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Succeed at
Catalyst SCALE-UP
Uday T. Turaga
Donald R. Engelbert
William H. Beever
ConocoPhillips Co.
J. Todd Osbourne
Ben Wagner
Richard Allen
Jeff Braden
Sd-Chemie Inc.
Polymers and
Polyolefins
21%
Petroleum
Refining
24%
atalysts are of vital importance to the global chemical, petrochemical, petroleum refining and transportation sectors. By some estimates, catalysts
have enabled worldwide value of trillions of dollars. In
2004, the global catalyst market was estimated to be worth
$10.5 billion (1). The figure shows the major catalyst
applications and their relative share of the global catalyst
market (13).
Catalysts have been a subject of vigorous research and
development in the last 50 years. Catalysts have helped
produce new and important chemicals, fuels and materials.
As a science, catalyst development has evolved from a
point where the catalyst was merely a serendipitously discovered and valuable black box, to the situation today
where modern synthesis, characterization, reaction and
kinetic modeling techniques have led researchers to confidently boast of their ability to design catalysts for whatever application they desire.
Most of these important advances have focused on
characterizing catalysts, discovering new catalysts, or
unraveling reaction schemes and kinetics occurring on catalytic surfaces. Little research has focused on understanding and improving the scale-up and commercialization of
laboratory-scale catalyst discoveries. Scale-up and commercialization continues to be mostly a trial-and-error
process. It is generally governed by empirical and experiential insights, and can take a long time.
Even so, the last decade has witnessed another wave of
Chemical
Industry
26%
Environmental
Control
29%
exciting scientific developments and innovations in catalysis. Some of the factors contributing to these developments
are: new methods and approaches to catalyst development
and testing (e.g., combinatorial catalysis); new problems
where catalysts play an important role (e.g., hydrogen production); the increasing interdisciplinary nature of catalysis
(e.g., catalysis through polyfunctional materials); an intensifying focus on continued process improvements (e.g.,
next-generation hydrotreating catalysts); identification of
appropriate catalyst systems for specific applications and
reactors (Table 1); and creation of new processes (e.g., catalytic processing of renewable feedstocks).
Clearly, the relative importance of scale-up and comCEP
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Shape
Dimension
Reactor Application
Microsphere
Dia = 20100 mm
Spheres
Dia = 110 mm
Granules
Dia = 120 mm
Fixed bed
Beads
Dia = 15 mm
Pellets
Extrudates
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Albemarle
Alcoa
Axens/Procatalyse
BASF
Criterion Catalysts
Engelhard
Grace Davison
Haldor Topsoe, Inc.
Intercat
PQ Corporation
Sd-Chemie, Inc.
Tricat
Zeochem
www.akzonobel-catalysts.com
www.adcats.alcoa.com
www.axens.net
www.basf.com
www.criterioncatalysts.com/
www.engelhard.com
www.gracedavison.com
www.topsoe.dk
www.intercatinc.com/
www.pqcorp.com
www.sud-chemie.com
www.tricatgroup.com
www.zeochem.com
Accelerate scale-up
using statistically designed experiments
Once researchers identify a promising lead, it often has to
be optimized for product properties and process parameters.
Because time and budgets are frequently limited, optimization efforts must be speedy, cost-effective and focused,
which can be accomplished using statistically designed
experiments and other Six Sigma techniques. In addition to
reducing time and work, such tools identify the effects of,
relationships between, and relative importance of multiple
variables. In designing the optimization studies, it is important to include all of the relevant scale-up variables.
Catalyst discovery programs focus on improving one or
two major properties, typically activity or selectivity. As a
result, during discovery, limited attention is paid to characterizing other properties, such as particle strength, particle size
distribution, density, flow properties, pore volume, surface
area, metal dispersion, crystallinity and morphology. Nevertheless, scale-up requires careful attention to all of the resulting products physical and chemical properties, since each
plays an important role and cannot be compromised. Often,
Table 3. Important unit operations in catalyst scale-up and manufacturing (6, 7).
Unit Operation
Description
Precipitation /
Co-precipitation
Solution/Slurry
Transfer
Vessel-to-vessel transfer of
solutions and slurries
Filtration
Drying
Calcination
High-temperature-assisted
solid-state reactions to
complete product activation,
impart strength and eliminate
templates and salts
Washing /
Ion-Exchange
Compaction /
Densification
Spray Drying
Crushing and
Screening
Coating
Three-way catalysts
Impregnation
improved understanding of the effects of manufacturing variations on critical product properties; and the development of
a commercial manufacturing process with Six Sigma capability, i.e., less then four defects per million opportunities (4).
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Literature Cited
1.
2.
3.
4.
5.
6.
7.
Acknowledgements
The authors acknowledge several useful discussions with current and past
colleagues, including Jim Scinta, Dennis Kidd, Ed Sughrue, Jason
Gislason, Ryan Zarnitz, Gary Hatfield and Debbie Just. In addition,
Richard Allen, Jeff Braden, Todd Osbourne, Ben Wagner, Eric Lowenthal,
Raj Rajagopalan, Marius Vaarkamp, John Macoay and John Henderson,
technical personnel from various catalyst vendors with whom the
authors have collaborated, are also acknowledged. The authors are
grateful to ConocoPhillips for permission to publish this paper.
process parameter measurements must yield samples capable of providing a diagnostic fingerprint of the commercial
campaign so that problems can be isolated and identified
should the product not meet specifications.
Closing thoughts
Catalysts will continue to play a vital role in improving the quality of modern life through the production of
chemicals, fuels and materials, in addition to having
important environmental applications. Scale-up is the critical link that will bring laboratory-scale innovations into
the commercial marketplace. While new tools and techniques will improve and accelerate the scale-up process
(7), the five principles identified here provide a generic
framework for enhancing the success rate of this
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vital link in the innovation chain.
UDAY T. TURAGA is an associate scientist in the Advanced Technology
Division, Downstream Technology, at ConocoPhillips Co.s Bartlesville
Technology Center (Bartlesville, OK 74006; Phone: (918) 661-0113; Email: Uday.T.Turaga@ConocoPhillips.com), where he has been involved
with the development, scale-up and commercialization of sorbents for
the proprietary S Zorb sulfur removal technology for gasoline
desulfurization since May 2002. He holds Bachelors and Masters
degrees in chemistry from the Univ. of Delhi in India and a doctorate in
fuel science from Pennsylvania State Univ.
DONALD R. ENGELBERT is a senior technologist at ConocoPhillips with 16
years experience in catalyst and sorbent synthesis, characterization,
scale-up and manufacturing. He has been involved with a suite of
proprietary catalysts and sorbents, including the sorbents used for the
S Zorb sulfur removal technology.
WILLIAM H. BEEVER leads the sorbent development group for the S Zorb
sulfur removal technology at ConocoPhillips. During his 25 years with
the company, his responsibilities have included managerial positions
leading several innovation projects in plastics, composite materials,
polyolefins and catalysts. He received Bachelors, Masters, and
doctoral degrees in chemistry from Missouri Western State College, the
Univ. of Iowa, and Colorado State Univ., respectively.
JOSEPH TODD OSBOURNE is the manager of the South Pilot Plant at SdChemie Inc. (Louisville, KY), where he has worked in refinery zeolite
catalyst R&D and led one of SCIs pilot plants. He has served as a team
member, project leader and technical resource on several custom
catalyst development projects, including sorbents used for the S Zorb
sulfur removal technology. He holds a Bachelors degree in chemistry
and mathematics from Campbellsville Univ.
BEN WAGNER has worked as an engineer in one of the pilot plants at SdChemie Inc. since May 2003. He holds a BS in chemical engineering
from the Univ. of Cincinnati.
RICHARD ALLEN has been employed by Sd-Chemie Inc. for 25 years in
various manufacturing managerial positions, which now involves the
scaling up of products from the pilot plant to commercial production,
including the sorbents for the S Zorb sulfur removal technology. He
received a Bachelors degree in chemical engineering from Eastern
Kentucky Univ. and an MBA from Bellarmine College.
JEFF BRADEN is currently director of sales and marketing for Sd-Chemie
Inc.s refinery catalysts, having worked for the firm for 22 years as an
R&D group leader, process control and product development manager,
and production manager. He received a BS in chemistry from the Univ.
of Louisville and an MBA from Indiana Univ.
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