Towards integration of continuous reactors, separation technology and process analysis Martijn de Graaff, Business developer TNO Knowledge for Business CPAC Satellite workshop 2010
Introduction to TNO The Netherlands Organization for Applied Scientific Research. - ± 4500 employees. - Broad knowledge and technology base. - 2/3 market funding, 1/3 government funding. Our mission: - To apply scientific knowledge with the aim of strengthening the innovative power of industry and government. Our main Business models: - Consultancy. - Contract Research & Development. - Open innovation. - Licensing of patents. 2
Process technology at TNO TNO is active in different markets for process technology Energy sector: Water sector: Oil & Gas sector: Chemical sector: CO2 Capture & Storage Decentral water treatment Oil & Gas treatment Water treatment Purification & separation Bio Process Technology Process Intensification Growth area s 3
Current forces in the chemical industry Competitive forces ( ) More cost-efficient processing - raw materials - energy consumption - waste treatment More consistent quality Shorter time-to-market Regulatory forces Environmental Safety Quality control 4 European Roadmap for Process Intensification
Process Intensification vision 2010 2025 Efficiency Efficiency F Process intensification will bring a breakthrough in chemical processing, leading to a more competitive and sustainable chemicals industry. 5 European roadmap for PI: Cost reduction of 20-50%
Focus on Flow Chemistry Use of new continuous process technologies which significantly increase the economic and ecological efficiency. Mainly for specialties, fine chemicals & pharmaceuticals. 6 Analytical & laboratory Equipment: ~ 1-100 cm Structures: ~ 10-1000 µm Throughput: g/d kg/d Production Equipment: ~ 0.1-10 m Structures: ~ 1-100 mm Throughput: T/y kt/y
Why flow chemistry? Main advantages of flow chemistry: Yield & selectivity increase. Increased safety. More tight process control. More constant product quality. Shorter time to market. 7 Batch process source: Pollak, fine chemicals (2007)
Necessary aspects for flow chemistry Waste Raw materials Reaction Separation Product Energy Labour Analysis & Control Benefit Cost 8 All must be incorporated to get the true benefit from continuous production!
Commercially available flow chemistry solutions Commercially proven & available Many To be adapted from other area s Some To be adapted for flow To be developed Some 9
Hurdles to be overcome Technical hurdles Downstream processing missing. Integrated process control missing. Multi-phase reactions difficult. Limited flexibility: How to make multi-purpose? Throughput: How to scale up cost-efficiently? In finechem & pharma: many different reactions many new products Non-technical hurdles No good evaluation & categorization. Low amount of publicly available demonstrations. Missing general awareness at plant (manager). 10
TNO flow chemistry roadmap 2 1 3 11
TNO Process intensification strategy 1. Exploit existing individual TNO technologies 2. Invest & cooperate in integration & demonstration 3. Involve all stakeholders Non-TNO technologies TNO technologies 12 Ideas Proof of Principle Feasibility Proof of Concept Pilots off/on site Demonstration Implementation
Exploit existing TNO technologies Separation technologies Reactor technologies Analytical technologies Crystallization based Sensor technologies TNO HWC purification TNO Helix reactor Flowmeters Particle monitors TNO HWC solvent switch Membrane based Microreactor technology FBG sensors Interpret, model & control Pertraction MGA Chemometrics & data processing 13 Pervaporation Model predictive control
Integration & demonstration Integration of technologies, both TNO and non-tno. a) Integration of unit operations. b) Combination of technologies into one continuous plant. Focus on flexible multi-purpose solutions. Comparison of technologies for different applications. Piloting & Demonstration in industrial environments. 14
Example 1: Membrane slurry reactor Membrane Slurry Reactor Reactant in Ceramic membrane Hollow fiber close-up surface Coolant Product Product in Product Product out Catalyst Membranes Examples reactions hydrogenations oxidations hydroformylations 15
Example 1: Membrane slurry reactor Principle Continuous reactor with membranes. Product can pass membrane, catalyst particles are retained. Advantages Continuous operation Expensive catalyst is not discarded Flowrate determines residence time Mild mechanical treatment of catalyst Suited for chemical and bio-catalysis 16 Lab scale MSR
Example 1: Membrane slurry reactor Enzyme catalyzed reaction Penicillin acylase CLEA 17 MSR with 5% CLEAs APA- Precipitation Conversion/mmol APA formed 100 90 80 70 60 50 40 30 20 10 mmol APA formed Conversion MSR 0 0 20 40 60 80 100 120 Time (min) Batch Enzymatic conversion of Penicillin G into Phenyl acetic acid and 6-aminopenicillanic acid (6-APA) Rate APA (mmol/min) 1,2 1 0,8 0,6 0,4 0,2 0 MSR CLEA Overview Continuous experiments Rate APA cumulative 5% CLEA Rate APA cumulative 7.5% CLEA Rate APA cumulative 10% CLEA 0 20 40 60 80 100 120 140 160 time (min) Continuous
Example 2: Integration of reaction & separation Combination of 2 proven technologies for multiphase reactions. Solv C (solv) A (aq) B (aq) Mixing Reaction Extraction D (aq) TNO Helix reactor: - Improved radial mixing - Minimal axial mixing - High heat transfer - Multi-phase continuous reactor - Scale-up by parallellization Pertraction: - L-L Membrane extraction - Organic/aqueous separation - Hydrophobic/hydrophilic membranes - Multiple scale-up strategies Project currently running. 18
Example 3: CoRIAC project Demonstration of Continuous Reactors with In-line Analytics for fine Chemical production. First phase call of the Action Plan Process Intensification (APPI). Partners: - 3 chemical companies - 4 reactor suppliers - 2 process analysis suppliers - 1 system integrator - 1 university Start in april/may 2010 19
Example 3: CoRIAC project Goal: Demonstration of existing equipment for highly exothermal and solid-liquid processes in relevant industrial conditions Benchmarking of continuous reactors for processes determined by end-users. Adapting existing analytical tools for continuous analysis. Preparation for model-based process control. Demonstration in multi-purpose pilot installation on end-user s sites. 20
Example 3: CoRIAC project WP 1: Reactor benchmarking WP 3: demonstration Benchmarking of several reactors for multi-phase and exothermal reactions WP 2: PAT Benchmarking/comparison of several analysis tools Onsite industrial Pilot for multi-purpose reactor @ 10-50 kg/hr Adapting existing analysis tools for continuous analysis Multiplexing / probe costprice 21 0-18 months 18-40 months
Scale-up, piloting & demonstration Scale-up strategy from the beginning. - How to go from lab to plant? Multiply or expand? - Is it technically and economically feasible?. Pilots prove strategy. - Reliability & robustness under practical industrial conditions. - Pilots give key design parameters for full scale plant. Demonstrations are convincing. - More demonstrations of a technology are better. - Secrecy obligations sometimes prevent this. TNO Pilots & Demo s 1998-2010 22
Involvement of all stakeholders Successful implementation of PI involves: - Chemical companies - Reactor suppliers - Separation suppliers - Analytical suppliers - System integrators - Knowledge institutes - Piloting & demonstration facilities TNO is actively looking for cooperation and partnering in: - Direct business opportunities - Further development and demonstration. - Cooperative consortium projects. 23
Conclusions TNO is a leading contract R&D organization working on integrated multi-purpose flow chemistry technologies. Process intensification requires the integration & combination of reactors, separation technology and analytical technology. Scale-up, piloting & demonstration are essential for adaptation. Close cooperation between all stakeholders and disciplines is required. 24
Innovation is mostly created at the interface where different worlds touch. Strategic Plan TNO 2007-2010 25
Thank you for your attention! For more information please contact: Dr. Jean-Marie Bassett Business Development Manager Chemicals & Separation Technology jean-marie.bassett@tno.nl +31 (0)15 269 2833 +31 (0)6 104 804 73 Ir. Martijn P. de Graaff Business Development Manager Chemical & Life Science Equipment martijn.degraaff@tno.nl +31 (0)15 269 2243 +31 (0)6 222 608 71 26