Key challenges for industrial use of research infrastructure

Alfons Molenbroekam@topsoe.dk

Haldor Topsøe A/S Catalyzing your business

Workshop - Forskningsinfrastruktur för industriella innovationer, 14 June 2012, Stockholm

Established 1940 Ownership: Haldor Topsøe Holding A/S (100%) Annual turnover (2011): ~600 MM EUR (> 4.46 billion DKK ) Number of employees ~2200

Topsøe Group’s headquartersin Lyngby, Denmark

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)

World population

– Food shortage

Resources

– Efficient use of resources

Pollution

– Reduction of smog, acid rain

Global Challenges

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)

In situ techniques in catalysis

Products - Mass Spectrometer

Reactants - Gas control system

XRD

EXAFS

TEM

Radiation: X-raysLight

Electrons

Relate Relate StructureStructureto to ActivityActivity

underunderprocess conditions process conditions

IR

Raman

SAXS

SEM

Tomography

Ammonia Synthesis Catalyst

It is the know-how that counts

N2(g) + 3 H2(g) → 2 NH3(g) Fe/FeO-catalyst

1 kg of catalyst → 25 tonnes of NH3

Annual production: 150*106 tonnes No catalyst? <150 tonnes

Wor

ld p

opul

ati o

n ( b

i lli o

ns)

Ann

ual u

se o

f fer

ti li z

er (

106

tonn

es)

1990

Wor

ld p

opul

ati o

n ( b

i lli o

ns) 10

9

8

7

6

5

4

3

20102030

20502070

20902110

21302150

Year

0

6

5

4

3

2

1

80

60

40

20

100

01900 1925 1950 1975

Year

World Population

PredictionPrediction (2 children/woman)

TK-558 BRIM™ (CoMo) andTK-559 BRIM™ (NiMo) for FCC P/TTK-576 BRIM™ (CoMo) for ULSD

Recent industrial refinery catalysts

Haldor Topsøe has introduced new generations of hydrotreating catalysts

Aided by the input from molecular-scale research

Named BRIM™ Technology

First in situ EXAFS Studies

of CoMo/Al2O3 Catalysts

2 4 6 8 10 R(Å)

Rel

ati

ve

mag

nit

ud

e

Sulf. CoMo/Al2O3

Sulf. Mo/Al2O3

Bulk MoS2

Clausen, Topsøe et. al (1981)

Mo present asMoS2 nanoclusters

Mo

S

In situ FTIR:Monolayers

(single MoS2 slabs)

N.Topsøe (1980)

New In Situ Techniques Provided Insight

First in situ EXAFS Studies

of CoMo/Al2O3 Catalysts

2 4 6 8 10 R(Å)

Rel

ati

ve

mag

nit

ud

e

Sulf. CoMo/Al2O3

Sulf. Mo/Al2O3

Bulk MoS2

Clausen, Topsøe et. al (1981)

Mo present asMoS2 nanoclusters

Mo

S

EXAFS: Does not providea unique 3D structure

Interpretation still controversial!(Clausen; Prins; Breysse;…)

New In Situ Techniques Provided Insight

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

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 orientedRIs: 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)

Thank you for your attention

Catalyzing your business