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Reflux in a gas dehydration plant

ARTICLE in PETROLEUM TECHNOLOGY QUARTERLY · JANUARY 2014

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 Reflux in a gas dehydration plant

Gas dehydration by adsorbent processes may lead to the damaging regeneration

reflux phenomenon during adsorbent regeneration

SAJAD MIRIAN and HOSSEIN ANISI Nitel Pars Co (Fateh Group)

XIANG YU Hengye Chemical Co
SEPEHR SADIGHI Research Institute of Petroleum Industry

D
ehydration of natural gas adsorbent. Hence, the inlet section
entails the removal of water of the adsorption bed is faced imme-
that is associated with natural diately with a high temperature
gases in vapour form. The natural from the start of the regeneration
gas industry has recognised that without any heating ramp. Heating
dehydration is necessary to ensure up the adsorber without using a
smooth operation of gas transmis- heating ramp causes a strong
sion lines. This pretreatment Solid caked layer
temperature difference in the bed.
prevents the formation of gas of adsorbent and So, at the bottom, the molecular
hydrates and reduces corrosion. salt fused together sieve is very hot and desorbs the
The three major methods of dehy- adsorbed water while the top layers
Effective
dration are direct cooling, bed diameter are still at adsorption (low) tempera-
adsorption and absorption. ture. Therefore, water desorbed in
Adsorption-based processes for Original the bottom layer condenses in the
separation of multi-component bed diameter top layer. This phenomenon is
gaseous mixtures are becoming called refluxing or retro-condensa-
increasingly popular. The new tion. A schematic diagram of an
generation of synthetic and more adsorber with regeneration refluxing
selective adsorbents developed in is shown in Figure 1. To prevent this
recent years has enabled adsorp- catastrophic phenomenon, a good
tion-based technology to compete molecular sieve formulation (binder
successfully with traditional gas and zeolite) or improvement in the
separation techniques. Figure 1 Schematic of a bed faced with regeneration condition is inevitably
Any adsorption-based separation regeneration reflux required.
process requires two essential steps: In this article, modelling of the
adsorption during which one or applications such as carbon dioxide regeneration reflux phenomenon
more components are preferentially stripping from air. TSA exploits the during regeneration is performed
adsorbed/separated; and regenera- capacity of certain adsorbent mate- and the effects of it on the adsorp-
tion during which these rials, such as activated alumina, tion process are reviewed.
components are removed from the silica gel and zeolites, to adsorb Recommendations to prevent this
adsorbent bed. The adsorbent is gases at moderate temperatures phenomenon in a commercial scale
repeatedly used in cycles by carry- (40°C, 100°F) and later release them dehydration unit (as a case study)
ing out these two steps. When a when the temperature rises above are presented.
regeneration step is carried out 120°C (250°F).
through reduction of the total pres- Natural gas treating units using Process description
sure, the process is called pressure molecular sieves and TSA technol- The purpose of a natural gas dehy-
swing adsorption (PSA). ogy are usually optimised by dration package is to reduce the
Temperature swing adsorption manipulating both the adsorption water content of the natural gas to
(TSA) is another technique used for and the regeneration time. By reduc- avoid freezing and hydrate forma-
regenerating a bed of adsorbent ing the adsorption time, both the tion in the pipeline. In order to
that is loaded with the targeted vessel size and the amount of adsor- utilise natural gas for urban
impurity gas. This technology bent used are reduced. Therefore, consumption, the water dew point
began commercially in the 1960s the total cycle time is usually should be reduced to below -10°C,
and continues today for drying designed such that at the end of the accomplished by using a molecular
continuous air and natural gas adsorption a short time is available sieve adsorption unit which
as well as other purification for appropriate regeneration of the adsorbs water from the inlet gas.

www.eptq.com PTQ Q4 2014 75

ripi.indd 1 10/09/2014 13:49

 the regeneration step is replaced. Energy equation:
Adsorption Regeneration During the regeneration process, a
mode mode
regenerative gas stream is passed ∂T
( ρC p ) eq + ρC p u ⋅ ∇T = ∇ ⋅ (keq ∇T ) + Q
through a heater where it is heated ∂t
to approximately 270°C. This hot Mass equation:
gas passes upwards through the
∂ci
offline saturated dryer heating the + ∇.( − Di ∇ci ) + u ⋅ ∇ci = Ri
∂t
molecular sieves. As the sieves are
heated up, adsorbed water begins In these equations, ρ (kg/m3) is
to desorb and is carried away by the density of the fluid; t (s) is the
the hot gas. The operating condi- time; u (m/s) is the velocity vector;
tions of the target adsorption and Qbr (kg/m3·s) is the mass source or
regeneration processes and specifi- mass sink; εp is the porosity of bed;
cations of their feeds are shown in P (Pa) is the pressure; µ (kg/m·s) is
Table 1 and Table 2, respectively. the dynamic viscosity of the fluid; κ
Figure 2 Schematic diagram of the (m2) is the permeability tensor of
dehydration unit studied Mathematical modelling the porous medium; βF (kg/m4) is
of regeneration Forchheimer drag option; F (kg/
To perform such a process, water A computational fluid dynamic m2·s2) is the influence of gravity
saturated natural gas from the modelling technique was used to and other volume forces; (ρCp)eq is
upstream unit is sent to the molec- model the momentum, heat content the equivalent volumetric heat
ular sieve dehydration plant where and mass transfer of fluid through capacity at constant pressure; T (K)
the gas stream passes through a porous media, and also to investi- is the bed temperature; Cp is the
separator to retain any free water gate the refluxing phenomenon in fluid heat capacity at constant pres-
carry-over from the upstream facili- the regeneration process studied. sure; keq is the equivalent thermal
ties. It is then routed to the To solve these set of equations, conductivity (a scalar or a tensor if
molecular sieve dryers. A dehydra- commercial software (Comsol the thermal conductivity is aniso-
tion package consists of four dryers Multiphysics Ver. 4.2) was tropic); Q is the heat source (or
loaded with a special type of employed that utilises the finite sink); c is the concentration of the
molecular sieve 4A; at any time element method to discretise partial species (mol/m3); D is the diffusion
three dryers are in adsorption and differential equations to ordinary coefficient (m2/s), and R is the reac-
one in regeneration. The feed differential equations and finally tion rate expression for the species
stream is split into three identical solve them. The following assump- (mol/m3·s). Furthermore, the major
streams, each of which passes tions are considered during the particular equations are the
downward through one of the beds mathematical procedure: Langmuir adsorption isotherm and
that are in adsorption mode (see • To reduce computation time, 2D ideal gas law. The proposed equa-
Figure 2). axisymmetric mode is assumed tions in 2D axisymmetric mode
Dry gas streams leaving the • The gaseous phase is an ideal gas have been solved using the
adsorption beds are joined and • Entrance and exit effects are required initial and boundary
passed through a filter to retain any negligible conditions.
solid particles coming from the • There is no slip condition near
dryers. Finally, dry and filtered gas the dryer wall. Feed and regeneration gas
is sent to the municipal gas station compositions
via a transmission pipeline. Governing equations
Each adsorption cycle takes eight Mathematical modelling of the Components Adsorption Regeneration
Methane, wt% 72.95 73.1
hours. After that, the dryer is target regeneration process is Ethane, wt% 8.13 8.14
switched to regeneration mode for obtained by coupling a set of Propane, wt% 4.1 4.11
removing the residual water. At general equations (including conti- i-Butane, wt% 1.22 1.22
once, that bed which has completed nuity, momentum, energy and n-Butane, wt% 1.56 1.56
i-Pentane, wt% 0.00 0.00
mass balances), and particular n-Pentane, wt% 0.140 0.141
Adsorption and regeneration equations such as physical proper- n-Hexane, wt% 1.73 1.73
operating conditions ties, adsorption and desorption n-Heptane, wt% 0.1897 0.19
isotherms and equation of state as n-Octane, wt% 0.1622 0.1625
n-Nonane, wt% 0.0337 0.0338
Specifications Value follows: CO2, wt% 3.79 3.8
Adsorption temperature, °C 47
Adsorption pressure, kPa 9101 Nitrogen, wt% 4.57 4.58
Adsorption mass flow, kg/h 2.409e+05 Continuity equation: H2O, wt% 0.1573 0.000
Regeneration temperature, °C 270 ∂ρ
+ ∇ ⋅ ( ρu ) = Qbr
Regeneration pressure, kPa 7929 ∂t Table 2
Regeneration mass flow, kg/h 4.751e+04
Momentum equation:
ρ ∂u u µ 2µ µ
( + (u ⋅ ∇) ) = ∇ ⋅ [− PI + (∇u + (∇u )T ) − (∇ ⋅ u ) I ] − ( + β f u + Qbr )u + F
Table 1 ε p ∂t εp εp 3ε p kbr

76 PTQ Q4 2014 www.eptq.com

ripi.indd 2 10/09/2014 13:49

 Sulzer Chemtech

Tower Technical Bulletin

Design and Installation of Cartridge Trays

Introduction The mechanical design of the cartridge trays should also be

Cartridge trays, also known as package trays, are generally stronger than segmented trays since as they will be transported
used for tower diameters in the range from 12” (300mm) up to in assembled condition. The tray thickness should be increased
36” (900mm). For tower diameters below 36”, the installation of (e.g 12ga or 2.5mm when referring to stainless steel) to maintain
segmental trays is difficult and packing is often preferable over rigidity and ensure a tight fit. Stronger tie-rods and Schedule 80
trays. Ultimately, the decision on what technology to use comes spacer pipes should be specified as well. Since the gaskets are
down to process requirements and economics. more prone to distortion, it is preferable to install them after the
trays arrive on site. The selection of gasket material should be
As can be seen below, the design and construction of cartridge based on temperature and service. Metal gaskets of a suitable
trays is unique and a bit complex. Cartridge trays typically material are often preferred for their mechanical durability.
consist of one or more bundles of 6 to 10 trays stacked together
and connected with several tie rods running through the bundle.
This can be a challenge; the trays must be assembled with
near perfect alignment to ensure trouble-free installation. The
resistance of the tray seal rings increases the force required
to install and remove the tray bundles so proper design and
correct dimensions are critical. Alternatively, Sulzer also offers
Slit TraysTM for smaller column diameters. These trays are
installed individually to help minimize installation issues.

Cartridge Tray Cross-Sectional Layout

Important Tips
During installation, the orientation of the trays with respect to
nozzles should be fixed prior to the bundle insertion as it will
be more difficult to rotate afterwards. Also, access around the
outside of the column must be properly allocated during the
design process to ensure that there is no external interference
with the bundle during insertion or removal.

Standard pipe sizes are typically used for columns with

cartridge trays. Care must be taken during construction not
Bundles of Cartridge Trays
to compromise the diameter and roundness of the column
to ensure that the tray bundles will pass through the without
Design Considerations interference.
The unique aspects of cartridge tray designs are both mechanical
and process related. The trays must have a perimeter deck seal
that maintains its integrity while the bundle is installed. The The Sulzer Applications Group
downcomers, which cannot seal to the column wall, must use Sulzer has over 150 years of in-house operating
an envelope design which results in some wasted area behind and design experience in process applications. We
the downcomer (shown on the sketch to the right). In order to understand your process and your economic drivers.
properly rate these trays hydraulically, the wasted area must be Sulzer has the know-how and the technology to design
accounted for to ensure that it is not inadvertently counted as
internals with reliable, high performance.
active area, AA.

The trays must be fixed together in a bundle form along with a

Sulzer Chemtech, USA, Inc.
mechanism to support the bundle within the column. The trays
8505 E. North Belt Drive | Humble, TX 77396
should be partitioned to maintain a maximum bundle length of
13ft (4m) for ease of handling. Phone: (281) 604-4100 | Fax: (281) 540-2777
[email protected]
www.sulzer.com

Legal Notice: The information contained in this publication is believed to be accurate and reliable, but is not to be construed as implying any warranty or guarantee of performance.
Sulzer Chemtech waives any liability and indemnity for effects resulting from its application.

sulzer.indd 1 10/09/2014 12:04

 preventing operational malfunctions.
As Figure 3 shows, for our case
6500 Temperature, K study liquid water moved down-
6000 543.15
ward until it encountered the
5500
heating zone. At this point, boiling
5000
4500 500 water created a reflux which ground
4000
Regeneration reflux the molecular sieve into a powder.
zone
3500 Since certain components of the
450
3000 binder were somewhat soluble in
2500 boiling water, the molecular sieve
2000 400 subsequently became a wet cake
1500
Desorption
(mud) which was then baked by the
1000 zone 350 rising hot gas. These soluble compo-
500 Starts at 120ºC-140ºC nents could ion exchange with the
0 320.14 zeolite and/or combine with anions
−4000 −3000 −2000 −1000 0 1000 2000 in water to form solid salts (Na2CO3,
CaCO3, MgCO3, NaNO3, and so on).
Figure 3 Temperature distribution during the regeneration process These solid salts could then paste
the remaining pellets or beads
Results and discussions with enough strength against reflux together to form a solid mass. This
Figure 3 shows the temperature which could work more than four
distribution of the adsorption bed years without any malfunction. But
at an early stage in the regeneration for the next loading, a regular molec-
A high regeneration
process. As is apparent in this ular sieve, manufactured by another gas temperature
figure, a high regeneration gas company, could not withstand those
temperature (without enough conditions. It was observed that, (without enough
ramp-up) leads to a large tempera- only three months from the start of
ture gradient along the bed, and run, the loaded molecular sieve was ramp-up) leads to a
creates reflux at the early stages of ruined due to the reflux phenome-
the regeneration cycle. non. It also increased the pressure large temperature
At these operating conditions, due drop of the dryers. Therefore, it can
to the high pressure of the regenera- be concluded that the molecular
gradient along the bed
tion gas, high moisture concentration sieve, especially the binder and addi-
and a large temperature gradient are tives, should be made of appropriate solid mass, formed in an annulus
inevitable. For the design case, the raw materials to be capable of resist- shape with a centre opening of less
licensor charged a molecular sieve ing the reflux phenomenon and than one foot, did not allow gas to
pass through, and consequently
Recommendations and consequences to prevent reflux phenomena reduced the effective diameter of the
bed (see Figure 1).
Therefore, boiling water destroyed
Recommendation Consequence
1 Decreasing the regeneration gas pressure • Needs compressor
the molecular sieve such that the
• Higher operating cost severity of the operating conditions
2 Regeneration gas temperature ramp-up • Hot oil system modification (if applicable) should be greatly reduced to extend
• Higher regeneration cycle time the replacement period of the adsor-
• Adsorption cycle time limitation
3 Layer of activated alumina at the top of the bed • This approach may minimise the rolling boil
bent. The regeneration reflux
but cannot fix the problem. Based on Figure 3, showed some undesirable effects on
the reflux happens through the bed because of the adsorption process which can be
a high temperature gradient, so it can only summarised as follows:
reduce the reflux. We can consider it
a modification.
• Molecular sieve particle break-up
4 Change the heating gas flow direction from the • This is costly. Co-current regeneration • Increasing pressure drop
top to the bottom of the bed requires more gas for stripping the • Gas channelling
bed completely. • Premature water breakthrough
• The downward flow pushes heavy liquid
contaminants, and possibly increases fouling
which all lead to poor adsorber
rate. performance.
5 Try to reduce the heat loss through the top of • This can only reduce temperature gradient As a consequence, these effects
the bed by adding extra insulation and even between the top and bottom of the vessel. increased the reflux phenomenon
installing a steam tracer
6 Reverse all flows • Bed fluidisation (lifting)
with the following malfunctions:
7 Using a special molecular sieve • The bed can possibly operate without any • High pressure regeneration gas
problem. • High moisture concentrations
• Large temperature gradients
Table 3 • High degree of solubility of

78 PTQ Q4 2014 www.eptq.com

ripi.indd 3 10/09/2014 13:49

 dust
water obtained
gas shift. after the second
As noted, hydrogen and material. Tungsten and molybde- Conclusion
binder
third
is held materials
filtration
constant. in water
stages is sold to the num are Company,
Nitel Pars present
60 a insubsidiary
the purified of Fateh The development
molecular sieve and howof a recycling
to prevent it, paper
• Choosing
paperIf theindustry,
entire an mixture
inappropriate
so the is at process flow
equilib-
Group, for technical assistance and 250
financial
solution which is mixed with process for NiW spent catalysts by ppm CO
presented at the 1000
Gas ppm CO
Processors Association
often need in
direction adjustment
adsorption to work and well support. 50precipitate calcium500responses ppm
Europe,COFebthat 2003,a2000 high-fidelity
Paris. ppm CO model
delivers
rium, thenzero COS waste.
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same reagents
Green-fieldtoprojects share many of the Eurecat, L’Electrolyse and Valdi
with even
regeneration. the most accurate simu- with
5 T Wa J non-complementary
Crittenden B, Adsorption Technology control &
and ifitsformodels.
aslation filtration
COS hydrolysissystem are or sour the tungstate
same or a mixture
characteristics as OTS of calcium was subsidised by the European
projects
Failure to allow for layer
Design,imported
Heinemannfrom the operating

COS wet, ppm

Further reading 40 Publication, 1998.
subject
shift. of patents.outlet mixtures are
However, molybdate
1 built
and tungstate.
for existing plants, but they The
fortend
yield Union and was awarded ‘Best of
controller
Recommendations tuning on
and the simulator Agarwal A, Advanced Strategies Optimal plant.
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Convection in Porous control Media,
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system because of to
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of tungsten
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3rd Best’
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but be tolerant of the
2006. in 2009.
consequences 30
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The hydrometallurgy
velocity (limited
overall project’s success. process
catalyst inven- moreand more
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Ph.D. This ismetallic
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implications morealloy
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solidification, J. of
Prognostications beneficial.
phenomena
treated
high by which are
hydrometallurgy
conversion reviewed
because in three in
inlet companies
operating plant looking for tungsten
and assumptions and of spent
Fluid NiWcontinue
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550, New
2006, 149-173. invest-
High-fidelity process simulation OTSs will to become
brief
steps: for
concentrations
models
the target
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is
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accurate, toif To date, the
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more readily tungsten
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andengineering
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carbide and cemented
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judged 240 Kluwer
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by or260opments 280 Academic
enabled alone.300 Publisher,
the Thecompany
320 1990. to reach
more 340 detailed
in
on Table
offer
COS 3, a special molecular sieve
theequilibrium
composition
a lot of value, ofparticularly
value the thancatalysts
would for Erasteel which produces steel and
less stringent criteria. The project team Sajad Mirian is a Project Manager in the
3000simulation,
the
Temperature, tonnes ºC capacity. the more With dataits and
pyro-
4A
and (with
their
OTSs.
the high pathway.
contaminants
However,
hydrolysis resistance (which
not everything against
As are
can
the
has shown a good
tungsten
generallyalloys.
recognises Thethat hydrometallur-
value is more Adsorbents Department of Nitel Pars Co.,
metallurgical and
understanding that hydrometallurgi-
it holds, and,
reflux phenomena), manufactured closely linkedequilibrium
to is
the delivery date Tehran, Iran. He holds a MSc in chemical
mainly phosphorus
be modelled and
says,perfectly. arsenic).
CO, In
Modelling gical process protected gasby cal O,process,
shifta1%consequently, the company
[email protected].
more engineering is able to
expression
by
agoes Shanghai
step using
toolsCOS.”and FigureHengye
“as
decantation
principles6 shows
goes
Chemical
andCOS
can Co.,
filtra-
still
so
be
for
performance and no
Figure
patent.
6 COS
(to maximise training time) than it is
– sour H 2
recycle
effort
2% H2 Email:
engineering.
aAnisi
large
required. range
AsAdsorbent
with of spent
any mate-
engi-
Hossein is an Expert in the
was aloaded into the target dryers to accuracy. Indeed, theisincremental
improved.
tion,
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about
further
alumina
solid
one and
There
concentrate
concentrations
year
development
is still
ago. To
silica, to
along
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Michael
The benefit
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consultant to industry
a process expert neering
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rials,
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NiCoMo
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Department
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the time NiW,
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isNitel
against
catalysts.
effort
theParsNiMo,
Business
Co. He
the
holds a BSc in Manager
chemical –engineering.
Gas Treating Catalysts
dehydration unit has shown a good
granularity
oxides
Part two of nickel, is produced. Thisas
performance
of
and
models (such observed
training
and is
treating, small
refining —
The leaching residues are melted much can
operation, be
CO 2
capture,
at value.
for The
Criterion best
Email: [email protected] OTS
Catalysts will and not be the
Technologies,
part no malfunction
smaller achieved with relatively simple, stable
material
The second is volumes,
reserved of smaller
for the pyro-
this time-
article
and related research.
a high temperature in a submerged His activities regarding best
Xiang choice
located Yuin is anfor
Houston. everyone.
He
Application has global
Engineer responsibility
of Hengye
has been
steps, observed.
more detailed unit operation and robust
sulphur forrecoverymodels. amine treating, Jean-Pierre
include adsorption-based Co.,Dufour
for Criterion’s is China.
gas treating the catalyst
Technical aand
business.
metallurgical
develops reactor process. modelling with electrode
model arc furnace.
multi-component Nickel alloys Chemical Shanghai, He holds BSc
models), although there are slurry
dimin- Claus, tail gas treating, and tail gas treating Industrial
Prior to Director
joining of Valdi. He
Criterion holds a PhD
Catalysts in&
aThe soluble
kinetic fraction
reaction ofmodel,
the the are obtained from this operation;
separations: application to pressure swing in chemical engineering.
ishing
Acknowledgmentreturns. catalyst
adsorption, development,
Chemical design and
Engineering Science, operation. metallurgy
Technologies and
54, Email: [email protected] inhas worked
2001, he for
held 20 years
positions in the
as a
iseffects
purified of to remove phosphorus
temperature and space they
He
are from
retired
sold to Oil
Shell
steelmakers
in 2005 with
while
36 years Martin
process Sneesby
metallurgicaldesign is an independent
industries.
engineer, unit contact dynamic
engineer,
The
We would increase
like to express inourfidelity of DCS
great appreciation system
1999,
the is complementary
5647-5666.
silico-aluminate to a plant simulation consultant with more than 20
Sepehr Sadighi is Assistant Professor with
and
to
arsenic.
velocity,
Mr F Noorbakhsh
These
catalyst
and
contaminants
Mr M A activation,
Fatemi for 3of
or experience.
simulation. HeAdsorption
holds A a slag
bachelor produced
of science
–low-fidelity Sophie anComte
and Catalysis
operationsisResearch
the superintendent
Laboratory Manager with
ofinResearch
two US
are emulation
not recycledthat is achieved
and and by
are disposed using Dabrowski
isdegree
usedin in
A,
roadworks,
from
while
theory years
the
dust Valdi. ofCoast
experience inwith Division
process simulation and
catalyst
their deactivation,
valuable and constructive determin-
suggestions chemical engineering from Georgia Gulf She started
refineries. He the company
holds a seven
bachelor of
‘real’ hardware and control config- process
to practice,model
Advances with a complemen-
in Colloid Institute of
and Interface modelling, Petroleum
including many Industry
operator (RIPI), Tehran,
training
ofingas TGU
during hazardous catalyst
the planning waste;
and health they from
development repre-
of thisa produced
Institute of from
Technology the melting
and is a stage is
registered years ago
science as
degreeR&D inproject manager
chemical and
engineering holds
froma
urations is laudable, but it should tary (well
Science, 93, 2001,tuned) 135-224.control layer simulators Iran. He holds a PhD inengineering
and detailed chemical engineering.
studies.
sent
researchlesswork.
commercial thanWe 1%
unit
would ofalso the likestarting
temperature
to thank recycled.
4professional Bengineer
Meyer P provide in Texas. damaging of PhD
Chr, Hydrothermal in A&M
Texas
Email: environmental
Sadighis @ripi.irchemistry.
University.
be remembered that a control might better overall Email: [email protected]
profile example. Email: [email protected] Email: [email protected]

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criterion.indd 12/03/2014
09/06/2014 12:07
12:54
ripi.indd 4 10/09/2014 13:49