields are achievable thanin conventional packed columns. Heat characteristics were monitored on-line and at real time by IR thermography withsub-micro channel spatial resolution. By CFD simulation, theparabolic fl ow pattern evolution was characterized. The good fl ow equidistribution by a pressure barrier was con-fi rmed by analytical calculations and experimental fl ow visualization.

Meanwhile, the Falling Film Micro Reactor was successfully used by many customers for such important gas/liquid pro-cesses as oxidations and hydrogenations. By means of washcoating, catalyst and carrier can be deposited in the reactionchannels so that gas/liquid/solid processes are amenable. For hydrogenation of nitro benzene at Pt/alumina contact almost complete conversion was achieved within a few seconds.

Falling fi lm principle in a multi-channel architecture

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Disassembled FFMR Reaction plates for FFMR FFMR made of Hastelloy C276

Technical Data

Name Falling Film Micro Reactor Order number FFMR Size (L x B x H) 120 x 76 x 40


Material 1.4571 for housing and reaction plate Copper for cooling plate Borofl oat glass for inspection glass

Standard mixing channels 300 x 300 (64 channels) (µm) 600 x 600 (32 channels) 1200 x 1200 (16 channels)

Standard cooling channels Width: 1.5 (mm) Depth: 0.5 Options Other materials like Hastelloy, Monell or Titan on request


Temperature (°C) 180 Pressure stability (bar) 10 (without Borofl oat glass: 20 bar) Flowrate (l/h) 0.05 for channel geometry 300 µm 0.6 for channel geometry 600 µm 1.5 for channel geometry 1200 µm


Liquid fi lm thickness (µm) 25 – 100 Leakage Class L0.01

Interfacial area (m2/m3) 20000

volume of gas chamber (mm3) 13336 Total inner volume (mm3) 1800 Active inner volume (mm3) 110

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Row of outlet holes for separate multi-phase fl ow in reaction channels

Gas/liquid UV-LIGA contacting unit

Micro Bubble Column

Principle

The Micro Bubble Coloumn performsdisperse-type gas/liquid contacting, similar to its macroscopic analogue. The fl ow patterns, however, resemble those of fl ow in small-channel mono-liths, such as slug, annular or spray fl ow, whereas the bubbly fl ow known for bubble columns is found only in small region of stability.

The Micro Bubble Column is a gas/liq-uid contacting device for very rapid re-actions, typically in the order of one second and below. The strength of this device is the possibility to switchbetween all these distinct fl ow pat-terns, by virtue of changing gas andliquid superfi cial velocities. The infor-mation to do so has been thoroughly documented in fl ow-pattern maps of various types such as Baker charts. In the two most prominent fl ow patterns, the slug and annular ones, mass trans-fer from gaseous to liquid phase is strongly enhanced via using very thin (~ 50 µm) liquid fi lms.

The Micro Bubble Column has an in-spection window for monitoring fl owpatterns. An integrated heat exchangerserves for proper temperature control.The mixing device is made via UV litho-graphy/electroforming with gas feed channels’ dimensions down to 3 µm to achieve equipartial gas distribution within the parallel channels.

The high mass and heat transfer of the Micro Bubble Column were outlined by performing direct fl uorination of toluene with elemental fl uorine. Thisso far uncontrollable and highly explo-sive reaction could be managed under safe conditions and with control over reaction mechanism. Via an electro-philic pathway, a yield of 20% of o- and p-mono-fl uorinated isomers was achieved. Fundamental studies on mass transport were carried out usingthe carbon dioxide conversion in alka-line media. It turned out that higher space-time yields are achievable than in conventional packed columns.

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MICRO BUBBLE COLUMNMBC

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Principle of gas/liquid fl ows in MBC Disassembled Micro Bubble Column MBC


Temperature (°C) 180 Pressure stability (bar) 30 Flowrate (ml/h) 5 – 100

Residence time (s) 0.14 – 0.56

Liquid fi lm thickness (µm) 30 – 70 Leakage Class L0.01

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Technical Data

Name Micro Bubble Column Order number MBC Size (L x B x H) 95 x 50 x 36 Connectors (Inlet/Outlet) 1/8˝ / 1/8˝

Material 1.4571 for housing and reaction plate Nickel (LIGA) for micro dispersion unit Copper for cooling plate Borofl oat glass for inspection glass

Size of micro dispersion 7 x 20 x 600 for gas (64 channels) unit (µm) 20 x 20 x 600 for liquid (64 channels)

Size of reaction channel Width: 200 µm plate Depth: 70 µm Length: 60.5 mm

Size of cooling channels (mm) Width: 3 Depth: 0.5 Length: 40

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GAS PHASE MICRO REACTORGPMR

Gas Phase Micro Reactor

Principle

The Gas Phase Micro Reactor com-prises a stack of several microstruc-tured plates (generally 10 + 10 plates) that are arranged for counter-fl ow or co-current fl ow practice. Each plate consists of 34 parallel micro channels of 300 µm width and 200 µm depth. The plate stack is encompassed by twoceramic Macor® plates, for thermal in-sulation 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 beoperated as gas-phase reactor, eitherwith or without internal heat transfer.

Intense studies on periodic reactions were made with this reactor by threewell-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 themicro channels can be offered as well.Most commonly, wash coating of dif-ferent carriers, e.g. of various alumi-nas, and subsequent catalyst impreg-nation are applied. Coprecipitation and sol-gel techniques were applied as well for catalyst deposition.

The device can also be used as a gas-phase and/or liquid-phase micro heat exchanger.

Counter-fl ow principle

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Plate coated with catalystGas phase reactor installed in bench-scale plant


Temperature (°C) 500 Pressure stability (bar) 3 Flowrate (l/h) liquid/gas 1 – 7 / 1 – 600

Leakage Class L0.1

Heat transfer area (m2/m3) 18000 Total inner surface per layer (mm2) 580 Specifi c inner surface per layer (m2/m3) 2900 Active inner volume per layer (mm3) 32 Operation mode Counter- or co-current fl ow

Technical Data

Name Gas Phase Micro Reactor Order number GPMR Size (L x B x H) 70 x 70 x 55

Connectors (Inlet/Outlet) 1/8˝

Standard material 1.4571 for housing and catalyst carrier Glass ceramics MACOR for insulation layer

Number of catalayst plates 20 Size of catalyst plate (mm) 40 x 40 Channel geometry of the catalyst plates (µm) 300 x 200 Options GPMR is also usable as a single heat exchanger; end caps for heating cartridges

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GAS PHASE MICRO REACTOR WITH MIXER AND INTERNAL HEATING/COOLING GPMR-MIX

Gas Phase Micro Reactor with Mixer and Internal Heating/Cooling

Top housing plate of reactor with mixer and reactor stack

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

Principle

The Gas Phase Micro Reactor with Mixer and Internal Heating/Cooling GPMR-MIX contains two recesses, each fi lled with one stack of microstructured platelets, which are con-nected via a conduit. Both stacks are connected to welded tubes, serving for feed and fl uid withdrawal.

The fi rst stack comprises two types of mirror-imaged platelets with parallel feeding channels which are alternately arranged so that a multi-lamination fl ow confi guration is created for gas mixing. In the conduit attached, form-ing a fl 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 assmall as possible. As a result, investi-gations in the explosive regime are safely amenable, as demonstrated by research with this and similar tools.

The second stack comprises plateletswith parallel channels of small depth so that very good heat transfer is pro-vided. By this means, hot-spots arereduced and near-isothermal operationcan be achieved. The platelet construc-tion material itself may act as catalyst or, more preferably, the channels maybe coated with a catalyst layer, e.g.

wet chemically using the wash-coatroute or by means of thin-fi lm deposi-tion. A small total mass of the con-struction 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. 100K/min), even when approaching rela-tively large temperatures, e.g. up to600°C. Internal cooling typically of similar time scale is provided by con-vection fl ow of a gas stream at highfl ow rate in a channel which surroundsthe functional units.

The mixer-catalyst zone reactor has been extensively studied for its use forethylene oxide synthesis. Among otherresults of the parametric study, safe operation in the ex regime (3 vol.-% ethylene, 50 vol.-% oxygen, balancenitrogen; 5 bar; 4 l/h; 277°C), 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; 290°C), not far from the industrial benchmark, and higher conversions at comparable selectivity compared to fi xed-bed technology (20 vol.-% ethy-lene, 80 vol.-% oxygen; 0.3 MPa; 3.17 l/h; 230/250°C) were demonstra-ted.

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Individual parts of GMPR-Mix Mixer and reaction platelet Laser-cut mixer platelets


Temperature (°C) 600 Pressure stability (bar) 50 Flowrate (l/h) 5


Leakage Class < L0.1 Specifi c surface area (m2/m3) 12700 Total inner surface per reaction layer (mm2) 54 Specifi c inner surface per reaction layer (m2/m3) 3840 Active inner volume per layer (mm3) 2.5

Technical Data

Name Gas Phase Micro Reactor with Mixer and Internal Heating Order number GPMR-MIX Size (L x B x H) 40 x 40 x 30

Connectors (Inlet/Outlet) 1/4˝

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

Number of mixing plates 10

Size of mixing plates (mm) 7.5 x 7.5

Channel geometry of mixing plates (µm) 180 – 490 x ~ 100 Number of catalayst plates 10

Size of catalyst plate (mm) 9.5 x 9.5 Channel geometry of the catalyst plates (µm) 460 x 125

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CATALYST MICRO BURNER REACTORCMBR

Principle

The Catalyst Micro Burner Reactor is atesting 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/catalystsystems. The CMBR was designed for testing the catalysed burning of fuels

Catalyst Micro Burner Reactor

with different catalysts, however, it may be as well applied as a testing re-actor for all kind of heterogeneous gas phase reactions at fl ow-rates exceed-ing the range of small-scale laboratory devices.

Heating of the reactor is realised by heating cartridges with temperature determination feasible at two positionsinside the reactor.

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The Catalyst Micro Burner Reactor isdesigned for a power generation in therange of several hundreds of Watts byburning various fuels. Full conversionof 32 g/h methanol was achieved witha conventional Pt-catalyst at 130°C re-action temperature. No other productsthan carbon dioxide and water were found above the detection limit. Thus absence of bypass effects could be proven.

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Single parts of the Catalyst Micro Burner Reactor


Temperature (°C) 550 Pressure stability (bar) 5 Flowrate (l/h) 10 – 150

Residence time (ms) 0.10 – 1


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Name Catalyst Micro Burner Reactor Order number CMBR Size (L x B x H) 160 x 120 x 50 Connectors (Inlet/Outlet) 1/4˝

Standard material 1.4571

Number of catalayst plates 1 – 16 Size of catalyst plate (mm) 50 x 50 Channel geometry of the catalyst plates (µm) 600 x 400

Micro channel surface area per platelet (mm2) 588

Options Other materials on request

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Catalyst Testing Micro Reactor with end caps for parallel operation

Stack of cartridges with coated micro-structured plates

Two end caps for parallel operation

Principle

The Catalyst Testing Micro Reactor con-sists of a housing comprising twentymicro structured plates positioned pair-wise face to face resulting in ten levelsof parallel microchannels. On demand,the micro structured plates can be coated with various carrier/catalystsystems. They are easily exchangeableusing 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 micro reactor in serial or in parallel mode.

Parallel operation (1 in, 10 out):

Using a diffuser-type end cap, the microstructured plates are fed simul-taneously 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 us-ing ten different gases (at similar pres-sure) can be applied by assembling thereactor with two end caps for parallel operation.

10 levels with different catalysts and/ or different gases.

Screening or numbering-up of cata-lysts.

Serial operation (1 in, 1 out):

Using two other end caps similar in shape, the one inlet stream fl ows seri-ally in a zigzag manner from one plate to the other, being turned around and guided to the next level and so on, fi nally resulting in a path of ten times length compared to the single plate length, respectively ten times the resi-dence time.

Up to 10 plates with identical catalyst may be installed.

Variation of the reactor length.

CATALYST TESTING MICRO REACTORCTMR

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Special version for 800°C and 20 bar operation

Standard version disassembled Alternative heating option with one heat jacket instead of 10 heat cartridges

Technical Data

Name Catalyst Testing Micro Reactor Order number CTMR Size (L x B x H) 100 x 100 x 108

Connectors (Inlet/Outlet) 1/4˝ / 1/16˝ for parallel operation 1/8˝ / 1/8˝ for serial operation

Standard material 1.4841 for housing 1.4742 for catalyst plates

Number of catalayst plates 20 Size of catalyst plate (mm) 50 x 14 Options Other materials on request


Temperature (°C) 800 Pressure stability (bar) 20 (100 bar at 400°C) Standard fl ow velocity (m/s) 0.4 – 40

Residence time (ms) 0.025 – 2000


Options

Catalyst plates can be delivered with various channel geometries:

Channel geometry (width µm x depth µm): 2900 x 300 Number of channels: 3 2000 x 300 4

1000 x 300 7

1000 x 100 7

750 x 300 9

750 x 100 9

500 x 300 12

500 x 100 12

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COUNTER-FLOW MICRO HEAT EXCHANGERWT-SERIES

Principle

The novel WT-series was developed as a heat exchanger for liquid/liquid, gas/liquid or gas/gas applications andcan also serve for evaporation or con-densation. They comprise a laser weld-ed stack of arranged microstructured plates enabling a counter- or co-currentfl ow scheme. Being assembled withconventional 1/4” or 3/8” tubes, easy integration into the existing tubing sys-tem of pilot- or small-scale productionplants is possible.

The core elements are chemically

Counter-fl ow Micro Heat Exchanger group class (WT-series), WT-404, WT-304, WT-204 (from left to right)

etched microstructured plates, sealed by high-precision laser welding. These new heat exchangers are normally de-signed for fl ow rates between 1 l/h upto 400 l/h; higher fl ow rates of up to 1000 l/h are possible at moderate pres-sure drops. The high effi ciency and heat transfer coeffi cients of the micro channels are even more enhanced compared to conventional heat ex-changers due to the low material thick-ness (low heat resistance) and high inner specifi c surface.

Single plates of the WT…08-series

Single plates of the WT…04-series

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Special type HxA Special Heat Exchanger, also for condensing

HCOMH

Technical Data

Name Micro Heat Exchanger Series Micro Heat Exchanger Series Micro Heat Exchanger Series Order number WT 204 WT 304 WT 404 Size (L x B x H) 60 x 24 x 23 80 x 34 x 32 100 x 44 x 42

Connectors (Inlet/Outlet) 1/4˝ / 1/4˝ 3/8˝ / 3/8˝ 3/8˝ / 3/8˝

Material 1.4571 1.4571 1.4571

Number of heat exchanger plates 34 50 66 Dimensions of heating channels (µm) 800 x 400 800 x 400 800 x 400


Temperature (°C) up to 500 up to 500 up to 500 Pressure stability (bar) 5 5 5 Flowrate (l/h) 0.5 – 50 2.5 – 250 6 – 600

Leakage Class L0.1 L0.1 L0.1

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Tube Heat Transfer Micro Device

Principle

The Tubular Heat Transfer Micro Deviceis a microstructured heat exchanger, designed for electrical heating of gas-es and liquids. The optimized size ofthis device allows a very fast heatingup as well as fast changes of tempera-tures. Being offered in two sizes, themaximum power rate to be transferredcan be up to 800 W with a thermal effi -ciency > 90% (depending on operationconditions).

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 thermo- couples and electronic control unit

THTMD in parts before laser-welding

Technical detail of heat exchanger structure

In the latter case, the temperature ofthe heating process is basically con-trolled 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 300°C and 45 bars.

TUBE HEAT TRANSFER MICRO DEVICETHTMD

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Explosion drawing of THTMD Heat control system for THTMD


Temperature (°C) up to 500 Pressure stability (bar) 45 Flowrate (l/h) liquid 1.0 – 20.0

Power rate (W) 800

Thermal effi cieny > 90%

Leakage Class L0.1

Technical Data

Name Tube Heat Transfer Micro Device Order number THTMD Size (L x B x H) 120 x 100 x 15


Material 1.4571

Number of heating channels 60 Width of heating channels (µm) 400 Options Other materials like Hastelloy, Monell or Titan on request

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LABORATORY EVAPORATOR

Temperature control unit with integrated mass fl 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 fl ow as well as the elec-trical heating and its temperatures to ensure the continuous use. Rapid pre-heating, evaporation and over-heatingare realized in one single device. Two

electrical heating cartridges supply theheat to the corresponding microstruc-tured plates with large specifi c surfacesfor excellent heat transfer.

Up to 100 g/h water (without carrier gas) can be evaporated. A maximum temperature of 350°C for the vapour or up to 6 bar system pressure are feasible.

LV1 – Laboratory evaporator for 100 g/h

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LV1 – with open heating housing LV1 – disassembled


Temperature (°C) 400 Pressure stability (bar) 6 Temperature (°C) of Vapor up to 350

Flowrate (g/h) 10.0 – 100.0

Power rate (W) 400

Technical Data

Name Evaporator System Order number LV1 Size (L x B x H) 300 x 300 x 360


Material 1.4301

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ACCESSORIES

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CONTENTS> a c c e s s o r i e s m a d e b y i m m

Accessories

Spare Parts

Gaskets for all types of micro reactors G-… 78

HPLC-fi ttings/-adaptors HPLC-f-… 78

Pre-fl anged PTFE tubing 1/8“ P-ft-… 78

Micro Bubble Column MBC-… 79

MBC-MDU200 79

Falling Film Micro Reactor FFMR-… 79

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SPARE PARTS

Pre-fl anged tubing to connect e.g. CPMM-SpMa-…

Gaskets for all types of

micro reactors G-…

HPLC-fi ttings/-adaptors

HPLC-f-…

Pre-fl anged PTFE tubing

1/8“ P-ft-…

HPLC-fi ttings/adaptors

1/16”

1/16”

M5

M3

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Although we attached great import-ance on durability of the applied gas-kets for our micro devices, the misuse of temperature, chemicals and/or sol-vents may destroy them. Therefore, it is sometimes unevitable to change such needed parts by time.

As a matter of fact, mostly the ubiqui-tous material Viton® was used wherev-er possible as it is offering a very goodprice-to-quality level. In cases that is not suffi cient we apply Chemraz 505 black seals or – at least – try to offer as an optional spare part. Both materials can be applied for temperatures -30°C –+220°C.

Some unique micro devices must use graphite as sealing as nothing else iscapable of the applied conditions; analternative in some cases is Klingersil®.Further special materials may be of-fered upon inquiry.

These special adaptors are being usedto connect 1/16” tubing with the threadinlet of mixers and reactors. They en-able the use of small tubing (less hold-up volume) at higher pressures; made of stainless steel 1.4401 (SS 316) in-cluding ferrule and nut.

Actually available are two types of adaptors for different threads:• M3 thread – 1/16” HPLC connection system, e.g. for the Standard Slit Interdigital Mixer• M5 thread – 1/16” HPLC connection system, e.g. for the Caterpillar Mixer

As special equipment for the Cater-pillar Micro Mixers these soft tubes are offered. Their maximum operation pressure is 10 bars/145 psig. 1/8“, ID 2.0 mm, delivered as 1 m length.

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Micro Dispersion Unit for MBC Top plate window for MBC Reaction plates for FFMR

Micro Bubble Column

MBC-…

Falling Film Micro Reactor

FFMR-…

Micro Dispersion Unit

MBC-MDU200

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• The micro dispersion unit MBC-MDU- 150 (made of nickel by LIGA) is necessary for using the reaction plates MBC-REAC50 (50 x 50 µm) (stainless steel1, cavity sinking by EDM) and MBC-REAC200 (200 x 70 µm) (stainless steel1, wet etched)

• The MBC-MDU200 (made of nickel by LIGA) is suitable for the MBC-REAC- 100 (100 x 50 µm) (stainless steel1, cavity sinking by EDM) and MBC- REAC300 (300 x 100 µm) (stainless steel1, wet etched)

• Top plate with window in PMMA (MBC-TpWIN-PMMA), PC (MBC- TpWIN-PC) or borofl oat glass (MBC- TpWIN-fl oat)

1Stainless steel: 1.4571 (316Ti)

• Reaction plates made of stainless steel1, wet etched:- FFMR-REAC300SS (300 x 100 µm)- FFMR-REAC600SS (600 x 200 µm)- FFMR-REAC1200SS (1200 x 400 µm)

• Reaction plates made of Hastelloy2

(cavity sinking by EDM):- FFMR-REAC300HC (300 x 100 µm)- FFMR-REAC600HC (600 x 200 µm)- FFMR-REAC1200HC (1200 x 400 µm)

1Stainless steel: 1.4571 (316Ti)2Hastelloy: Hastelloy C-22, 2.4602 (B 575)

• Inspection glasses:- Made of borofl oat glass, FFMR- WIN-fl oat- Made of fused silica, FFMR-WIN-fs

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GENERAL TERMS AND CONDITIONS OF SALE

1. General

1.1 The general terms and conditions of sale (“Sales Conditions”) set forth herein apply to all delivery items or services supplied by Institut für Mikrotechnik Mainz GmbH, Carl-Zeiss-Str. 18-20, 55129 Mainz, Germany, VAT-ID-Number DE149054596 (“Seller“) to a purchasing company (“Pur- chaser”) in a sales transaction. Seller does not accept Purchaser‘s conditions which are contradictory to or diverging from these Sales Conditions unless Seller expressly approves their validity in writing. These Sales Conditions also apply in case Seller supplies Purchaser without reservations even though contradiction or divergence of the Purchaser’s conditions from these Sales Conditions is known to Seller.

1.2 All agreement between Seller and Purchaser concerning performance of the contract at hand is set down in writing therein. For the avoidance of doubt, subsidiary agreements not set down in writing do not exist.

1.3 These Sales Conditions only apply to entrepreneurs.

2. Offer – Additional Offer Documents – Samples

2.1 Text of purchase orders has to contain Seller‘s reference number.

2.2 Provided that the order states an offer in accordance with § 145 BGB (German Civil Code), Seller is entitled to accept the order within ten (10) working days after receipt.

2.3 Seller’s offers are not binding unless expressly stated otherwise.

2.4 Paragraph 10 of these Sales Conditions shall apply additionally.

3. Performance Specifi cation

3.1 Specifi cations of delivery items and products are based on Seller’s general experience and knowledge, and shall only state labelling or guideline values.

3.2 Specifi cations concerning condition and possible use of Seller’s products do not imply any guarantee, particularly not in accordance with §§ 443, 444, 639 BGB (German Civil Code), unless they are expressly labelled as such in writing. Solely our legal representatives and authorized offi cers are authorised to issue a guarantee.

3.3 Delivery items may be subject to deviations as far as customary in trade or technically inevitable and not unreasonable for Purchaser.

3.4 In view of paragraph 3.1 and 3.2 Purchaser is obliged to test the delivery item’s suitability for the intended purpose.

4. Prices – Payment Terms

4.1 Unless otherwise agreed by Seller in the order confi rmation, prices are quoted in EURO and are effective “ex works“ (EXW) according to the respectively relevant version of Incoterms, dispatch extra.

4.2 Prices do not include value added tax which – if mandatory – will be declared separately on the invoice at the rate effective at the invoice‘s date.

4.3 In case of unusual, substantial increases in costs after conclusion of the contract, e.g. in Seller’s or Seller’s suppliers’ costs for material, energy or freight, and shall these rises lead to a considerable increase of Seller’s purchase prices or prime costs, Seller is entitled to demand negotiations with Purchaser for price adjustment immediately.

4.4 Outside of paragraph 4.3 Seller reserves the right to appropriate price changes in case of cost decrease or increase after conclusion of the contract, particularly if due to changes in cost of materials or due to wage settlements.

4.5 Invoices are payable net within 30 days as of invoice date. 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 fi rst rate. The second rate is due after delivery. Bills of exchange and cheques are only accepted on explicit agreement. 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.

4.6 In case of late payment, statutory provisions apply. Particularly, Purchaser has to pay interest at 8 percentage points above the current base rate of the European Central Bank on Seller‘s claim.

4.7 Purchaser is not entitled to set off with counterclaims unless said claims are legally confi rmed, undisputed or have been accepted by Seller. Furthermore, Purchaser is entitled to lay a lien on his payment as far as the counterclaim is based on the same contractual relationship.

4.8 Seller’s prices apply for the scope of performance and delivery that has been agreed. Additional or special performances will be charged separately.

5. Delivery Terms – Transfer of risk

5.1 Delivery will be ex works (EXW) according to the respectively relevant version of Incoterms unless otherwise defi ned in the order confi rmation. 5.2 Way of delivery and packaging type are chosen at Seller’s discretion.

5.3 Unless unreasonable for Purchaser partial delivery is permitted for relevant reasons. Seller is entitled to invoice partial delivery separately. In case of reasonable partial delivery Purchaser is not entitled to lay a lien on his payment for reasons of outstanding parts of delivery.

5.4 In case Purchaser has to accept delivery due to statutory provisions or explicit contractual agreement, delivery at the latest shall be considered as accepted if and to the extent of which - after delivery Purchaser sells the delivery items to or lets them being used by third parties, or - the delivery items are used beyond simple testing by Purchaser or third parties, or - Purchaser approves processing of the delivery items as well as their mixing with other items.

5.5 In case Purchaser may be in default of acceptance or culpably infringes upon other contractual duties of contribution, Seller is entitled to demand compensation of damage arising therewith, including possible additional expenditure. Seller reserves the right for further claims.

5.6 Purchaser bears the risk of accidental destruction or deterioration of the delivery items from the time of default of acceptance or of default of payment, in case the premises of paragraph 5.5 apply.

5.7 Seller assumes liability according to statutory provisions if the delay in delivery is due to intentional or grossly negligent breach of contract. As far as the delay is not due to intentional breach of contract, Seller’s liability for indemnity covers foreseeable typical damages only.

5.8 Seller is also liable according to statutory provisions as far as the delay in delivery caused by Seller is due to culpable infringement of essential contractual duties; in this case, liability for indemnity covers foreseeable typical damage only.

6. Delivery Time

6.1 The beginning of delivery time as presented by Seller requires clarifi cation of all technical and commercial details.

6.2 Delivery time is quoted “ex works“ (EXW) according to the respectively relevant version of Incoterms. Delivery shall be considered as performed in time, if the merchandise has left Seller‘s site or readiness for dispatch has been announced before expiration of delivery time.

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6.3 If the Parties agree that Seller‘s 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 Sellers business account.

6.4 Delivery time will be extended accordingly, if possible contractual duties of contribution are not attended to by Purchaser. The same shall apply in case of Seller being not or wrongly supplied by Seller‘s subcontractors or in case of delay in delivery due to force majeure, industrial action or other occasions beyond Seller‘s control. If any such delay becomes apparent, Seller will inform Purchaser immediately.

6.5 If Purchaser defaults in payment in the context of other contracts between Purchaser and Seller, Seller is entitled to detain delivery under this contract for the duration of default, prior notice to Purchaser provided. This shall not apply in case of minor outstanding payment.

6.6 In case of application to open insolvency proceedings as well as of affi davit of means according to § 807 ZPO (German Code of Civil Procedure) Seller is entitled to detain delivery until full payment has been made or until Purchaser furnishes appropriate security. Furthermore, Seller is entitled to claim full payment and – after futile expiration of a reasonable extension of time granted by Seller – to withdraw from the contract unless Purchaser furnishes adequate security on Seller‘s demand.

7. Liability for Faulty Goods

7.1 Purchaser‘s assertion of rights concerning faulty goods provides examination of the delivered items immediately on delivery according § 377 HGB (German Commercial Code). If any defect becomes apparent during such inspection, Purchaser has to give written notice thereof to Seller immediately, but not later than fi ve (5) working days after discovery of said defect. Omission of notifi cation shall be deemed to be acceptance of the delivery items unless a defect appears later which could not be identifi able during above inspection. Nevertheless, the delivery items are deemed accepted as well, if Purchaser omits immediate (not later than fi ve (5) working days‘) notifi cation of said (hidden) defects in writing. Complaint‘s timely dispatch shall preserve Purchaser‘s rights. Furthermore, legal requirements shall apply.

7.2 Seller shall be liable for considerable defects only. In case of justifi ed complaints Seller is entitled to subsequent performance which may be carried out as elimination of defect or delivery of items free of defects, as Seller‘s choice may be.

7.3 Costs of subsequent performance will be borne by Seller. Additional costs caused by transfer of the faulty goods to a place other than Recipient‘s site after delivery will be borne by Purchaser unless transfer corresponds to the delivery item‘s conventional use.

7.4 Subsequent performance – irrespective of its extent – shall not be considered as an acknowledgement of any asserted defect. Solely our legal representatives and authorized offi cers are authorised to issue an acknowledgement.

7.5 In case subsequent delivery fails, Purchaser is entitled to withdraw from the contract or demand price reduction according to his choice.

7.6 Should complaints turn out to be unjustifi ed and should Seller not have given reasons therefore, Purchaser has to reimburse any and all of Seller‘s costs in connection with the putative subsequent performance which Seller could reasonably deem appropriate.

7.7 Seller shall not be liable for consequences resulting from improper remedy of defects performed by Purchaser or any third party. The same shall apply in case of modifi cation of the delivery items without Seller‘s prior agreement.

7.8 Statutory provisions shall apply in case of Purchaser‘s claims due to Seller‘s intent or gross negligence. As far as claims do not concern intentional breach of contract, Seller shall be liable for foreseeable, typically arising damages only.

7.9 Furthermore, statutory provisions shall apply in case of Seller‘s culpable breach of cardinal contractual obligations; in this case Seller‘s liability shall be limited to foreseeable, typically arising damages only.

7.10 As far as Purchaser is entitled to claim damages instead of Seller‘s performance, Seller‘s liability in the context of paragraph 7.5 shall as well be limited to foreseeable, typically arising damages only.

7.11 Seller‘s liability for culpable personal injury shall remain unaffected as well as liability according to ProdHaftG (German Product Liability Act). 7.12 Seller assumes no further liability than stated above, particularly not for claims concerning indirect damage or loss of profi t. 7.13 In particular, Seller is not liable for defects arising from improper use or maintenance, faulty installation or implementation, fair wear and tear, careless or faulty treatment or use of unapt equipment. Additionally, Seller assumes no liability for damages arising from corrosion unless Purchaser has informed Seller of the intended use of the delivery item in connection with specifi c chemicals when ordering. 7.14 Seller does not warrant freedom from third parties‘ rights in the delivery items.

7.15 Period of warranty shall expire twelve (12) months after transfer of risk.

7.16 Limitation period in case of regress against Seller‘s suppliers according to §§ 478, 479 BGB (German Civil Code) shall remain unaffected.

8. Liability

8.1 Unless stated in paragraphs 5 and 7 of these Sales Conditions, Seller assumes no liability, no matter what legal ground claims may be based on.

8.2 Limitation according to paragraph 8.1 shall apply as well, if Purchaser does not claim damages instead of Seller‘s performance but refund of vain expenditure.

8.3 Claims other than those concerning defects of the delivery items shall be subject to a preclusion period of eighteen (18) months, starting from Purchaser‘s awareness of specifi c damage and tortfeasor. 8.4 Limitation or exclusion of liability shall extend to the individual liability of Seller‘s employees, legal agents and vicarious agents. 9. Retention of Title

9.1 Seller reserves the right of property in the delivery items until Purchaser completely satisfi es Seller‘s claims already perfected at conclusion of the contract at hand. In case of current account, retention of title serves as security for Seller‘s entire balance claim.

9.2 Purchaser shall store the reserved property free of charge for Seller. Pur- chaser is obliged to treat Seller‘s property with care. Necessary maintenance or inspections are to be performed by Purchaser at Purchaser‘s own expenses. Particularly Purchaser is obliged to insure Seller‘s property suffi ciently according to its replacement value and at Purchaser‘s own expenses against damage caused by fi re, water, theft and vandalism. 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 Seller; Seller hereby accepts assignment. Notwithstanding the assignment, Purchaser is authorised to assert and collect claims in his own name, by legal proceeding if necessary. Seller‘s entitlement to collection of debts remains unaffected by Purchaser‘s authorisation.

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9.3 In case of garnishment or other intervention of third parties, Purchaser is obliged to notify Seller in writing at once in order to enable Seller to institute an action (third-party claim proceedings) in accordance with § 771 ZPO (German Code of Civil Procedure); Purchaser is obliged to inform said third parties concerned of Seller’s rights. Purchaser shall be liable for Seller’s 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.

9.4 Purchaser is entitled to resale delivery items under reserved property in regular course of business; Purchaser herewith assigns to Seller all claims against Purchaser‘s customers or other third parties arising from said resale at the amount of the invoice (incl. taxes) irrespective of whether the delivery items under reserved property were resold without or after product processing. Seller hereby accepts assignment.

9.5 With the exception of what is stated above, Purchaser is not entitled to assignment of claims arising from resale of merchandise under reserved property.

9.6 Even after cession Purchaser remains authorised to collect outstanding claims. This shall not infl uence Seller’s right to collect the debt. However, Seller will not collect the debt as long as: - Purchaser fulfi ls his obligation of payment from the sales revenue, - Purchaser is not in arrears with payment, - no application for opening composition or insolvency proceedings is fi led, - payment has not been stopped. Shall one of these cases apply, Purchaser may be required to inform Seller about the assigned debts and the respective debtor, to give all detail necessary for collection, to hand over all necessary documents and to inform the debtor (third party) about the assignment of claims.

9.7 If the delivery items under reserved property are processed or modifi ed by Purchaser, such processing and modifi cation shall always be deemed to be performed on Seller’s behalf. Shall the delivery items under reserved property be processed or modifi ed together with other objects not belonging to Seller, Seller acquires co-ownership in the resulting merchandise at an interest depending on the ratio of delivery items‘ value (amount of the invoice, taxes incl.) to the other objects‘ value which do not belong to Seller. Relevant value will be that at the time of processing or modifi cation. Furthermore, above provisions concerning delivery items under reserved property apply accordingly.

9.8 If the delivery items under reserved property are mingled, mixed or combined inseparably with other objects not belonging to Seller, Seller acquires co-ownership in the resulting merchandise at an interest depending on the ratio of delivery items‘ value (amount of the invoice, taxes incl.) to the other objects‘ value which do not belong to Seller. Relevant value will be that at the time of mingling, mixing or combination. Should the resulting merchandise consist of Purchaser‘s objects forming the main part, Purchaser herewith undertakes to assign proportionate co-ownership to Seller according to Seller‘s contribution. The parties hereby agree with passage of title. Furthermore, above provisions concerning delivery items under reserved property apply accordingly.

9.9 Seller hereby covenants to gradually release at Purchaser‘s demand the securities obtained by retention of title in so far as the property’s realisable value exceeds the debts to be secured not only temporarily by more than 10 %. The selection of securities to be released is incumbent upon Seller. 10. Copyright and Secrecy

10.1 Seller reserves all copyright and rights of ownership concerning all samples, illustrations, drawings, calculations or other documents and information given to Purchaser.

10.2 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 Seller’s explicit written consent.

10.3 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. 10.4 Purchaser is not allowed: - to disassemble the delivery items, samples etc., 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.

10.5 In case of violation of the terms of this paragraph 10 Seller is entitled to claim damages according to the statutory provisions.

11. Intellectual Property Rights

11.1 Purchaser warrants that production of items according to Purchaser‘s instructions does not infringe third parties‘ rights.

11.2 Should infringement of said rights be substantiated to Seller by a third party, Seller is entitled to stop any further activity being in opposition to said rights. If so, Purchaser will indemnify Seller from third parties‘ claims on fi rst demand.

11.3 Purchaser‘s obligation of release from liability comprises any expenditure Seller necessarily incurs in the context of third parties‘ claims.

11.4 Seller‘s claims for damages remain unaffected.

11.5 Statute of limitation concerning said claims expires ten (10) years as of conclusion of the respective contract.

12. Applicable Law

12.1 The Laws of the Federal Republic of Germany with the exception of its Confl ict of Laws – if referring to another legal system – shall apply exclusively to these Sales Conditions and to any legally relevant relationship between Seller and Purchaser. The UN Convention on Contracts for the International Sale of Goods (CISG) dated 11.04.1980 is excluded as well.

12.2 Incoterms‘ respectively relevant version shall apply additionally to these Sales Conditions.

13. Place of Performance – Place of Jurisdiction

13.1 Unless otherwise stated in the order confi rmation, place of performance shall be Seller‘s site.

13.2 Provided that Purchaser is a salesman according to German Commercial Code, exclusive jurisdiction shall be at Seller‘s place of business unless another place of jurisdiction is mandatory by law. However, Seller is entitled to invoke the aid of any other competent court.

Effective as of: March 2006

GENERAL TERMS AND CONDITIONS OF SALE

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REFERENCES

Hessel, V., Löwe, H., Müller, A., Kolb, G.; Chemical Micro Process Engineering – Processing and Plants, Wiley-VCH, Weinheim (2005).

Hessel, V., Hardt, S., Löwe, H.; Chemical Micro Process Engineering – Fundamentals, Modelling and Reactions, Wiley-VCH, Weinheim (2004).

Ehrfeld, W., Hessel, V., Haverkamp, V.; “Micro-reactors”, in: Ullmann’s Encyclopedia of Industrial Chemistry, Wiley-VCH, Weinheim (1999).

V. Hessel, C. Serra, H. Löwe, G.Hadziioannou; “Poly-merisationen in mikro-strukturierten Reaktoren: EinÜberblick“, Chem. Ing. Tech. 77, 11 (2005) 39-59.

Hessel, V., Angeli, P., Gavriilidis, A., Löwe, H.; “Gas/liquid and gas/liquid/solid microstructured reactors – contacting principles and applications”, Ind. Eng. Chem. Res. 44, 25 (2005) 9750-9769.

Hessel, V., Löb, P., Löwe, H.; “Development of micro-structured reactors to enable organic synthesis rather than subduing chemistry”, Curr. Org. Chem. 9, 8 (2005) 765-787.

Jähnisch, K., Hessel, V., Löwe, H., Baerns, M.; “Chemistry in Microstructured Reactors”, Angew. Chem. Int. Ed. 43, 4 (2004) 406-446.

Kolb, G., Hessel, V.; “Micro-structured reactors for gas phase reactions: a review”, Chem. Eng. J. 98, 1-2 (2004) 1-38.

Pennemann, H., Watts, P., Haswell, S., Hessel, V., Löwe, H.; “Benchmarking of microreactor applications”, Org. Proc. Res. Dev. 8, 3 (2004) 422-439.

Pennemann, P., Hessel, V., Löwe, H.; “Chemical micro process technology – from laboratory scale to production”, Chem. Eng. Sci. 59, 22-23 (2005) 4789- 4794.

Hessel, V., Löwe, H., Schönfeld, F.; “Micro mixers – a review on passive and active mixing priciples”, Chem. Eng. Sci. 60 (2005) 2479-2501.

Löb, P., Löwe, H., Hessel, V.; “Fluorinations, chlor-inations and brominations of organic compoundsin micro structured reactors”, J. Fluorine Chem. 125, 11 (2004) 1677-1694.

Hessel, V., Löb, P., Löwe, H.; “Direct fl uorination of aromatics with elemental fl uorine in microstruc-tured reactors”, Chimica oggi – Chemistry Today 5 (2004) 10-15.

Hessel, V., Hofmann, C., Löb, P., Löhndorf, J., Löwe, H., Ziogas, A.; “Organic Process Research & Development”, 9, 4 (2005) 479-489.

Pennemann, H., Hessel, V., Löwe, H.; “Chemical Engineering Science”, 59, 22-23 (2004) 4789-4794.

Löb, P., Hessel, V., Klefenz, H., Löwe, H., Mazanek, K.; “Letters of Organic Chemistry”, 2, 8 (2005) 767-779.

Pennemann, H., Forster, S., Kinkel, J., Hessel, V., Löwe, H., Wu, L., “Org. Proc. Res. Dev.“, 9, 2 (2005) 188-192.

Jähnisch, K., Dingerdissen, U.; “Chemical Engineer-ing and Technology”, 28, 4 (2005) 426-427.

Müller, A., Cominos, V., Horn, B., Ziogas, A., Jähnisch, 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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Institut für Mikrotechnik Mainz GmbHCarl-Zeiss Str. 18-2055129 Mainz, Germanywww.imm-mainz.de

Concept, creation and realization

tausendwattagentur für kommunikation & marketingbrahmsweg 1 | 57076 siegen, germanywww.tausendwatt.de

For further questions please do not hesitate to contact us:

Institut für Mikrotechnik Mainz GmbHCarl-Zeiss-Straße 18-2055129 Mainz

Phone: +49 61 31 / 990 - 0Fax: +49 61 31 / 990 - 205

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