Advanced Process Technology Shared Innovation Program Provide! Overview of technical program lines

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1 Advanced Process Technology Shared Innovation Program Provide! Overview of technical program lines

2 2 Shared Innovation program lines Cases from industry Small-scale dedicated production Flexible & scalable multipurpose continuous Versatile programmable Formulation systems a) Small scale continuous flow processing b) Highly selective separation concepts c) Electrochemistry & external field enhanced d) Handling & processing of complex fluids e) Modularity, flexibility & asset-light Technologies/tools from partners (equipment, academica)

3 A) Reactor Technology Demonstration of reactors for challenging processes L.F.G. Geers, J. Urbanus

4 4 Properties & options of continuous reactor technology

5 5 Reactor Technology: Impact & Focus Impact: Improved product quality in terms of yield, selectivity and product concentration (reduces use of solvents) Scalability of process equipment to reduce development time (easier translation from lab to pilot), shorten time to market, and to facilitate variable production sizes (for volatile markets) Focus: Flexibility of products for volatile demand/supply & variety of consumer interests Reduced costs of equipment modules to compensate loss of economy of scale when numbering up

6 6 Visionary goal & TNO focus Functionality manufacturing enabling main topics: - Multiphase (solid-liquid) processing - Strongly exothermic processes source: Miscellaneous: nano-particles, highly-viscous media

7 7 State-of-the-art outside TNO F3 factory (FP7 project) Goal: Development of plug&play modular equipment & holistic design methodology FLOWID Lab scale development platform for fast and easy modular process development Flow mini plant (Micro Innova) Modular design combined with process intensification technologies provides efficiency and flexibility. Chemtrix / ESK Development and consultancy on scalable modular continuous flow equipment

8 8 State-of-the-art at TNO DiMeCo: dissolving metals in a continuous flow process CoRIAC: demonstration of flow chemistry on lab, bench and pilot scale Industrial scale installation (Zeton & TNO for Solvay) Flow4API: screening chemistry to optimize for flow chemistry and telescoping, and demonstration on production scale

9 9 Potential industrial applications of (TNO) continuous reactor technology Solid-liquid processes Heterogeneously catalysed reactions (hydrogenations, formylations) Reactions with solid reagents or products (organometalics, pharmaceuticals production) Oscillating baffled crystallizer (source:tno) Nano-materials production Highly viscous liquids Twin screw extruder (source: TNO) Dangerous chemistry Novel process windows (high pressure & temperature) Production of energetic materials TNO Helix reactor

10 10 Next steps - What would we do with 500 keur? Demonstrate continuous reactor technology for new challenging cases: construct a flexible skid in which modular systems can be assembled consisting of process modules with reactors, feed sections, product sections including process monitoring and control system for in-line product quality assessment Develop/improve/apply innovative reactor modules: for heterogeneous processes (especially solid-liquid, but also gas-liquid) with alternative energy sources, e.g. ultrasound, microwave, photochemistry, etc. to demonstrate and evaluate their applicability for highly viscous media, e.g. using extrusion with integrated separation of products or by-products with multiple feed points along the reactor, e.g. for telescoping reactions

11 B) Modular Separation Technology Translating principles to proven modules C.P.M. Roelands, J. Urbanus Functionality manufacturing enabling

12 12 PROVIDE! Modular Separation Technology General concept: separation as integral part of the modular process system

13 13 Modular Separation Technology: Focus & Results Higher operating margins desired for EU for (fine)chemical industry: a. Lower operating cost - expressed in: - lower PMI [kg feedstock+auxiliairies /kg product ] - lower E-factor [kg waste /kg product ] - lower E-consumption [kwh/kg product ] improved mass & energy efficiency => also less equipment needed b. Lower capital cost - lean infrastructure for distributed / localized production, utilizing renewable energy & feedstock: - modular flexible equipment boundary condition for technology Key role for Separation Technology Innovations c. Higher income on products: - improved product quality (purity, particle size) - higher added value products opportunity to integrate separation with product forming

14 14 Potentially relevant topics for industrial cases Objectives: To build industrial case based program for development of modular separation technologies (toolbox will be filled gradually) To connect industrial cases with technologies from (SME) equipment manufactures To demonstrate advantages for industrial cases at bench scale feed A recycle recycle reactor 1 separation 1 reactor 2 separation 2 formulation product feed B purge feed C purge feed D Integrated reaction / separation : - to improve overall yield /productivity 2. Highly selective separations: -recycle of unreacted feedstock - recovery of auxiliaries (e.g. catalyst) - removal of similar byproducts -separation of enantiomers 3. Solvent switch / swap between two steps: - for solutes and for particles 4. External field driven separations - to enhance separation efficiency - to use renewable energy 5. Separation from highly viscous systems - lifting mass transfer limitations 6. Integrated separation / particle formation -in one step right size, structure, shape

15 15 MATCH methodology to select appropriate separation technology for a specific industrial case Principle for Separation Integrated Reactor / Separation In-line separations Solvent switch / swap External field assisted separation High viscosity separations Integrated Separation / Formulation Vapour pressure Falling film evaporator Flashevaporator / Microsieve Spray evaporator Rotating Packed Bed Spray Crystallization Solvent affinity (dissolved) Pulsed Packed Column Membrane Contactor Spinning Disc Contactor Solvent affinity (crystal) Oscillating Baffled Crystallizer Hydraulic Wash Column Crystel/ Ultrasound / Electrospray Pulsed Helix mild shear crystallizer Surface affinity Pervaporation / Ligands OrganophilicPV / SMB Electro Dialysis Template Induced Crystallization Molecular size Size Exclusion Chromatography Organic Solvent Nanoniltration

16 16 6 examples of potential developments (2) Integration Reaction + Separation: Pervaporation of reaction water In-Line Separations: Membrane extraction from suspension Solvent switch: Flash evaporator Field enhanced separation: in-situ electrochemical crystallization High viscosity separation: HiGee/HighShear equipment Integration Separation + Particle formation: Pulsed Helix for cooling crystallization Illustration of options for research possible within Provide! Actual research topics depend on industrial cases of participants

17 17 Partners on separation technology 1. Universities (discovery and early stage technology development) e,g, TU Dortmund, TU/e, TU Delft, UT, WURC 2. SME Equipment manufacturers (develop and launch technology) e.g. Pervatech, Solsep, TOP, Evodos 3. Equipment manufacturers (sell and manufacture proven technology) e.g. Sulzer, GEA 4. Engineering Consultants / Contractors (select proven technology for implementation) e.g. PDC, Avantium, Novasep, Traxxys 5. R&D departments large companies (select technology for piloting and implementation) e.g. DSM, AkzoNobel, GSK 6. Plant technologists (implement technology)

18 MATCH methodology to select appropriate separation technology for a specific industrial case 18 Half a Million Advanced Euro Process Technology Shared to spend Principle for Separation Vapour pressure Solvent affinity (dissolved) Solvent affinity (crystal) Surface affinity Molecular size Integrated Reactor / Separation Falling film evaporator Pulsed Packed Column In-line separations Continuous Flashevaporator / Microsieve separations Membrane Contactor for integrated Oscillating Baffled modular Crystallizer Pervaporation OrganophilicPV / Ligands systems / SMB Size Exclusion Chromatography Solvent switch / swap Spray evaporator Hydraulic Wash Column Organic Solvent Nanoniltration External field assisted separation Crystel/ Ultrasound / Electrospray Electro Dialysis High viscosity separations Rotating Enhanced Packed Bed continuous Spinning Disc Contactor separations (fields, higee, hybrids) Integrated Separation / Formulation Spray Crystallization Pulsed Helix mild shear crystallizer Template Induced Crystallization

19 C) Electrochemical production Towards electrification of the chemical industry

20 20 The applications of electrochemistry

21 21 Incentives for employing organic electrosynthesis Organic electrosynthesis has the following advantages amongst others 1,2 : Elegant control of reaction rate High selectivity High efficiency Ease of automation Green methodology The use of pollutant free electrons as reactant Reactions conducted at ambient pressure and temperature Low emission of toxics Electrolysis is modular Possibility of flexible employment 1 Schäfer H.J., C.R. Chimi 14 (2011), Schmidt V.M. Elektrochemische Verfahrenstechnik (2003)

22 22 Example 3 of conventional vs. electrochemical production of p-methoxy benzaldehyde Activation by chlorine: Electrochemical activation: Advantages: Avoiding use of toxic chlorine, lower operating temperatures, no byproduct (HCl) formation 3 Steckhan et al., Chemosphere 43 (2001),

23 23 Electricity market developments Present situation of centralised electricity production: coal, oil, gas thermal mechanical electrical Trend towards renewable electricity production: wind / water mechanical electrical sun electrical Fluctuations of electricity prices ascribed to renewable energy 4. Renewables only accounts for 16.4% of Germany s electricity production in Fanone et al., Energy Economics 35 (2013), Bundesministerium, für Umwelt, Naturschutz, Bau und Reaktorsicherheit

24 24 Exploitation of low and negative electricity prices Exploitation by electrochemistry Electrochemical energy storage systems are suggested for balancing supply and demand but are relatively costly Electrochemical synthesis can profit from low electricity prices Typical electricity consumption: Large scale (chlorine production): 43% of CAPEX Fine and specialty chemicals: 13% of CAPEX

25 25 Research path for electrochemical applications (1) Determination of the technical feasibility of the proposed electrochemical system by electro-analytical methods. Development of an electrochemical reactor to handle the selected electrode materials and fluids amongst others System Reactor design Lab- / bench scale TEMPO = 2,2,6,6-tetramethylpiperidine-1-oxyl Does electrochemical production meet the economical and technical requirements such as product concentration, current density, current efficiency,.?

26 26 Research path for electrochemical applications (2) Integration of the electrochemical reactor in an envisioned process. Focus on product separation and electrolyte recycling. Process Validation of the electrochemical process together with parametric research for model validation Piloting Economics Determination of optimal economic conditions of the electrochemical process

27 27 Envisioned objectives Work out cases for electrochemical technology including downstream processing such as: Ethylene oxide or ethylene glycol production Paired electrosynthesis of propylene oxide CO 2 utilisation by electrochemical reduction Production of fine chemicals / specialties such as. Development of generic electrolyser technology which can handle different type of electrode materials liquids and gasses Integrate electrolyte models to enable down-stream process estimations Incorporation and/or development of electrolyte models Description of unit-operations standard not present in flowsheet progs

28 D) Handling & production of complex fluids Processes and processing towards industrial (nano)-specialities, composites and heterogeneous catalysts

29 29 Context processing of complex fluids The nano-promise: control of dimensions in the nanometer regime leads to outstanding product properties. Processing routes 1. Top-down (physical means of size-structuring, such as milling, spraying, etc). 2. Bottom-up (clever chemical routes, self-organisation, NP growth) TNO takes its role when it comes to adapting scalable instrumental techniques, equipment and processes from other industries TNO wants to develop academic recipes into scalable processes by using scalable setups, a nanoparticle pilot production plant and making use of new-to-develop in- and on-line QC instrumentation

30 30 Top-down processing: printing techniques Conventional process Drying (swirl flow results nozzle) Printing powder process (Rayleigh break-up nozzle) Improving the product quality of dried dispersions by adapting industrial style inkjet printing heads for spray drying technology

31 31 Top-down processing: printing techniques Conventional process Drying (swirl flow results nozzle) Printing powder process (Rayleigh break-up nozzle) To be used in solvent swapping?

32 32 Top-down processing: printing techniques TNO Encapsulation Printer New processing technology for microencapsulation: Generate core droplet by inkjet technology Encapsulation by a liquid film / curtain of shell material Formulating encapsulated micron-sized beads by custom-made printing setup

33 33 Bottom-up approach Using novel colloid synthesis routes from academia and adapt them for scalable setups: Towards continuous nanoparticle synthesis (Quality/scalability improvement) Towards in-line and on-line QC (using partly in-house developed ultrasound and light scattering tools) Towards integrated down-stream processing Focus on: batch->continuous, controlled shear fields, in-line quality control and automized downstream processing continuous reactors, in-line analytics, integrated downstream processing

34 34 State-of-the-art Off-line quality control using electron DLS, electron microscopy, reology, mechanical stirrers At TNO: we are building up in-line sizing and aggregation state measurement tools, continuous reactors, scalable shear fields (static mixers) Our focus on scalability, repeatability and precision

35 Nanomaterials development for Chemical and High tech Industries Expertise on sol-gel, mineral, metal, polymer, hybrids Nucleation and growth Hybridization Surface modifications 35 Homemade nano-titania-filled translucent resist for NIL hollow silica beads Quantum dots Photonic crystals Lanthanide Nanodot tracers Ag- wires

36 F) Modularity, flexibility and asset-light Facilitate profitable modular processes I. Hernandez-Mireles, D. Verdoes, J. Urbanus Functionality manufacturing enabling

37 37 Supporting tools & technologies 3 main topics: - Module manufacturing - Modular infrastructure - Systems, models & tools Mainframe Modular reactors Modular separations Modular components

38 38 Supporting Technologies & Tools: Enablers & Results Continuous & multipurpose processes Modular separation technology Manufacturing technology Enablers Adv. Modular reactors Adv. sensors and controls Adv. Systems modelling and logistics These enablers will result in: - Localized production, utilizing renewable energy & -feedstocks - Reduction of equipment cost per unit produced - Decreased energy consumption & waste production - Improved product quality - Minimization of operating labour - Less investment risks for developing markets through scalable technology - Flexibility for volatile demand/supply & variety of consumer products

39 39 Some flavours of module manufacturing ADMATEC Module manufacturing: Automated manufacturing Innovative manufacturing Throw-away principles 3D printing printing of conformal µ fluidic channels Source: TNO Single-use reactor bags Sartorius Stedim Biotech S.A.

40 40 Automated manufacturing: 3D printing Advantages for 3D printing reactors Tailored shape and size Integrated functions, i.e. catalyst contained in material Cronin L. Nature Chemistry Volume: 4, Pages: D printing on different materials Plastics (reactors, prosthesis/implants) Concrete (houses) Ceramics Food. In the future: metals WinSun Decoration Design Engineering Cornucopia, MIT

41 41 Innovative manufacturing: membrane welding techniques Membrane modules can be used in a broader range of operating conditions High temperature High pressure New applications need to be developed to exploit these features and manufacturing techniques TNO

42 42 Some flavours of modular infrastructure Modular infrastructure: In-line PAT sensors New sensors (rheology, fouling) BAM.de - Sensor node of a selfconfiguring wireless sensor network Remote operation TNO/SPIRE1 fouling & rheology sensors Plug & play mainframe

43 43 Some flavours of systems, models & tools Systems, models & tools: Sustainability Logistics and systems Decisions support tools Electricity to chemistry Resource efficiency Bio-based economy TNO-VITO-GCC MATCH Chemistry Technology EU - DIMENSIONS

44 44 Next steps What would we do with 500 keur? Focus on innovative manufacturing methodologies 3D-printing Explore possible specifications/properties of printed reactor modules Reproducibility of performance Recycling of reactor material Investigation of business models & business cases Q Stick-built plant capacity Production output 3 (years 13- ) 3 rd module Production output 2 (years 8-12) 2 nd module Production output 1 (years 3-7) 1 st module t

45 45 More information? Please contact: TNO Sustainable Chemical Industry Business Line Enhanced Processing Leeghwaterstraat CA Delft Ir. Martijn P. de Graaff Business Line Manager +31 (0) (0) Ir. Peter Wolfs Marketing & Sales Manager +31 (0) (0) Dr. Jean-Marie Bassett Business Development Manager +31 (0) (0)

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