(643b) From High Throughput Lab to Pilot-Plant Scale – Parallel Testing of Hydroprocessing Catalysts

From high throughput
lab to pilot plant scale ?

Parallel testing of Hydroprocessing Catalysts

Sascha Vukojevic*, Florian Huber, Tilman Sauer, Jochen Berg,
Alfred Haas

hte Aktiengesellschaft -the high throughput
experimentation company-, Kurpfalzring 104, 69123 Heidelberg, Germany

www.hte-company.com

*Sascha.Vukojevic@hte-company.de

Introduction

Increasing global demands for fuels, the tightening of
environmental regulations and the optimization of refineries has led to an
increasing demand for commercial catalyst testing capacity for refining
applications. High throughput catalyst testing is a time and cost efficient
approach that can meet this demand. In the past, the domain of high throughput
testing was the evaluation of powder samples (typically below 200 μm).
Over the last couple of years hte has developed standard operating procedures
(SOP) for parallel testing of commercial catalyst sizes (typical diameter for
extrudated hydroprocessing catalysts of around 1.5 mm) at scales of 1 to 100
ml.

A
typical example for comparative testing of commercial catalysts in the refining
area is the ranking of hydroprocessing catalysts for HDS, HDN and HAD
applications. Depending on the scope of the catalyst evaluation, different
bench-scale reactor systems can be used. Catalyst development and discovery,
hence screening of a large  number of powder-, or full-size extrudated catalyst
samples with main focus on catalyst activity and basic product characteristics
calls for small catalyst amounts (typically 1-3 ml) and high degree of
parallelization (typically 16-fold high throughput systems). Ranking of
catalysts for commercial scale installations with focus on catalyst performance
as well as detailed product characteristics requires somewhat larger catalyst
amounts (typically 5 ? 50 ml) and modest degree of parallelization (typically
4-fold pilot plant reactor systems).

In
the present case study, we will discuss the progress in experimental procedures
and workflows developed at hte company for ranking commercial catalysts at
these different scales in parallel fixed-bed trickle flow reactor systems. The
latest developments in the field of high throughput reactor technology for
refinery applications will also be shown, including parallel catalyst testing
technology in a pilot-plant scale with higher catalyst volumes.

Results and
Discussion

Figure
1 shows the comparison of two commercial HDS catalysts in a 16-fold high
throughput reactor system with a catalyst volume of 1.5 ml. The comparison is
based on the ratio of the reaction rate constants. Figure 2 shows the
comparison for the same two catalysts tested in a 4-fold pilot plant reactor
system with a catalyst volume of 35 ml. When comparing both figures, it can be
seen that catalyst ranking at different scales gives the same result when
proper experimental procedures are applied. In addition, it can be seen that
small scale high throughput setups can have higher data resolution and better
statistics.

The
aim of the hte workflows is not only to rank catalysts at a certain scale under
given fluid dynamic conditions, but even more important to get the same
quantitative ranking at different scales by tuning the fluid dynamic
environment in the reactor systems. For instance, the comparison of Figure 1
and 2 shows that despite a scaling factor of around 20, the ranking in the
small scale 16-fold high throughput reactor system and the larger scale 4-fold
pilot plant reactor system gives the same quantitative result. Consequently,
these workflows allow up- or downscaling of commercial catalyst testing in
bench-scale reactor systems depending on the focus of a testing campaign.

Figure 1  Comparison of two
commercial HDS catalysts, A and B, in a 16-fold high throughput reactor
system (catalyst volume of 1.5 ml). Ratio of reaction rate constant
k_B/k_A and operation temperature as function of time on
stream.

Figure 2  Comparison of two
commercial HDS catalysts, A and B, in a 4-fold pilot plant reactor system
(catalyst volume of 35 ml). Ratio of reaction rate constant k_B/k_A
and operation temperature as function of time on stream.

In our case study, we will present the latest
trickle-flow reactor technology developments at for high throughput
experimentation in heterogeneous catalysis and discuss the variables that can
be tuned to control and compare the hydrodynamics of gas and liquid flow at
different scales ? from lab scale to pilot plant scale. Especially the
importance of reproducible reactor packing and controlling the particle size
distribution of diluent materials will be emphasized.