Combining New and Old Technologies -
Inlet Diffuser and Random Packing
Dramatically Improve Reactor
Performance
Garry E. Jacobs
Technical Director,
Process Engineering
Fluor Enterprises, Inc.
Aliso Viejo, CA, USA
Gerianne D’Angelo
Senior Technical Service Engineer
ADVANCED REFINING
TECHNOLOGIES
Chicago, IL USA
he performance of hydropro-
T cessing reactor internals has
improved significantly over
the past decade, driven in part by
ultra low sulfur product specifications.
Yet, some reactors continue to operate
with internals that are inadequate for
the operating conditions. This inade-
quacy may be caused by the intro-
duction of heavier feedstocks or by
constraints that preclude installation of
the appropriate hardware.
This paper presents the case history
of a kerosene hydrotreater that failed
to meet product sulfur targets, subse-
quent to a catalyst changeout. The
reactor operates with a mixed-phase
ART Catalagram® 104 Special Edition Fall 2008 19
feed, but is lacking a liquid distribu-
tion tray. Troubleshooting work
included pilot plant testing of the
catalyst retains, leak testing of the
feed/effluent exchangers, and
radioactive tracer tests and gamma
scans of the reactor. A charge rate
test was also performed which sug-
gested significant underutilization of
the catalyst. Evidence of liquid
maldistribution was also obtained
by visual inspection of the catalyst
bed surface and analysis of “spent”
catalyst samples.
Using computational fluid dynamic
(CFD) modeling, a new inlet diffuser
was designed to improve liquid dis-
 Figure 1
Existing Inlet Diffuser
tribution to the top of the catalyst
bed and was installed during a cat-
alyst changeout. In addition, high
void fraction random packing was
loaded at the top of the bed to pro-
mote radial liquid dispersion. After
restart of the unit, the reactor was
able to meet the refiner’s 10 ppmw
sulfur target for ultra low sulfur
kerosene (ULSK) product.
Background
Subsequent to a catalyst changeout
in the spring of 2007, a kerosene
hydrotreater failed to meet ULSK
specifications. The unit feed con-
sists of a mixture of straight-run
kerosene and coker naphthas.
During the previous catalyst cycle,
the reactor initially treated only fully
vaporized naphtha. A couple of
years into that eight-year cycle, the
straight-run kerosene was intro-
duced, creating a mixed phase
feed. During the final year of that
cycle, the reactor was able to pro-
duce ULSK. The catalyst change-
out was dictated by concerns of sil-
icon breakthrough into the reformer
feed.
The reactor did not have a liquid
distribution tray. The distribution
hardware consisted solely of a
basic inlet diffuser, shown in
20 www.e-catalysts.com
Troubleshooting Activities
A simplified comparison of the
operating conditions and perform-
ance for the two catalyst cycles is
presented in Table I. Of particular
note was the approximately 1½-PSI
reactor pressure drop through the
post 2007 T/A catalyst load. With
uniform vapor/liquid distribution, the
pressure drop should be at least
two times higher. This was the first
evidence of significant liquid mal-
distribution. The ensuing trouble-
shooting activities further explored
this and other possible causes of
the higher-than-expected product
sulfur levels.
Feed/Effluent Exchangers
When producing ultra low sulfur dis-
tillates, extremely small and previ-
ously unnoticeable leaks in
Figure 1. The inlet diffuser is insert- feed/effluent exchangers can result
ed in the reactor inlet nozzle and in off-spec product. Several tech-
helps dissipate the momentum of the niques were used by the refiner to
incoming feed. The addition of a check for such leakage, including
tray was considered by refinery per- feed and product sulfur speciations
sonnel, but could not be justified and tracer tests. If raw feed is leak-
based on acceptable performance ing into the reactor effluent, then
during the catalyst cycle leading up easily hydrotreated sulfur com-
to the 2007 turnaround. pounds (e.g., mercaptans and
alkylthiophenes) will be present in
the product. The speciation results
Table I
Comparison of Operating Conditions and Performance
Catalyst Cycle 1999-2007 Post- 2007 T/A
Naphtha Only (~2 Yrs)
Feedstock Naphtha + Kerosene (~6Yrs) Naphtha + Kerosene
Loading Method Sock Dense
Severity ULSK (Final Year) Inadequate HDS
Axial Temp Profile Typical Typical
Pressure Drop 7 - 9 PSI (Final Year) ~1 1/2 PSI
T/A Observations No Agglomeration
confirmed the presence of mercap-
tans, but not propyl- and lighter thio-
phenes that were abundantly pres-
ent in the feed. The absence of
these thiophenic compounds, which
can not be produced by recombina-
tion reactions, provided strong evi-
dence that feed/effluent exchanger
leakage was not the cause of high
sulfur levels in the kerosene prod-
uct. This result also indicates that
the mercaptans were formed by
recombination reactions, as dis-
cussed subsequently.
Two tracer tests were also per-
formed on the feed/effluent
exchangers. In separate tests, a
high volatility sulfiding agent and a
radioactive noble gas tracer were
injected on the feed side of the
exchangers. The effluent side of
the exchangers was then monitored
for presence of tracer. Both tests
indicated no leakage across the
exchangers, within detection limits.
Implicitly, the absence of sulfiding
agent in the reactor effluent was
also an indication of liquid phase
maldistribution, as the fully vapor-
ized sulfiding agent was completely
converted to hydrogen sulfide in the
reactor.
Catalyst Activity
Since the reactor does not have a
distribution tray, liquid phase sulfid-
ing could not ensure proper activa-
tion of the entire catalyst load. For
this reason, vapor phase sulfiding
was performed using dimethyl
disulfide (DMDS). The sulfiding
step was uneventful, with the low-
and high-temperature hydrogen sul-
fide breakthroughs occurring as
expected.
The catalyst Certificate of Analysis
(COA) was reviewed and found in
compliance with the Process and
Quality Assurance Specifications.
Catalyst retains from the commer-
cial reactor were loaded in a pilot
plant reactor and tested using a
representative blend of the refiner’s
feedstocks. For comparison, a stan-
dard sample of the same catalyst
type was also tested in the pilot
plant. The results confirmed that
Figure 2
Radioactive Tracer Test Results
0
1
2
3
Distance from Top Tangent Line (ft.)
4
5
6
7
8
9
10
11
12
13
14
15
100 1000 10000 100000
Radiaton Intensity (Counts per Time Interval)
the activity of the retained sample was services company to perform two
essentially equal to that of the stan- separate tests.
dard sample, within pilot plant testing
tolerances. Furthermore, the temper- Radioactive Tracer Test
ature required to meet the ULSK sulfur
target in the pilot plant was actually The radioactive tracer test was
10°F lower than the SOR projection for intended to quantify the liquid distri-
the commercial reactor. bution within the catalyst bed. A
radioactive halogenated hydrocar-
The pilot plant results indicated an bon was injected into the reactor
activity disparity of approximately feed. As the feed mixture passed
60°F, compared with commercial unit through the bed, the radioactive
performance. This is roughly equiva- halogen adsorbed onto the catalyst.
lent to a 16-fold difference in space Eight uniformly spaced detectors
velocity. At first glance, this disparity were then lowered about the periph-
may seem too dramatic to be ery of the reactor, and radiation
explained by liquid maldistribution. measurements were obtained at
This point will be addressed subse- multiple elevations.
quently, with the benefit of further
observations. The results of this radioactive tracer
test are shown in Figure 2. The rel-
Vapor/Liquid Distribution Within the ative uniformity of the eight scan
Reactor lines was interpreted as an indica-
tion of “…good liquid distribution
To explore the possibility of liquid within the bed…”, with the caveat
maldistribution within the reactor, the that the test could not identify
refiner utilized a process diagnostics axisymmetric maldistribution.
ART Catalagram® 104 Special Edition Fall 2008 21

Normalized Radar Plots of Radioactive Tracer Test Results
A B
N 2.00 N
2.00
NW 1.50
1.00
0.50
W 0.00
SW
S
4.0 ft. 5.0 ft. 6.0 ft.
Unfortunately, this tracer test was
significantly flawed. A simple flash
calculation at the reactor inlet oper-
ating conditions revealed that the
halogenated hydrocarbon tracer
was approximately 50% vaporized.
Therefore, the results did not pro-
vide an accurate indication of the
liquid distribution, as tracer from the
vapor phase also adsorbed onto the
catalyst. A closer examination of
the data suggests the results are
actually indicative of the vapor
phase distribution.
At each elevation, the raw data was
normalized and graphed on radar
plots (see Figure 3), to facilitate
visualization and interpretation.
• Figure 3A indicates that the
peak tracer deposition shifted from
the E/SE region to the S/SW region.
This shift occurred between the 5’-
0” and 6’-0” elevations, which is
consistent with the transition from
¼” grading to 1/10” silicon guard
catalyst.
• Figure 3B indicates that
another shift in the peak tracer dep-
osition occurred (from the S/SW
region to the West region) between
the 8’-0” and 9’-0” elevations. This
shift is consistent with the transition
from 1/10” silicon guard catalyst to
1/20” HDS catalyst.
• Figure 3C indicates that the
peak tracer deposition stabilized in
the West region through the 12’ 0”
22 www.e-catalysts.com
Figure 3
NW 1.50
NE
1.00
0.50
W 0.00
E E
SW
SE
S S
7.0 ft. 7.0 ft. 8.0 ft. 9.0 ft.
elevation. Minimum tracer deposition
stabilized in the SE region.
These shifts in peak tracer deposition
occurred rapidly, within elevation
changes of one foot or less. In this
reactor, vapor is the continuous
phase. Liquid trickles over the grad-
ing and catalyst, and as such, can not
make rapid radial transitions.
Therefore, the rapid shifts shown in
Figure 3 are likely attributable to
changes in the vapor flow path,
caused by porosity variations. If this
interpretation is correct, the tracer
data indicates locally high and low
vapor-phase space velocities, respec-
tively, in the West and SE regions.
These deviations from uniform flow,
however, are not of the magnitude
necessary to explain the poor reactor
performance. Most notably, the tracer
results provided no meaningful infor-
mation on the liquid-phase distribu-
tion.
Gamma Scan
The gamma scan was intended to
quantify the vapor and liquid distribu-
tion prior to entering the catalyst bed.
A 9 x 9 horizontal fan-patterned scan
was performed, utilizing 9 source
placements and 9 detector place-
ments. The 81 data points were used
to produce the results shown graphi-
cally in Figure 4. This figure indicates
very high densities near the reactor
wall and very low densities in the cen-
C
N
2.00
NE 1.50
NW NE
1.00
0.50
E W 0.00
SE SW SE
10.0 ft. 10.0 ft. 11.0 ft. 12.0 ft.
ter of the reactor. The results were
interpreted as evidence of an
“…annular flow pattern…” with
“…virtually no (liquid) flow in the
center of the bed…”.
An alternate, more probable inter-
pretation of Figure 4 is that the reac-
tor wall was too thick (~3”) to pro-
vide any meaningful information
about the phase distribution above
the bed. As presented below, evi-
dence gathered during the subse-
quent turnaround confirmed liquid
flow primarily in the central region of
the bed. The limitations of gamma
scan technology are discussed
elsewhere.
Charge Rate Test
A charge rate test was performed to
provide an indication of catalyst uti-
lization. The test is performed at
two different reactor feed rates (i.e.,
space velocities), holding feed
quality, reactor temperature, and
gas-to-oil ratio constant. Catalyst
activity is dictated primarily by the
latter two variables. Therefore, the
rate constants for both space veloc-
ities can be equated, as shown in
Equation 1. The feed and product
sulfur concentrations, along with the
two space velocities, are inserted
into this equation to determine the
apparent HDS reaction order, n.
 Figure 4 Intrinsic kinetics for individual sulfur-
Gamma Scan Above Catalyst Bed bearing species (e.g., thiophene)
are generally first order with respect
to the species concentration.
However, petroleum-derived oils
contain a broad spectrum of sulfur
species, with widely varying reactiv-
ities. This wide variation increases
the apparent (i.e., observed) HDS
reaction order to 1.5 – 2.0 for bulk
desulfurization.

The processing objective of the

kerosene hydrotreater is ~99.5%
HDS. This level of treating is beyond
bulk desulfurization, with only alkyl-
benzothiophenes remaining in the
reactor effluent. Therefore, the
apparent reaction order is likely in
the range of 1.0 – 1.5. In contrast,
the charge rate test indicated an
apparent reaction order of 4.3,
which corresponds to 25 – 30% of
the catalyst not being utilized,
depending upon the assumed reac-
tion order (see Figure 5).

Equation 1 The charge rate test has shortcom-

Analyzing Charge Rate Test by Equating Rate Constants ings, though. It does not consider
whether the reacting sulfur species
are present in the vapor phase, liq-
uid phase, or both phases. In this
regard, it seems more applicable for
troubleshooting reactors in which
the reacting species remain pre-
dominantly in the liquid phase at the
reactor operating conditions (e.g.,
gas oil hydrotreaters). This was not
Figure 5
the case for the kerosene
Estimate of Unused Catalyst (Based on Charge Rate Test) hydrotreater, as approximately 35%
of the feed was in the vapor phase
during the charge rate test.
Observed HDS Reaction Order

Subsequent to these troubleshoot-

ing activities, the refiner requested
that Fluor design a new inlet diffuser
to improve liquid distribution to the
catalyst bed.

Inlet Diffuser and Random

Packing Improve Liquid
Distribution

The vapor and liquid phases enter-

ing a reactor can be highly maldis-
tributed due to the impact of the
elbows in the reactor feed line, just
upstream of the inlet nozzle. The
flow paths taken by both phases are
% of Catalyst Not Utilized dependent upon their relative
ART Catalagram® 104 Special Edition Fall 2008 23
 momentums and the piping geome- Figure 6
try, and are not easily predicted Vapor/Liquid Maldistribution at Reactor Inlet
without a tool such as CFD. The
potential extent of maldistribution is
illustrated in Figure 6.

This picture is the result of CFD

modeling of the refiner’s reactor
inlet line. The model extends from
near the heater outlet, through the
combining tee, and along the com-
mon line to the reactor inlet. In the
picture, the interface between the
vapor phase and the liquid phase is
green. At the inlet to the vertical
run, the liquid collects on the far
side of the elbow. In the horizontal
run above the reactor, the flow
begins transitioning into a stratified
regime, with the majority of the liq-
uid flowing along the bottom of the
line. At the final elbow, the liquid’s
momentum carries it to the far side Figure 7
(i.e., east side) of the reactor inlet Fluor Inlet Diffuser
nozzle.

The inset circular image is a cross-

sectional view, just as the flow pass-
es through the reducing flange and
enters the top of the reactor. In this
image, the liquid is red and the
vapor is blue. The two phases are
quite segregated, with liquid heavily
biased toward the east side of the
reactor. The function of the Fluor
inlet diffuser is to correct this mald-
istribution.

New Technology: U.S. Patent No.

7,281,702

Fluor’s patented inlet diffuser is

illustrated in Figure 7. It has been
designed to accommodate the wide
variations in vapor and liquid mal-
distribution that may occur due to
different operating conditions and
reactor inlet line routings. This dif- Figure 8
fuser utilizes three stages, con-
tained in a cylindrical cartridge, fol- Inlet Diffuser Liquid Spray Pattern
lowed by a deflector plate. Each
stage consists of two sets of vanes.
Flow is outward through the upper
set of vanes and inward through the
lower set of vanes.

The upper vanes induce swirling,

which forces the liquid toward the
cartridge wall, creating hold up (i.e.,
allowing the vapor to slip past the
24 www.e-catalysts.com
liquid). The lower vanes act as vor- Figure 9
tex breakers, reducing the swirl of 50mm Ceramic Raschig Rings
the inflowing fluid. The fluid flows
downward in the center of the car-
tridge to pass from one stage to the
next. The swirling action redistrib-
utes the liquid circumferentially.
Exiting the third stage, the liquid
and vapor discharge onto a deflec-
tor plate, creating a hollow cone
spray pattern (see Figure 8).

With this spray pattern, liquid wet-

ting at the top of the catalyst bed is
in the form of an annular ring. The
benefits of an annular ring wetting
pattern have been revealed and uti-
lized , previously. Prior to reaching
the active catalyst, liquid distribu-
tion within the bed can be further
improved using old technology.

Old Technology – Raschig Rings (Courtesy of Saint-Gobain NorPro)

Raschig rings (see Figure 9) were

invented at the end of the 19th cen-
tury by Fritz Raschig to improve the packings to be objectively compared. refiner install a custom designed
fractionation of carbolic acid. The radial dispersion coefficient is inlet diffuser, along with 3 feet of 50-
Since then, higher efficiency ran- dependent upon the packing diame- mm raschig rings, loaded on top of
dom packings have been devel- ter. Figure 10 illustrates that 50-mm the existing catalyst. This combina-
oped for distillation applications. raschig rings are approximately three tion is illustrated in Figure 11. The
Interestingly, though, raschig rings times more effective than the 15-mm reactor feed liquid is treated in an
can still play an important role in spheres commonly used as grading in annular portion of the catalyst bed,
process engineering. These high hydroprocessing reactors. while the vaporized feed is treated
void fraction rings promote rapid liq- primarily in the unwetted portion.
uid dispersion in trickle flow appli- Combining Technologies
cations. This characteristic is quan- Unit Shutdown Activities
tified by a radial dispersion coeffi- To improve liquid distribution in the
cient, which allows various random reactor, Fluor recommended that the In the fall of 2007, the kerosene
hydrotreater was taken off-line. The
refiner felt that a catalyst changeout
Figure 10 was warranted, to maximize the
Radial Dispersion Coefficients probability of achieving ULSK sulfur
levels upon restart. Prior to unload-
6 ing, the top of the bed was visually
Radial Dispersion Coefficient (mm)

inspected. The inspection revealed

an ~3-foot diameter, ~8-inch deep
crater below the inlet diffuser. This
4 crater was unambiguous evidence
Raschig Rings that liquid had “channeled” down
the center of the reactor and
Pall Rings caused localized settling. Due to
2 the settling, the grading materials
had become intermixed. The
Spheres inspection confirmed the inaccura-
cy of the gamma scan results.
0 Approximately 4½ feet of grading
0 5 10 15 20 25 30 35 40 45 50 and catalyst were then vacuumed
Nominal Diameter (mm) from the top of the catalyst bed.
ART Catalagram® 104 Special Edition Fall 2008 25
 Figure 11
Improved Liquid Distribution
HDS catalyst samples were
obtained by coring several feet fur-
ther into the bed. The remaining
catalyst was dumped and the reac-
tor was sock loaded with new cata-
lyst. Because the catalyst did not
pack as densely as planned, only 2
feet of 50-mm raschig rings were
loaded on top of the bed. The Fluor
inlet diffuser was installed prior to
closing the reactor.
Post-Shutdown Performance
Activities
Subsequent to sulfiding activities,
the unit processed only the straight-
run kerosene for several days, after
which the coker naphtha was intro-
duced and operating severity was
slowly increased. The reactor was
able to produce ULSK at a temper-
ature level below the SOR projec-
tion. The refiner was extremely
pleased with the reactor perform-
ance.
Cored Catalyst Samples – Silicon
Loading
The cored catalyst samples were
analyzed for trace contaminants. Of
particular note were the silicon
loadings, as silicon can be used as
26 www.e-catalysts.com
a good marker of the liquid distribu-
tion. As shown in Figure 12, the cen-
ter and east samples contained signif-
icantly more silicon than the other
samples. This silicon distribution is
consistent with the observed crater
and with the CFD modeling (which
indicated an easterly bias to the
incoming liquid).
Cored Catalyst Sample – Activity
Testing
Catalyst from the east core sample
(with 0.68 wt.% silicon loading) was
loaded in a pilot plant reactor and
Figure 12
Silicon Loadings on Cored Catalyst Samples
tested side-by-side with a standard
sample of the same catalyst type.
The tests were performed using a
much heavier (API = 11°) distillate
feedstock, as the refiner’s feed
blend was no longer available. The
results indicated that the east core
sample was 5 – 7°F less active than
the standard sample, at ULSD prod-
uct sulfur levels. Therefore, within
the reproducibility of the pilot plant
testing, this core sample was only
marginally less active than the fresh
retains (tested during the perform-
ance troubleshooting). As such, it is
very inappropriate to refer to this
sample as ”spent” catalyst.
Observed Kinetics Revisited
With visual confirmation that liquid
had indeed channeled down
through the central region of the
reactor, the kinetic performance
during one of the troubleshooting
days was revisited. The basis for
this analysis is presented in Table II.
At the reactor operating conditions,
approximately 70% of the feed was
vaporized. The catalyst volume was
divided into two portions, with one
portion treating the vaporized feed
and the other portion treating the
unvaporized feed.
Gas distribution between the two
portions was estimated based on
the requirement of equal pressure
drop across both portions. The sig-
nificantly reduced gas flow in the
liquid wetted portion most likely
caused localized hydrogen starva- Table II
tion and “hot spots”, an environment Kinetic Analysis of Kerosene Reactor
which promotes mercaptan forma-
tion. Interestingly, mercaptan con-
(Accounting for Feed Vaporization and Liquid
centrations decreased at higher Maldistribution)
operating temperatures, which is
inconsistent with conventional wis- Unvaporized
Vaporized Feed
dom regarding recombination. Feed
Typically, recombination is attrib-
uted to very high operating temper- Unit Feed Rate (BPD) 13,100
atures , rather than localized hydro- Phase Split (BPD) 9,300 3,800
gen starvation. In this instance, API Gravity 41.6 38.8
higher reactor inlet temperatures
Total Sulfur (ppmw) 0.19
increased feed vaporization, which
TBP Distillation (˚F)
increased the gas-to-oil ratio (i.e.,
hydrogen partial pressure) in the 10% 262 310
wetted portion of the catalyst bed. 50% 369 420
90% 481 511
With an LHSV ≈ 3hr-1, the sulfur con-
tent of the vaporized portion is LHSV (hr1)
reduced to less than 1 ppmw. Overall 2.25
Based on an overall product sulfur Each Phase (Note 1) ~3 (Note 2) ~35
content (excluding mercaptans) of
~150 ppmw, the unvaporized por-
Gas-to-Oil Ratio (SCFB)
tion had to contain ~500 ppmw.
Overall ~1100
This concentration requires an
LHSV of approximately 35hr-1. The Each Phase (Note 3) > 1400 < 300
quantity of catalyst involved is
equivalent to the volume of a cone Catalyst WABT (˚F) Same for Both Phases
with a 3-ft. diameter base (i.e., the
diameter of the observed crater) Product Sulfur (ppmw)
and a height equal to that of the Total ~150 (excluding mercaptans)
HDS catalyst bed. Each Phase nil ~500

Repeat Charge Rate Test Notes:

1. Determined by kinetic analysis, using catalyst activity derived from pilot plant testing of
commercial retains.
The refiner is interested in repeating
2. LHSV≈3hr-1 required to treat vaporized feed to <1 ppmw sulfur. Actual LHSV is less
the charge rate test. This test
than 3hr-1.
requires that the coker naphtha be
3. Estimates - based on requirement of equal pressure drop for both the unwetted portion
removed from the unit feed. With no
(vaporized feed) and wetted portion (unvaporized feed) of the catalyst bed.
other convenient destination avail-
able, the test will not be conducted
until the coker is shut down for
maintenance.
It is also important to follow the trail For reactors operating with mixed
that the evidence provides. With cata- phase feed, an appropriately
Concluding Remarks
lyst activity confirmed by testing of the designed distribution tray maxi-
commercial retains and the possibility mizes catalyst utilization and result-
When troubleshooting reactor per-
of exchanger leakage eliminated by ing reactor performance. When
formance problems, it is very impor-
two independent tests, maldistribution installation of a distribution tray is
tant to understand the fundamentals
became the prime suspect. Very low not possible in a revamp applica-
behind the diagnostic tests being
pressure drop – about 1½ PSI – tion, liquid distribution can be
performed. Nothing hampers an
across the reactor was the first direct improved through the use of a new
investigation more than misconcep-
evidence of severe liquid maldistribu- technology, a unique inlet diffuser,
tions and misinformation. In the
tion. The mercaptan-containing prod- and an old technology, raschig
case history presented here, the
uct and the high apparent HDS reac- rings. Together these two elements,
“liquid” phase radioactive tracer
tion order provided further indications at very low relative cost, improve liq-
test results and the gamma scan
of liquid maldistribution. uid distribution and catalyst utiliza-
results both produced misinforma-
tion when producing ultra-low sulfur
tion regarding the vapor and liquid
products in a trayless reactor. The
distribution within the reactor.
ART Catalagram® 104 Special Edition Fall 2008 27
 alternative, neglecting liquid distri-
bution and hoping for adequate per-
formance, should be considered
too great an engineering and eco-
nomic risk to accept.
References
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node=208&/~=cb89f5851d60aae8
b6c72ce2779814d5
McCulloch, D. C., “Catalytic
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