Key challenges for industrial use of research infrastructure Alfons Molenbroek

Transcription

1 Workshop - Forskningsinfrastruktur för industriella innovationer, 14 June 2012, Stockholm Haldor Topsøe A/S Catalyzing your business Key challenges for industrial use of research infrastructure Alfons Molenbroek am@topsoe.dk Topsøe Group s headquarters in Lyngby, Denmark Established 1940 Ownership: Haldor Topsøe Holding A/S (100%) Annual turnover (2011): ~600 MM EUR (> 4.46 billion DKK ) Number of employees ~2200 1

2 Our business areas founded in heterogeneous catalysis Fertiliser industry (ammonia, ) Heavy chemical and petrochemical industries (synthesis gas, methanol, hydrogen, ) Refining industry (hydrotreating, hydrocracking) Environmental and power sector (DeNOx, WSA, SNOX) Renewables (e.g. biofuels, biochemicals) Global Challenges World population Food shortage Resources Efficient use of resources Pollution Reduction of smog, acid rain 2

3 Goals in Catalysis Understand and predict relation between material properties and reactivity Towards a rational design of catalysts: Improve design and production of existing processes and catalysts and develop new ones Tailoring of: selectivity (100%), activity, deactivation, shape, size, mechanical strength, thermal stability, material costs, purity of raw materials Driving forces: often (environmental) regulations What type of RI does industry need? Type of industrial use of RI s: mainly strategic R&D (not basic research, not quality control) Different ways: fully involved in experiments collaboration with academic world analytical service (full analytical lab) Balance between techniques new for synchrotrons (fs methods, high brilliance nano-beams) and established techniques (high flux, robust techniques) 3

4 In situ techniques in catalysis Relate Structure to Activity under process conditions Radiation: X-rays Light Electrons Reactants - Gas control system Tomography XRD SAXS EXAFS SEM TEM IR Raman Products - Mass Spectrometer Ammonia Synthesis Catalyst N 2 (g) + 3 H 2 (g) 2 NH 3 (g) Fe/FeO-catalyst 1 kg of catalyst 25 tonnes of NH 3 Annual production: 150*10 6 tonnes No catalyst? <150 tonnes It is the know-how that counts 4

5 World Population Prediction Prediction (2 children/woman) Year Year Recent industrial refinery catalysts Haldor Topsøe has introduced new generations of hydrotreating catalysts Aided by the input from molecular-scale research Named BRIM Technology TK-558 BRIM (CoMo) and TK-559 BRIM (NiMo) for FCC P/T TK-576 BRIM (CoMo) for ULSD 5

6 New In Situ Techniques Provided Insight First in situ EXAFS Studies of CoMo/Al 2 O 3 Catalysts Mo present as MoS 2 nanoclusters Mo Relative magnitude Bulk MoS 2 Sulf. Mo/Al 2 O 3 S In situ FTIR: Monolayers (single MoS 2 slabs) Sulf. CoMo/Al 2 O 3 N.Topsøe (1980) R(Å) Clausen, Topsøe et. al (1981) New In Situ Techniques Provided Insight First in situ EXAFS Studies of CoMo/Al 2 O 3 Catalysts Mo present as MoS 2 nanoclusters Mo Relative magnitude Bulk MoS 2 Sulf. Mo/Al 2 O 3 Sulf. CoMo/Al 2 O 3 S EXAFS: Does not provide a unique 3D structure Interpretation still controversial! (Clausen; Prins; Breysse; ) R(Å) Clausen, Topsøe et. al (1981) 6

7 Do we get what we need? YES, but Key challenges for industrial use of RI s - 1 Large expenses, large distance travel, hotel, beamtime, equipment Many experienced researchers needed for one experiment Complex experiments, unique results?, complex data analysis Peer review system for beamtime applications: Judged on scientific quality, not on technological quality or industrial relevance Confidentiality, IPR, secrecy agreements, bureaucracy Beamline/experimental staff: Lack of staff: experiments run 24 hours/day, but staff not always available Lack of experienced staff (short-term contracts) Full remote control of experiments is hardly possible Extra facilities, e.g. preparation lab not always available 7

8 Key challenges for industrial use of RI s - 2 Differences with academic use of large-scale facilities: Industry: larger amount of samples; model vs. real catalysts Industry: faster results are demanded: robust methods + on-line analysis + fast access to facilities Trend: reduced time from R&D to market Industry: product and process oriented RIs: method, instrument/beamline, fundamental understanding oriented Lack of quality control of beamlines/instruments: no standard protocols Lack of automated on-line data analysis and reduction software Lack of standardization: Interfaces between beamline and sample environment Data formats Limited interest in industrial use by many RI s Increase of industrial use of SR Short access time to beamlines (2-4 weeks), preferably at short distance from home laboratories Professional and reliable operation of beamlines and synchrotron State-of-the-art beamline equipment, laboratories (also for sample preparation) and data analysis Building and operation of beamlines is responsibility of SR sources industry is willing to pay for beamtime Beamline staff on long term contracts to improve competent service; basic understanding of catalytical processes performed present at beamline Coordination of industrial beamtime applications by an industrial user office to ensure use of the proper beamlines + scientific support Partly from: Final declaration at Industrieforum In Situ Charakterisierung Katalytischer Prozesse, Nov. 2003, Hasylab (Bessy, Anka) 8

9 Thank you for your attention Catalyzing your business Future possibilities for industrial use of RI s Imaging: Nano-tomography including element mapping as complementary method to transmission electron tomography: X-rays have larger penetration depth: in situ studies on < 10 nm length scale Design of new facilities: workhorses vs. high brilliance Improved instrumentation (detectors): Follow dynamic changes on short (<1ms) time scale e.g. during crystallization and agglomeration of catalysts New methods and techniques: Improve sensitivity for surface and active sites XFEL: Femtochemistry: Movie of chemical reaction during adsorption and desorption of gasses at a catalyst surface 9

10 Use of RIs at Haldor Topsøe A/S: Since 1981 (synchrotron): About 3 refereed publications by HTA/S authors per year (average): fundamental understanding Techniques used: XAFS, XRD, X-ray tomography, SAXS, XRF, XPS, XPCS Synchrotrons used: HASYLAB, ESRF, SLS, ASTRID, MAXLAB Amount of beam time per year: ~120 shifts (8 hour) Topsøe - A global supplier of catalysts and technologies Headquarters Topsøe offices Research Production Engineering Sale & Marketing Alberta Copenhagen Moscow Los Angeles Houston Bahrain New Delhi Beijing Kuala Lumpur Rio Buenos Aires Cape Town Subsidiaries Haldor Topsoe, Inc. Haldor Topsøe International A/S, Denmark Haldor Topsoe India Pvt. Ltd. India ZAO Haldor Topsøe, Russia Subcontinent Ammonia Investment Company ApS (SAICA) Topsoe Fuel Cell A/S, Denmark 10

11 and a leading market player Market share between 15-25% for established products Supplier of solutions for 50% of new ammonia plants built within the last decade More than 60% of ammonia is produced worldwide on Topsøe catalyst Supplier for 40% of catalysts for production of ultra-low sulphur diesel > 30% market share of hydrogen catalysts Many leading environmental technologies 30% market share of FCC pretreatment catalysts 20% market share of hydrocracking catalysts Topsøe is dedicated to Research and development in heterogeneous catalysis Production and sale of catalysts Licensing of technology Equipment supply Engineering and construction of plants based on catalytic processes 11

12 Research for process and catalyst development 300 employees in R&D Topsøe annually applies 10% of gross revenues to support these R&D efforts Industry Basic Research Fundamental Studies Catalyst Characterisation Scale-up Pilot Operation Computer Modelling Catalyst Formulation Process Development R&D is multi-disciplined Fundamental research Catalyst development Catalyst manufacturing Pilot plant studies Process development Process impact studies Equipment development Computer modelling Catalysts Catalyst production and supply Loading/start-up assistance to operators Troubleshooting assistance Analysis of plant operation 12

13 Catalysing your business 13