2nd Flow Chemistry Demonstration Workshop

May 11, 2017

Open House Spring 2017

At this event you will discover the entire range of Fraunhofer ICT-IMM’s capabilities in the field of continuous liquid and gas phase processing centered on process development, multi-step organic synthesis, inline monitoring, process control and scale-up and, linked to that, our contribution to future chemical production concepts. You will see how Grignard reagents can be formed continuously using a large excess of magnesium being activated in situ. Have a look at the continuous formulation of functional polymer-based particles/capsules with controlled composition, the efficient preparation and loading of carrier systems followed by cross-flow filtration for direct purification and with online process monitoring by dynamic light scattering, a process for the continuous synthesis of size-tunable nanocrystals for catalytic applications and a set-up for the aryldiazonium salt synthesis with consecutive TiO2-photocatalyzed C-H arylation of heteroarenes including online 19F NMR analysis. Complete the picture by a visit to our demonstration facility in container-format showcasing activities related to the generation of synthetic gasoline and reforming processes.

Lab Stations - Find your expert, discuss your needs

You will have plenty of time to individually discuss the possibilities with our experts.

Reactive Intermediates in Flow

Lab-scale reactor
© Photo Fraunhofer ICT-IMM

Lab-scale reactor

Pilot-scale reactor
© Photo Fraunhofer ICT-IMM

Pilot-scale reactor

It will be showcased how Grignard reagents can be formed continuously in a novel process window constituted by a large excess of magnesium that is activated in-situ. On the laboratory scale, process development and optimization for a variety of Grignard reagents has been done. Additionally, the pilot reactor setup provides a continuous feed not only of the liquid but also the solid component rendering the process truly continuous in nature. This results in on-demand production of the Grignard reagent which is already optimized in terms of time and quantity. Through continuous processing quality improvement goes hand in hand with cost savings as well as an increase in production flexibility.

Thinking ahead:

  • Multi step synthesis e.g. in API production including in-situ generation and consumption of Grignard reagents.
  • Fast scale-up to industrially relevant throughputs.
  • Potential use in other solid-consuming reactions, such as Friedel-Crafts acylation.

Your expert:

Dr. Gabriele Menges-Flanagan
© Photo Fraunhofer ICT-IMM

Dr. Gabriele Menges-Flanagan, graduate chemist, joined the Fraunhofer ICT-IMM team in 2005. Her research focuses on reactive intermediates, solid processing in flow, C-C bond formation, and inline analytics. 

Immediate conversion of intermediates in a 2-step synthesis

FFMR with royal blue illumination
© Photo Fraunhofer ICT-IMM

FFMR with royal blue illumination

Flow cell installed in benchtop NMR spectrometer
© Photo Fraunhofer ICT-IMM

Flow cell installed in benchtop NMR spectrometer

Aryldiazonium salt synthesis in flow with consecutive TiO2-photocatalyzed C-H arylation of heteroarenes including online 19F NMR analysis

You can expect to experience the continuous formation of reactive intermediates (aryldiazonium salts) in a capillary loop reactor at room temperature and, then, the direct transfer of the reactive intermediates into a falling film microreactor for a heterogeneously photocatalyzed carbon-carbon coupling reaction. The final product analysis is subsequently done via online 19F NMR analysis. Direct conversion of a reactive intermediate in such a 2-step synthesis contributes to a safer handling of potentially dangerous substances in flow reactors. Performing a heterogeneous photocatalysis using visible light as well as immobilized and noble metal free catalyst for carbon-carbon coupling offers many advantages to our customers such as cost reduction and saving resources. At the same time the use of lower energy radiation gives access to a broader range of aryldiazonium salts and allows for the use of a wider variety of heteroarenes in the second step of the synthesis.

Thinking ahead:

  • Immobilization of various inorganic photocatalysts in microstructured equipment
  • Doping of inorganic photocatalysts with organic dyes for accessing the visible light region
  • Easy scale-up with larger reactors of the FFMR family
  • Online-NMR analysis of fluorine-containing compounds directly coupled to flow synthesis module

Your expert:

Dr. Thomas Rehm
© Photo Fraunhofer ICT-IMM

Dr. Thomas H. Rehm, graduate chemist, joined the Fraunhofer ICT-IMM team in 2011. His research focuses on homogeneous and heterogeneous flow photochemistry for fine chemical synthesis and online-NMR analysis for PAT applications.

Platform Technology for Nanoformulations

Caterpillar micromixer
© Photo Fraunhofer ICT-IMM

Caterpillar micromixer

Niosome dispersions
© Photo Fraunhofer ICT-IMM

Niosome dispersions with different average particle sizes at identical concentration

A continuous micromixer-based process for the efficient preparation and loading of versatile carrier systems will be presented. The process is based on the controlled self-assembly of amphiphiles, e.g. phospholipids, blockcopolymers, surfactants. It is characterized by gentle conditions (renouncing high sheer forces and sonication) and high control over the chemical and physical properties (particularly size control without post-treatment). Based on our knowledge and experience in the formation of supramolecular structures we offer the development of customized carrier systems manufactured in a reliable and reproducible process. Due to the modular concept you also get access to more complex materials. The presented setup includes modules for direct purification by cross-flow filtration as well as for online analysis by dynamic light scattering and process control.

Thinking ahead:

  • Carrier systems for nanomedical research and development.
  • Formulations for cosmetic, pharmaceutic and other additives.
  • Composite materials with combined carrier and imaging features.

Your expert:

Dr. Regina Bleul
© Photo Fraunhofer ICT-IMM

Dr. Regina Bleul, graduate biotechnologist and chemist, joined the Fraunhofer ICT-IMM team in 2014. Her research focuses on nanomedicine, e.g. multifunctional drug delivery systems and continuous nanoparticle synthesis, e.g. magnetic nanoparticles as contrast agents in medical imaging.

Scaled-up process for the continuous synthesis of size-tunable nanocrystals for catalytic applications

Microfluidic devices for rapid mixing
© Photo Fraunhofer ICT-IMM

Microfluidic devices for rapid mixing

You can expect to learn how ultra-small metallic nanoparticles can be easily synthesized via a continuous process in a microfluidic reactor. The setup allows an easy and fast parameter optimization and includes all necessary inline analytics. Due to its modularity and an easy parameter change the whole setup becomes multi-purpose. A tight process control guarantees scalability and reproducibility of results. You can achieve a nano-catalysts production with a high space-time yield.

 

 

Thinking ahead:

  • Modular setup allowing the synthesis of metallic nanoparticles like Cu, Au and Pd, in combination with carriers or co-catalysts like ZnO or Al2O3.
  • Process development / screening of different sizes, formulations and combinations.
  • Pilot-scale production for kilogram amounts.

Your experts:

Dr. Ralph Sperling
© Photo Fraunhofer ICT-IMM

Dr. Ralph Sperling, graduate physicist, joined the Fraunhofer ICT-IMM team in 2012. His research includes nanoparticle synthesis and analysis, in particular quantum dots, with a focus on continuous processes and optical spectroscopy for online analysis.

Christoph Schindler
© Photo Fraunhofer ICT-IMM

Christoph Schindler, graduate chemical engineer, joined the Fraunhofer ICT-IMM as a PhD student in 2015. His research focuses on the process development for nanoparticle synthesis, including the adaption of systems to flow chemistry, scale up and process intensification and the integration of process control systems.

Continuous Flow Production of Functional Polymeric Particles

Temperature-responsive polyacrylate-based capsules
© Photo Fraunhofer ICT-IMM

Temperature-responsive polyacrylate-based capsules

Hybrid polyacrylate/SiO2 particles
© Photo Fraunhofer ICT-IMM

Hybrid polyacrylate/SiO2 particles

You can expect to learn how functionalized particles/capsules can be formulated continuously from synthetic and natural polymers through an emulsification solvent evaporation method. A continuous and controlled feed of the components results in the formation of particles with adjustable size (between 100 nm and 10 μm) and degree of functionality. Encapsulation yield of hydrophobic and hydrophilic liquid or solid agents up to 80 wt% can be reached. The process for the production of aqueous polymer-based dispersions is applicable for versatile materials, highly reproducible and scalable. The implementation of inline/online process control and particle characterization is possible.

Thinking ahead:

  • Combination of materials with different properties in one particle to produce advanced products with unique synergetic effects.
  • High yield encapsulation of active agents for effective protection and controlled release upon physical, chemical or biological stimulus.

Your expert:

Dr. Anna Musyanovych
© Photo Fraunhofer ICT-IMM

Dr. Anna Musyanovych, graduate biotechnologist, joined the Fraunhofer ICT-IMM team in 2013. Her research focuses on the development of formulation concepts and continuous processes for the production of polymer-based particles and capsules with on-demand release function.

BIOGO – Conversion of pyrolysis oil to synthetic gasoline via synthesis gas and methanol

EcoTrainer® for synthetic fuel production
© Photo Fraunhofer ICT-IMM

EcoTrainer® for synthetic fuel production

Miniplant set-up for the conversion of pyrolysis oil to synthesis gas
© Photo Fraunhofer ICT-IMM

Miniplant set-up for the conversion of pyrolysis oil to synthesis gas

You can expect to experience the continuous conversion of synthesis gas from pyrolysis oil in a miniplant environment, which is currently set up at Fraunhofer ICT-IMM in the scope of the European project BIOGO (www.biogo.eu). The basic idea of the process envisaged is the utilization of renewable non-food related biomass to synthetic gasoline-grade fuel. Wood residue, as it is available in large quantities e.g. in Germany (annual available quantity: about 12 million tons vs. a gasoline consumption of 16 million tons) has been chosen as source material which is converted through a thermochemical process to pyrolysis oil. The pyrolysis oil is then converted to synthesis gas, which is further converted to yield methanol after a purification process. In the last methanol-to-gasoline (MtG) step, synthetic gasoline is generated over zeolitic catalysts (ZSM-5) in a process remotely similar to Fischer-Tropsch but avoiding the wax formation which complicates this well-known technique inevitably. The miniplant is already set up in a containerized environment (Evonik’s EcoTrainer®).

Thinking ahead:

  • De-centralized production of synthetic fuels from organic residues in the size range of up to 100 barrel/day: Lowering transportation costs for the source material.
  • Easy scale-up through the early implementation in a container environment during the miniplant phase.
  • Easy scale-up through utilization of microstructured reactors for a majority of the process steps.

Your expert:

Prof. Dr. Gunther A. Kolb
© Photo Fraunhofer ICT-IMM

Prof. Dr. Gunther A. Kolb, graduate chemical engineer, joined the Fraunhofer ICT-IMM team in 2001. Since 2016 he leads the Division Energy and Chemical Technology at ICT-IMM. His research focuses on heterogeneous catalysis, fuel processing and microreactors for energy related applications. He is co-ordinator of the large European project BIOGO.

Energy supply for aircraft

CAD model of the energy trolley
© Photo Diehl Aerospace

CAD model of the energy trolley

fuel processor for propylene glycol
© Photo Fraunhofer ICT-IMM

World-wide first fuel processor for propylene glycol (5 kW power equivalent) developed by Fraunhofer ICT-IMM

You can expect to experience the world-wide first electric power generation by fuel cell technology from propylene glycol, which is currently under development at Fraunhofer ICT-IMM in the scope of the German project GETpower (Galley Energy Trolley Power) together with partners Diehl Aerospace and German Aerospace Center (DLR). The basic idea of the project is auxiliary power supply for the passenger area of aircrafts. For this purpose the power generation system is housed by a regular trolley, which can be connected to the galleys of the aircraft (which are the main consumers in the passenger section) providing up to 15 kW of peak power and up to 5 kW of permanent power supply. Propylene glycol was chosen because it is an approved substance for aircraft (cooling agent and de-iceing), it is non-toxic and not flammable and a “green fuel” - regeneratively producible and biodegradable. The fuel processor of ICT-IMM converts propylen glycol into hydrogen supplying a fuel cell and, ultimately, a buffer battery.

Thinking ahead:

  • De-centralized production of energy from non-toxic, renewable sources such as propylene glycol, ethylene glycol or glycerol in the size range up to 100 kW.
  • Easy scale-up through the application of microchannel reactor technology.
  • Low production costs of the reactors through the application of cheap fabrication techniques such as embossing of microchannels, screen printing of catalysts and laser welding of reactors.

Your expert:

Jochen Schürer
© Photo Fraunhofer ICT-IMM

Jochen Schürer, graduate process engineer, joined the Fraunhofer ICT-IMM team in 2001. Since 2016 he leads the group Process Design and System Development at ICT-IMM. His research focuses on setting up complete systems for fuel processing and fuel synthesis and other energy related applications.