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MOLECULAR SIEVE DEHYDRATION PROCESS

TRAINING FOR PROFESSIONAL PERFORMANCE

This manual is one of a series for your In order for you to learn the contents of
use in learning more about equipment that the manual, you must dig out the pertinent
you work with in the petroleum industry. Its facts and relate them to the subject. Simply
purpose is to assist in developing your knowl- reading the material and answering the ques-
edge and skills to the point that you can per- tions is not enough. The more effort you make
form your work in a more professional man- to learn the material, the more you will learn
ner. from the manual.

The manual was prepared so that you Teaching yourself requires self-disci-
can learn its contents on your own time, with- pline and hard work. In order to prepare your-
out the assistance of an instructor or class- self for the sacrifice you will have to make,
room discussion. Educators refer to learning you should set goals for yourself. Your ultimate
by self-study as Programmed Learning. It goal is to perform your work in a more profes-
is a method widely used in all industries as a sional manner. Training is one step in reach-
means of training employees to do their job ing that goal. Application of what you learn is
properly and teach them how to perform another. Seeking answers to questions is a
higher rated jobs. third.

You can demonstrate your desire to be a Once you have established your final
professional by taking a positive attitude to- goal, you must determine the means for
ward learning the contents of this manual and reaching that goal. You may decide, for ex-
others that are applicable to your job. ample, that you must complete a series of 10
to 15 manuals to get the basic knowledge and
The author of this manual has years of skills you need. After you decide which train-
experience in operating petroleum equipment. ing material is required, you should set a time
He also has the technical knowledge of how table for completing each section of the ma-
and why petroleum equipment functions. The terial.
text was written for use by personnel with little
or no previous experience with petroleum Achieving your final goal may take more
equipment. Consequently, some of the mate- than a year, and will require hours of hard work
rial may be familiar to you if you have experi- on your part. You will know you have achieved
ence with oilfield equipment. From such ex- your goal when you understand how and why
perience, you have observed the effect of to operate oilfield equipment in order to ob-
making operating changes. The manual will tain the maximum product at the lowest cost.
help explain why the changes occurred that Your sacrifice will have been worth-while from
you observed. It will also teach you how and the satisfaction of knowing that you can per-
why equipment functions. form your job in a methodical professional
manner, instead of a trial-and-error approach.

© 2003 Petroleum Learning Programs Ltd. No part of this manual may be reproduced in any form. Its use as a
reference in training courses is specifically reserved for Petroleum Learning Programs Ltd. All translation rights are
likewise reserved.

MOLECULAR SIEVE DEHYDRATION PROCESS


INSTRUCTIONS FOR USING THIS MANUAL

This your manual. You should write your 1. Turn to Page 1. Read the material until
name on the cover. Upon completion you will you come to the first problem or ques-
find it helpful to keep it in an accessible place tion.
for future reference. 2. Work the first problem or answer the
question and enter the answer in the
Problems are included throughout the text. proper space in ink. If the problem or
The solutions to the problems are given at the question is shown in both SI and En-
end of the book. glish Units of measurement, answer
only the part in units of measurement
The manual is used in training programs that you use.
all over the world. In some countries, English 3. Compare your answer with that shown
units of measurement such as feet, gallons, at the end of the book; be sure to use
pounds, etc, are used. In other countries, solutions to the problems in the units
Systems Internationale (SI) or Metric units, you are working in.
such as meters, liters, kilograms, etc., are If your answer is correct, continue read-
used. In order for the manual to be of maxi- ing until you come to the next problem
mum use, both SI and English units are shown. and work it. If not, restudy the manual
until you understand the reason for
The SI unit always appears first, and the your error. Rework the problem if
English unit follows in brackets [ ]. Example: necesary. Leave your wrong answer
the temperature is 25°C [77°F]. The English and note the correct one. This will keep
equivalent of the SI unit will be rounded off to you from making the same mistake
the nearest whole number to simplify the text later on.
and examples. A distance of 10 m may be 4. Proceed stepwise as shown above
shown as 33 ft whereas the exact equivalent until you have completed the text.
is 32.81 ft.
The above approach will require thought,
If you are working in English units, you making mistakes, and rethinking the situ-
may find it helpful to mark out the parts that ation. Concenrate on two things — the how
are in SI units and vice versa. and why. Do not cheat yourself by taking
short-cuts or looking up the answers in ad-
Some of the Figures have units of meas- vance. It saves time and errors but produces
urement. In such cases, two figures are in- no real understanding. Your future depends
cluded. The first one is in SI units, and the on how efficiently you perform your job and
second-figure will be on the next page and will not on how rapidly you proceed through this
have English units. Each figure is identified manual. Since this is your manual, any errors
with SI or English units. Be sure you use the you make are private.
figures in the units you are working in.
A validation or test covering the entire
The following procedure is recommended manual is included at the back of the book.
for using this manual: Answers will be sent to your supervisor or
training director at their request at no cost.

MOLECULAR SIEVE DEHYDRATION PROCESS


ABBREVIATIONS USED UNITS OF MEASUREMENT
IN THIS MANUAL
SI UNITS OF MEASUREMENT
SI UNIT ABBREVIATIONS
Most of the SI units of measurement used in the
oilfield are traditional metric units. The exceptions we
s, min second, minute, time
are concerned with are pressure and heat units. The
h, d hours, day time
SI pressure unit is kilopascal; the heat units are joule
mm millimeter length and watt. A watt equals 1 joule per second. Coversions
cm centimeter length from traditional metric units to SI units are as follows:
m meter length
m2 square meter area METRIC SI
CONVERSION
m3 cubic meter volume UNIT UNIT
m3/d cubic meters per day volume rate Pressure bar kilopascal, kPa kPa = bar x 100
l liter volume joule, J or J = cal x 4.2
Heat calorie
g, kg gram, kilogram weight watt, W W = J ÷ time, sec.
Pa, kPa pascal, kilopascal pressure
kPa(a) kilopascal absolute pressure
MPa megapascal pressure
bar bar (1 bar = 100 kPa) pressure
STANDARD CONDITIONS
J, kJ joule, kilojoule heat, work FOR GAS
MJ megajoule (J x 106) heat, work
W,kW watt, kilowatt power Measurement units for gas volume are cubic meters
per day (m3) or thousands of cubic feet per day (Mcf/
ENGLISH UNIT ABBREVIATIONS d). The letters st or s are sometimes used with the
units to designate volume at standard temperature
s, min second, minute time and pressure: m3d (st) or Mscf/d. In this manual,
h, d hour, day time standard volumes are corrected to a temperature of
in, ft inch, foot length 15°C and a pressure of 101.325 kPa(a), or 60°F and
sq in square inch area 14.7 psia.
sq ft square foot area
cu ft cubic foot volume To simplify the text, the letters st and s are omitted.
gal gallon volume However, all gas volumes shown are at standard
bbl barrel (42 US gal) volume conditions unless specifically stated otherwise.
BPD barrels per day volume rate
lb pound weight
psi lbs per square inch pressure
psia lbs per sq in absolute pressure HEAT CAPACITY AND
Btu British thermal unit heat RELATIVE DENSITY
MBtu thousand Btu heat
MMBtu million Btu heat
Specific heat and specific gravity are traditional
W, kW watt, kilowatt electric power terms that have been used in both Metric and English
hp horsepower mechanical power units for many years. These names are being re-
cf/d cubic feet per day gas flow rate placed with the terms: heat capacity and relative
Mcf/d thousand cf/d gas flow rate density. The new names are used in this manual.
MMcf/d million cf/d gas flow rate When you see the term heat capacity (Ht Cap), it will
M thousand have the same meaning as specific heat, and relative
MM million density (Rel Dens) means specific gravity.

MOLECULAR SIEVE DEHYDRATION PROCESS


MOLECULAR SIEVE DEHYDRATION
TABLE OF CONTENTS
INTRODUCTION ..............................................................................................................1
DEFINITIONS .................................................................................................................3
I. EQUIPMENT IN AN ADSORPTION PLANT ............................................................5
A. Inlet Separator ....................................................................................................5
B. Adsorber Tower ...................................................................................................6
C. Outlet Filter .........................................................................................................7
D. Regeneration Gas Heater ...................................................................................8
E. Regeneration Gas Cooler ...................................................................................9
F. Regeneration Gas Separator ..............................................................................9
G. Regeneration Gas Blower .................................................................................10
H. Regeneration Liquid Pump ...............................................................................10
II. APPLICATION OF ADSORPTION PLANTS ..........................................................11
A. Flow Dehydration ..............................................................................................11
B. Simultaneous Dehydration and Sweetening .....................................................12
III. PROCESS FLOW ..................................................................................................13
A. Flow in 2-Tower Plant .......................................................................................13
B. Flow in 3-Tower Plant .......................................................................................15
1. Flow in 3-Tower Plant with Regeneration Gas Blower .................................16
C. Flow in 4-Tower Plant .......................................................................................17
D. Flow When Pressure of Regen Gas is Different from Main Gas .......................19
E. Tower Switching Sequence ...............................................................................19
F. Switching Valve Operation ................................................................................21
IV. REGENERATION OF ADSORBENT .....................................................................23
A. Principles of Regeneration ...............................................................................23
B. Heat Transfer During Regeneration ..................................................................30
C. Optimizing Regeneration ..................................................................................31
D. Cooling Phase of Regeneration ........................................................................35
E. Source of Regeneration Gas ............................................................................36
F. Flow Direction of Regeneration Gas .................................................................37
G. Regeneration Gas Flow Control .......................................................................38
H. Regeneration Gas Channeling .........................................................................39
V. OPERATION ..........................................................................................................40
A. Start-Up After Adsorbent Replacement ............................................................40
B. Routine Operation.............................................................................................41
C. Shut Down ........................................................................................................44
D. Breakpoint Test Procedure................................................................................46
VI. CONTROL OF ADSORPTION PLANT ..................................................................48
VII. TROUBLESHOOTING ...........................................................................................52
A. Loss of Capacity ...............................................................................................54
B. Loss of Efficiency ..............................................................................................58
Troubleshooting Chart ............................................................................................61
VALIDATION, SI UNITS .................................................................................................63
SOLUTIONS TO PROBLEMS - SI UNITS .....................................................................64
VALIDATION, ENGLISH UNITS .....................................................................................65
SOLUTIONS TO PROBLEMS - ENGLISH UNITS .........................................................66

MOLECULAR SIEVE DEHYDRATION PROCESS


LIST OF DRAWINGS, EXAMPLES, AND GRAPHS

Photographs of Adsorption Plants.....................................................................1, 5, 11,12


Breakpoint Curve .............................................................................................................3
Inlet Separator ..................................................................................................................6
Adsorber Tower ................................................................................................................6
Outlet Filter .......................................................................................................................7
Regeneration Gas Heater ................................................................................................8
Regeneration Gas Cooler ................................................................................................9
Regeneration Gas Blower ................................................................................................9
Flow Diagram of 2-Tower Plant ..........................................................................14, 23, 38
Flow Diagram of 3-Tower Plant ................................................................................15, 16
Flow Diagram of 4-Tower Plant ......................................................................................17
Flow Diagram of 3-Tower Plant with Regeneration Gas Blower .....................................18
Tower Switching Sequences ....................................................................................19, 20
Switching Valve Operation..............................................................................................21
Temperatures in Adsorber During Regeneration - SI Units ............................................26
Temperatures in Adsorber During Regeneration - English Units ...................................27
Regeneration Gas Temperature Recording Charts ............................................29, 33, 34
Breakpoint Test Procedure .............................................................................................47
Breakpoint Curves Showing Loss of Capacity & Efficiency ...........................................53
Temperature Traces of Regeneration Gas Leaving Tower when Heating
Time is not long enough or Regeneration Flow is Low ..............................................58
Temperature Traces of Regeneration Gas Leaving Tower when
Channeling Occurs.....................................................................................................59
Temperature Traces of Regeneration Gas Leaving Tower when
Temperature of Heating Gas is not High Enough .......................................................59

MOLECULAR SIEVE DEHYDRATION PROCESS


MOLECULAR SIEVE DEHYDRATION PLANTS 1
INTRODUCTION
Almost all gas which flows from a gas these processes are described in the
well or is produced from an oil well, con- manuals for Glycol Dehydration, Amine
tains moisture and other impurities which Sweetening and Lean Oil absorbers. This
must be removed from the gas before it manual covers the process for removing
can be used as fuel in homes or industry. water vapor and other contaminants from
In addition, refinery and gasoline gas plant a gas or liquid stream. It is different than
liquid products, such as LPG, often con- the other processes in that it can perform
tain moisture and sulfur compounds which more than one purification step in a single
must be removed before the products can process. For example, molecular sieves
be sold. may be used to remove both water and H2S
There are several ways to perform from gas in one operation.
each of these purification steps. Some of

4-TOWER DEHYDRATION

MOLECULAR SIEVE DEHYDRATION PROCESS


2 INTRODUCTION

Even when only one type of purifica- equipment in an adsorption plant. There are
tion is needed, the solid bed system is of- also different adsorbents that can be used.
ten used because it does the job more The number of adsorbers can vary from two
completely than other processes. For ex- to more than a dozen. The stream used for
ample, a solid bed dehydrator is normally regeneration, and the disposal of this
used to dry gas entering a cryogenic gas stream, can vary from plant to plant. The
plant. The adsorption process is used direction of both the process stream and
rather than a glycol dehydrator because the the regeneration stream, as they go through
solid bed process dries the gas to a much the bed, may be either up or down. When
lower water content than the glycol pro- all of these possible variables are com-
cess. This is important when the cryogenic bined, the differences in plants can be al-
plant must be protected from freeze-ups most endless.
at very low temperatures. We will cover the most frequently used
The adsorption process is a batch type combinations and arrangements of adsorp-
operation. The process fluid flows through tion and regeneration in plants using mo-
a bed of adsorbent until the adsorbent is lecular sieves. We will also learn why the
loaded or saturated with material removed flow varies from one plant to another. If
from the fluid. At this point, the process fluid you’re familiar with a plant that is different
is diverted to a bed of fresh adsorbent, and than any described in the manual, you
the saturated bed is regenerated. Regen- should be able to figure out what specific
eration is accomplished by boiling out the requirements led to the arrangement of that
adsorbed material from the saturated bed particular plant. This manual is primarily
by passing a stream of hot gas through it. concerned with the entire adsorption plant.
Since the system is a batch type, it Manual P-6 MOLECULAR SIEVE
must have 2 or more towers containing ADSORBERS, covers the details of
adsorbent. One or more towers are adsorber towers, and adsorbent capacity
adsorbing, and one or more towers are re- and efficiency. We will frequently refer to it,
generating. so you should have a copy of it as you study
There are several ways to arrange the this manual.

MOLECULAR SIEVE DEHYDRATION PROCESS


DEFINITIONS 3

Adsorbent - Solid material that re- dries gas to a dew point of -50°C [-58°F]
moves water vapor or other components with new adsorbent, it will produce the
from gas or other process fluid. It is usu- same dew point months or years later at
ally in a pellet or bead. In this manual the the same operating conditions.
adsorbent is molecular sieve. Breakpoint - The number of hours an
Adsorbent Capacity - Weight of wa- adsorbent can remain in adsorbing service
ter vapor or other material the mole sieve and produce an outlet process fluid that
removes from the process inlet stream, meets quality specifications. Example: gas
expressed as weight % of adsorbent. Ex- leaving an adsorber tower has a moisture
ample: 100 kg [100 lb] of adsorbent hav- content below the specified limit for 8.5
ing a moisture capacity of 12 weight % will hours at design gas flow rate. At the end of
remove 12 kg [12 lb] of moisture from gas. 8.5 hours, the moisture content of the out-
An adsorbent loses capacity with age. New let gas rises rapidly. The breakpoint is 8.5
adsorbent has about twice the capacity of hours.
that which has been in service for several Desiccant - Adsorbent used to re-
years. move moisture from process fluid.
Adsorbent Efficiency - The measure Process Fluid - Gas or liquid stream
of an adsorbent’s ability to remove 100% containing contaminants which are re-
of moisture or other components from a moved as the stream flows through the ad-
process fluid. The efficiency is indicated by sorption plant.
the quantity of compo-
100
nent that remains in the
outlet process fluid after
treating. Example: an
% MOISTURE IN
TREATED GAS

adsorbent which dehy-


drates gas to a dew
50
point of -75°C [-103°F],
has a higher efficiency BREAKPOINT
than one which pro-
duces a dew point of the
same gas of -50°C [-
0
58°F]. Efficiency does 0 4 8 12
not change with age. In
HOURS IN ADSORPTION SERVICE
other words, if a plant
BREAKPOINT CURVE

MOLECULAR SIEVE DEHYDRATION PROCESS


4 DEFINITIONS

Dew Point - The temperature to which will depend upon the gas pressure. This is
gas must be cooled before moisture will discussed in detail in Manual P-6. The dew
start to condense from it. Gas contains point of gas leaving a dehydration plant is
moisture just as air has humidity. When gas often the quality control measurement for
or air are cooled to the point at which the evaluating the performance of the plant. As
gas is saturated with moisture, or the rela- long as the outlet gas dew point is below
tive humidity is 100%, additional cooling will the specified temperature, the moisture
result in water formation. The water con- content of the outlet gas is below the speci-
tent of the gas at its dew point temperature fied limit.

Problem 1

Match the items in the column on the left with those on the right.

______ 1. Adsorbent capacity a. Gas stream flowing through adsorption


plant.

______ 2. Adsorbent efficiency b. Temperature that moisture will condense


from gas.

______ 3. Breakpoint c. Outlet gas dew point.

______ 4. Desiccant d. Wt % of adsorbent that represents the


quantity of water vapor it will remove from
gas.

______ 5. Dew Point e. Adsorbent that removes moisture from fluid.

______ 6. Process Fluid f. Hours process gas can flow through adsor-
bent tower before outlet gas moisture con-
tent rises above specification.

MOLECULAR SIEVE DEHYDRATION PROCESS


I. EQUIPMENT IN AN ADSORPTION PLANT 5

The 2-tower adsorption plant shown adsorbent with hydrocarbon liquid, or


below has most of the equipment that is breakage of the adsorbent if water is
common to almost all adsorption plants. present. It must also remove particles of
Some plants may have 3 or more adsorber scale, dirt, etc., from the gas to prevent
towers, others may have energy-saving plugging the adsorbent.
heat exchangers and compressors. Re- The type of separator will depend upon
gardless of the number of adsorber tow- the source of the stream being processed.
ers, the main items of equipment are the If the gas is flowing from a multi-well gath-
same, and are discussed below. ering system or from an offshore produc-
A. Inlet Separator tion platform, the separator must be large
enough to catch slugs of liquid which may
The inlet separator in a treating plant enter with the gas. In addition, the separa-
is of vital importance. It must remove liq- tor should include some media to remove
uid from the gas to prevent coating of the solid particles which may be present in the

ADSORBER
TOWERS

REGENERATION
GAS SEPARATOR
REGENERATION
INLET GAS GAS COOLER
SEPARATOR
REGENERATION
GAS HEATER

EQUIPMENT IN ADSORPTION PLANT

MOLECULAR SIEVE DEHYDRATION PROCESS


6 ADSORBER TOWER

gas. Filters or a wire mesh must extractor B. Adsorber Tower


will adequately remove solid material from The adsorber tower contains molecu-
the gas stream. lar sieves which removes material from the
Regardless of the source of the gas, process fluid. The tower usually has a bed
the separator must remove essentially all support system to hold the adsorbent in the
of the liquid and solid particles from the gas. tower. It is usually insulated, to prevent heat
The double barrel separator shown below loss during regeneration. Refer to Manual
is the preferred type. In this separator, liq- P-6 for a detailed description of Adsorbers.
uid falls to the bottom and collects in the
lower chamber, which is segregated from
the gas flowing through the upper cham-
ber. This segregation prevents the
gas from flowing across the surface FILL MANWAY
and possibly picking up some liq- RELIEF
INLET
uid and carrying it out the vessel. PROCESS VALVE
FLUID

DISTRIBUTION
PLATE

DUMP
MANWAY

OUTLET
PROCESS
FLUID
INLET GAS SEPARATOR ADSORBER TOWER

MOLECULAR SIEVE DEHYDRATION PROCESS


OUTLET FILTER 7

C. Outlet Filter top of the bed. Either of these occurrences


When adsorbents are heated they ex- will produce broken adsorbent particles,
pand, and when they are cooled they con- and dust.
tract or shrink. This means that during ev- Therefore, the outlet process stream
ery heating and cooling cycle of regenera- must have a filter to keep dust and broken
tion, each particle of adsorbent in a bed adsorbent pieces out of the system beyond
swells and shrinks. The total amount of their the adsorption plant. If it is going to a cryo-
change in size is so small it would be diffi- genic plant, a small amount of fine dust
cult to measure, but since there are mil- could foul expanders or heat exchangers
lions of particles in a bed the total change so the filter should be capable of removing
is enough to produce considerable pres- everything over one micron in size.
sure on the individual particles. The filter should be equipped with a dif-
They tend to move and rotate to estab- ferential pressure gauge. This accurately
lish a packing arrangement which will mini- measures the pressure drop across the fil-
mize this pressure. In so doing, they rub ter elements; as the filter gets coated with
against each other and against the vessel solid particles the pressure drop increases.
walls. This produces a small amount of very Each installation should have a base pres-
fine dust or powder. Also, even the best sure drop, for a given gas flow rate with
regulated plant may occasionally have a fresh filters. This figure, along with a maxi-
slight upset which may result in the bed mum pressure drop, and suitable flow rate
being “bumped” or in gas “jetting” into the corrections, should be posted so that op-
erators can keep track of the degree of
plugging in the filter.
When the maximum
pressure drop is
reached, the filter
should be bypassed
and the elements
changed. If this is not
done, the pressure drop
may become large
enough that one or
more of the elements
will rupture. If
OUTLET GAS FILTER

MOLECULAR SIEVE DEHYDRATION PROCESS


8 REGENERATION GAS COOLER

this happens, all of the dust and grit that tion gas can vary quite a bit, depending on
was trapped will suddenly be released into the source of this stream. Therefore, the
the system following the filter. heater must be capable of accommodat-
D. Regeneration Gas Heater ing these flow fluctuations while maintain-
ing the required temperature. The control
The purpose of this heater is to pro-
system should include a recorder for the
vide the hot gas necessary for regenera-
gas temperature as it leaves the heater.
tion of the beds. There are two types that
Quite often, the same recorder has a sec-
are frequently used. One is the so called
ond pen that indicates the temperature of
“direct fired heater” and the other is “indi-
regeneration gas as it flows out of the bed
rect fired.” Both types are described in other
being heated.
training manuals.
Some plants get heat for regeneration
Since regeneration of adsorbent is sen-
from a source other than a heater such as
sitive to temperature, it is important that
a waste heat recovery system in exhaust
the controls on the heater be adequate to
gas from turbines of engines.
control the regeneration gas temperature
within a few degrees of the desired setting
of 230 - 290°C [450 - 550°F].
In some plants the volume of regenera-

INDIRECT FIRED HEATER DIRECT FIRED HEATER

MOLECULAR SIEVE DEHYDRATION PROCESS


REGENERATION GAS COOLER & SEPARATOR 9

E. Regeneration Gas Cooler prevent it from adequately cooling the re-


The purpose of the cooler is to lower generation gas stream.
the temperature of the regeneration gas
F. Regeneration Gas Separator
so that water and sometimes hydrocarbons
will condense. It may be that the regen- The regeneration gas separator re-
eration gas enters a fuel system, which moves liquid from the stream of regenera-
requires cooling to avoid problems of con- tion gas flowing out of the cooler. The type
trol in the system. of separator used will depend upon the
The cooler may be an aerial type or it quantity and type of liquid contained in the
may be a water cooled exchanger, or some stream.
other form.
Regardless of the type of cooler, its
function is the same — to cool the regen-
eration gas to approximately ambient tem-
perature. The regeneration gas entering the
cooler has just left an adsorber tower. Con-
sequently, the gas may contain some par-
ticles of broken adsorbent. It will probably
be necessary to periodically shutdown the
cooler and remove the dust particles from
it. Otherwise, it may plug the cooler and

REGENERATION GAS BLOWER

HAIRPIN EXCHANGER AERIAL COOLER

MOLECULAR SIEVE DEHYDRATION PROCESS


10 REGENERATION GAS BLOWER

If the liquid is primarily water, a single the treated gas stream, or from the sales
liquid removal system is all that is required. gas from the plant that processes the out-
If, on the other hand, the liquid is a mixture let gas from the mole sieve dehydrator. As
of water and hydrocarbon, a level control the regeneration gas flows through the
system should be provided for each liquid. plant, it has a pressure loss of 175 - 210
Quite often, the separator is similar to kPa [25 - 30 psi]. A blower or compressor
the inlet gas separator described on page is often provided to make up this pressure.
6, except that it is smaller because the re- H. Regeneration Liquid Pump
generation gas flow is much less than inlet
gas. Dehydration plants treating liquid pro-
pane or LPG often use treated product for
G. Regeneration Gas Blower
regeneration. A pump is provided to make
Regeneration gas is withdrawn from up the pressure loss in the system.

Problem 2

Match items in the two columns.

______ 1. Inlet Gas Separator a. Raise temperature of heating gas.

______ 2. Outlet Gas Filter b. Make up pressure loss.

______ 3. Regeneration Gas Heater c. Removes contaminant from process


fluid.

______ 4. Regeneration Gas Separator d. Remove liquid and solids from pro-
cess inlet gas.

______ 5. Regeneration Gas Cooler e. Lower temperature of regeneration


gas.

______ 6. Regeneration Gas Compressor f. Remove adsorbent dust from pro-


cess outlet gas.

______ 7. Adsorber Tower g. Remove liquid from regeneration


gas.

MOLECULAR SIEVE DEHYDRATION PROCESS


II. APPLICATION OF MOLECULAR SIEVE 11
ADSORPTION PLANTS
A. Dehydration Gas entering a pipeline usually has a
The most common application of ad- maximum moisture specification of 96 - 112
sorption plants is that of dehydrating gas. kg/million m3 [6 - 7 lb/MMcf], which is
Another process for removing moisture equivalent to a dew point of -4° to 2°C [25°
from gas is that of glycol dehydration. Se- to 35°F] at typical pipeline operating pres-
lection of adsorption or glycol is based on sures. The glycol dehydration process is
the relative cost and efficiency the two pro- usually less expensive to install and oper-
cesses, which, in turn, depends upon the ate in this application, which requires only
quantity of moisture that must be removed 80 - 90% moisture removal from the gas.
from gas. The adsorption precess is more effi-
cient than glycol dehydration when the
application required 99 - 100% moisture
removal from gas. An example of this ap-
plication is that of gas entering a cryo-
genic plant, which required almost 100%
moisture removal from the gas to prevent
freeze-up.

2-TOWER AIR DEHYDRATION


PLANT 2-TOWER GAS DEHYDRATION PLANT

MOLECULAR SIEVE DEHYDRATION PROCESS


12 APPLICATION OF ADSORPTION PLANTS

B. Simultaneous Dehydration and lecular sieves are used to simultaneously


Sweetening
dehydrate and sweeten gas. A common
Natural gas often contains moisture application of the dual adsorption process
and H2S that must be removed. The ad- is that of treating gas entering a cryogenic
sorption process is ideally suited for remov- plant.
ing moisture and H2S when the acid gas Propane and LPG made in a gasoline
concentration is less than 50 ppm H2S. A plant or refinery often contains moisture
sweetening plant using a chemical such as and H2S and other sulfur compounds. Type
amine is less costly for removing higher 13X molecular sieves will remove the con-
concentrations of acid gas. Type 5A mo- taminants to meet product specifications.

3-TOWER PLANT DEHYDRATING GAS ENTERING A CRYOGENIC PLANT

MOLECULAR SIEVE DEHYDRATION PROCESS


III. PROCESS FLOW 13

An adsorption plant contains two systems: In the section that follows, the most com-
mon process flow plans are described. In
1. An adsorption system in which impuri-
order to simplify the discussion, the inlet
ties are removed from the process fluid
separator and outlet filter shown on the next
onto a bed of adsorbent.
page are omitted in subsequent flow de-
2. A regeneration system in which the
scriptions. However, these items are in-
adsorbed material is removed from the
cluded in adsorption plants.
adsorbent.
A. Flow in 2-Tower Plant
Although the adsorption and regen-
In a 2-tower plant, one tower is
eration systems are independent from one
adsorbing and the other tower is regener-
another, they must have a common ele-
ating. The regeneration time period is ob-
ment — time. A tower must be regener-
viously the same as the adsorption time.
ated and ready to switch into adsorbing
Process flow in a 2-tower system drying
service when an adsorbing tower is satu-
gas that enters a cryogenic plant is shown
rated with material it removed from the pro-
on the next page. The process inlet gas
cess fluid. The adsorbing time is the con-
enters the inlet separator, where water and
trolled time period. Towers are sized to
solid materials drop to the bottom and are
operate in adsorption service for a certain
dumped to a disposal system with a level
minimum time period — often 8 hours. The
controller. Gas flows out the top of the
regeneration system is then designed to
Separator and enters the top of Tower 2. It
complete its function in the allotted time
flows down the tower, which contains mo-
based on the adsorption time and the num-
lecular sieves that remove almost 100% of
ber of towers in adsorption service.
moisture from the gas. Dry gas flows out
Most adsorption plants have either 2,
the bottom of the tower and passes through
3, or 4 identical adsorber towers, although
a filter, which removes particles of adsor-
some plants have as many as 12. In a 2-
bent that the gas may have picked up. Gas
tower plant, one tower is adsorbing and the
leaving the filter enters a low temperature
other is regenerating. A 3-tower plant usu-
process plant.
ally has two towers adsorbing and one re-
Regeneration gas is often withdrawn
generating. Regeneration gas usually flows
from the residue gas leaving the process
up, although some plants have upflow on
plant. Its flow rate is usually 5 - 10% of the
heating and downflow on cooling. The re-
process inlet gas flow rate. Regeneration
generation gas may be process outlet gas
consists of 2 phases: a heating phase to
or gas from an outside source.
boil out the moisture and other adsorbed

MOLECULAR SIEVE DEHYDRATION PROCESS


14 PROCESS FLOW IN 2-TOWER PLANT

material that the molecular sieve removed bent boils out and is swept out of the bed
during the adsorbing cycle; a cooling phase in the regeneration gas leaving the tower
to lower the temperature of the adsorbent at the top. The gas flows through a cooler
to approximately that of the process inlet where its temperature is lowered to approxi-
gas temperature. During the heating phase, mately ambient. Most of the moisture con-
control valves switch so that inlet regen- denses from the gas in the cooler. The com-
eration gas flows through the heater, where bined gas and moisture stream out of the
its temperature is raised to 230 - 290°C cooler enters a Separator, where the mois-
[450 - 550°F]. The gas flows out of the ture drops to the bottom and is withdrawn
heater to the bottom of Tower 1 and passes to a liquid disposal system. The regenera-
up the tower. Heat in the regeneration gas tion gas flows out the top of the Separator
transfers to the adsorbent and raises its and returns to its original source.
temperature. Water contained in the adsor-

REGEN
GAS
OUTLET
REGENERATION
PROCESS REGENERATION GAS GAS COOLER
INLET FLUID TEMP RECORDER REGENERATION
GAS SEPARATOR

LIQUID
TO
DISPOSAL

INLET GAS
SEPARATOR

CYCLE
LIQUID TO
TOWER 1 SWITCHING
TOWER 2
DISPOSAL
REGENERATING VALVES
ADSORBING

TEMP
CONT

FUEL
GAS TEMP
REGENERATION RECORDER ∆P
GAS HEATER REGENERATION PROCESS
GAS FLOW OUTLET
CONTROLLER FLUID
OUTLET GAS
LINE SHADING LEGEND REGENERATION FILTER
PROCESS FLUID GAS FROM
REGENERATION GAS OUTSIDE SOURCE

2-TOWER ADSORPTION PLANT

MOLECULAR SIEVE DEHYDRATION PROCESS


PROCESS FLOW IN 3-TOWER PLANT 15

During the cooling phase of regenera- flows through each adsorbing tower. The
tion, switching valves are activated at the 3rd tower is regenerating. The regeneration
heater which by-pass the heater so that time period is half that of the adsorption time.
inlet regeneration gas flows directly to the If the adsorption time is 12 hours, a tower is
bottom of Tower 1. regenerated in 6 hours. The 2 towers in
At the end of the adsorbing time pe- adsorbing service switch 6 hours out of
riod, switching valves operate so that the phase rather than switch at the same time.
process inlet gas flows through Tower 1, The drawing below indicates the flow
and regeneration gas flows to the heater immediately after a switch. Assume the
and to Tower 2. adsorbing time period is 12 hours. Flow is
B. Flow in 3-Tower Plant with 2 as follows:
Towers Adsorbing and 1 Tower The process inlet gas stream is di-
Regenerating verted to Towers 1 and 2. The gas enters
When 2 towers are in parallel adsorp- the top, flows downward and exits at the
tion service, half of the inlet process gas bottom. Since the two towers are identical,
LINE SHADING LEGEND PROCESS
PROCESS FLUID INLET FLUID
REGENERATION GAS

REGENERATION
GAS OUTLET

REGENERATION
GAS COOLER

REGENERATION
GAS SEPARATOR

LIQUID TO
DISPOSAL

FUEL
GAS TEMP
CONT
TOWER 1 TOWER 3
ADSORBING TOWER 2
ADSORBING REGENERATING

REGENERATION
GAS HEATER REGENERATION
GAS FLOW
CONTROLLER
REGENERATION
GAS FROM
OUTSIDE SOURCE

3-TOWER PLANT WITH 2 TOWERS ADSORBING IN PARALLEL

MOLECULAR SIEVE DEHYDRATION PROCESS


16 PROCESS FLOW IN 3-TOWER PLANT

flow through each tower should be approxi- Tower 1, which has been regenerated,
mately one half of the total inlet gas stream. switches to adsorbing service.
The regeneration gas flow to Tower 3 Tower 2, which had been adsorbing for
is the same as that in the 2-tower system 12 hours, switches to regeneration.
previously described.
After 6 hours, Tower 3 is regenerated, Tower 3, which had been adsorbing for
and a switch occurs which results in flow 6 hours, remains in adsorbing service.
as follows: 1. Flow in 3-tower plant with
Tower 1, which had been in adsorbing regeneration gas compressor
service for 12 hours, switches to regen- As the regeneration gas flows through
eration. the plant, it has a pressure drop of 150 -
Tower 2, which had been in adsorbing 200 kPa [20 - 30 psi]. In some plants, a
service for 6 hours, remains in compresser is installed to make up the
adsorbing service. pressure drop. The drawing below shows a
plant in which regeneration gas is with-
Tower 3, which just completed regen-
drawn from the plant outlet gas stream, and
eration, switches to adsorbing service.
after regenerating tower No 1, it recycles
Six hours later, Tower 1 is regenerated, to the process inlet line.
and another switch occurs: PROCESS
INLET FLUID

REGENERATION
GAS COOLER
REGENERATION
GAS SEPARATOR
LIQUID TO
DISPOSAL

FUEL TEMP
GAS CONT

TOWER 1
REGENER- TOWER 2
ATING ADSORBING TOWER 3
ADSORBING

REGENERATION
GAS HEATER REGENERATION
GAS FLOW
CONTROLLER

LINE SHADING LEGEND


PROCESS FLUID
REGENERATION GAS
PROCESS
OUTLET GAS
REGENERATION
GAS COMPRESSOR

3-TOWER PLANT WITH REGENERATION GAS COMPRESSOR

MOLECULAR SIEVE DEHYDRATION PROCESS


PROCESS FLOW IN 4-TOWER PLANT 17

C. Flow in 4-Tower Plant with Two eration, and Tower 4 is heating. The inlet
Towers Adsorbing and Two Towers
Regenerating regeneration gas flows to Tower 3 which
just switched from the heating phase, and
A 4-tower plant with 2 towers the gas cools the molecular sieve in it. The
adsorbing and 2 towers regenerating is temperature of cooling gas leaving Tower
shown below. Assume towers 1 and 2 are 3 has been raised as it removed heat from
in adsorbing service for a period of 8 hours, the adsorbent in the vessel. The gas leav-
and the heating and cooling phases of re- ing at the top of the tower flows to the
generation are each 4 hours long. Flow is heater. Hot gas from the heater enters the
as follows. bottom of Tower 4 and flows upward. Gas
The process inlet gas flows to Towers from the top of Tower 4 passes through a
1 and 2 which are in adsorbing service. Dry Cooler and Separator and flows back to its
gas leaves at the bottom and exits the plant. original source.
Tower 3 is in the cooling phase of regen- After four hours, Tower 4 has been
PROCESS
INLET FLUID heated and Tower 3 has been cooled. A

REGENERATION
REGENERATION GAS OUTLET
GAS COOLER

REGENERATION
GAS SEPARATOR

LIQUID TO
DISPOSAL

TOWER 1 TOWER 2 TOWER 3


TOWER 4
ADSORBING ADSORBING COOLING
HEATING

FUEL
REGENERATION GAS
GAS HEATER

REGENERATION
GAS FROM PROCESS
OUTSIDE SOURCE OUTLET FLUID

4-TOWER PLANT WITH 2 TOWERS


ADSORBING IN PARALLEL & 2 TOWERS REGENERATING

MOLECULAR SIEVE DEHYDRATION PROCESS


18 PROCESS FLOW IN 4-TOWER PLANT

tower switch occurs. Flow is shown below. to heating. Tower 3 had been in adsorbing
Tower 4, which has been heated, switches service for 4 hours, and it remains in that
to cooling service. Tower 3, which has been service for another 4 hours.
heated and cooled, switches to adsorbing The advantage of the 2-Tower regen-
service. Tower 1, which had been in eration system is that gas entering the
adsorbing service for 8 hours, switches to heater has been pre-heated as it picked up
heating. Tower 2, which had been heat from the adsorbent in the cooling
adsorbing for 4 hours, remains in adsorbing phase. The net effect is to reduce the heater
service. fuel requirements about 20%. The main dis-
At the end of 4 hours, another switch advantage of the 2-tower regeneration sys-
occurs. Tower 4 has completed its cooling tem is that the regeneration gas flows
cycle, so it switches to adsorption. Tower 1 through 2 towers instead of one, so it has a
has completed its heating phase, and it higher pressure drop which must e made
switches to cooling. Tower 2 has been in up with a compressor at some point.
adsorbing service for 8 hours, so it switches
PROCESS
INLET FLUID

REGENERATION
REGENERATION GAS OUTLET
GAS COOLER

REGENERATION
GAS SEPARATOR

LIQUID TO
DISPOSAL

TOWER 1 TOWER 2 TOWER 3


TOWER 4
HEATING ADSORBING ADSORBING
COOLING

FUEL
REGENERATION GAS
GAS HEATER

REGENERATION
GAS FROM PROCESS
OUTSIDE SOURCE OUTLET FLUID

4-TOWER PLANT WITH 2 TOWERS


ADSORBING IN PARALLEL & 2 TOWERS REGENERATING

MOLECULAR SIEVE DEHYDRATION PROCESS


TOWER SWITCHING SEQUENCE 19

D. Flow When Pressure of Regenera-tion Small valves for pressuring and


Gas and Main Gas are Different
depressuring are provided so that a gradual
In most cryogenic facilities, regenera- pressure change can take place. Valve op-
tion gas is withdrawn from the cryo plant eration at the time of a tower switch is as
outlet gas line, which is often at a different follows:
pressure from the inlet pressure to the de- 1. Tower 1 will switch to adsorbing service.
hydrator. The flow sheet below shows a a. Close valve R-1.
situation in which the regeneration gas b. Close valve R-2.
c. Open valve P-1. Pressure in
pressure is 700 kPa [100 psi] lower than
Tower 1 will slowly rise to inlet gas
the inlet gas pressure. Significant damage
pressure.
could occur to the mole sieves if a pres- d. When pressure in Tower 1 and 2
sure shock of this magnitude should oc- equalize, open valves M-1 and M-2.
cur. Severe packing of adsorbent could TO GAS
SALES

occur with a sudden increase in pressure, 5300 kPa


[750 psi]

and severe breakage could result from a


sudden reduction in pressure. REGENERATION
REGENERATION GAS GAS COOLER
INLET FLUID TEMP RECORDER REGENERATION
GAS SEPARATOR FC
6000 kPa M-1
[850 psi] R-1 R-3 M-3
P-1 LIQUID
PRESSURING
TO
VALVES
DISPOSAL
P-2
INLET GAS
SEPARATOR
FC

LIQUID TO
TOWER 1 TOWER 2
DISPOSAL
REGENERATING DRYING

TEMP
CONT
R-4

FUEL M-2 R-2 M-4


GAS
REGENERATION ∆P
GAS HEATER
OUTLET
FLUID
OUTLET GAS
FILTER

REGENERATION GAS

RESIDUE
GAS
FROM
GAS DEHYDRATION PLANT WITH CRYOGENIC
PLANT
REGENERATION GAS PRESSURING VALVES

MOLECULAR SIEVE DEHYDRATION PROCESS


20 TOWER SWITCHING SEQUENCE

Tower 1 is now in adsorbing service. heater and start heater.


2. Tower 2 will switch to regeneration ser- E. Tower Switching Sequence
vice. In a 2-tower plant, one tower is
a. Close valve P-1. adsorbing and the other is regenerating.
b. Close valve M-3. The regeneration time period is obviously
c. Close valve M-4. the same as the adsorbing time period. An
d. Open valve P-2. Tower will 8-hour cycle is commonly used. One tower
depressure. adsorbs for 8 hours and the other tower
e. When tower 2 pressure drops to regenerates in 8 hours. Regeneration usu-
regeneration pressure, open valve ally includes 5 hours of heating followed by
R-4. 3 hours of cooling.
f. Open valve R-3 and close valve P-2. A daily switching sequence chart for
g. Open flow of regeneration gas to such a plant is as follows. The gray area
represents the regeneration phase.

SWITCHING SEQUENCE FOR 2-TOWER PLANT ON 3 HOUR CYCLE


TOWER 1 Heating Cooling Adsorbing Heating Cooling
TOWER 2 Adsorbing Heating Cooling Adsorbing
12 M 5 AM 8 AM 1 PM 4 PM 9 PM 12 M

In plants having two towers in adsorp- adsorption service, and the adsorption time
tion service and one tower regenerating, is often 12 hours. The regeneration time is
the time of regeneration will be half that of half the adsorption time. The daily switch-
adsorption. The most common multi-tower ing sequence for a 12-hour adsorption cycle
adsorption plant has two towers in parallel is as follows:

SWITCHING SEQUENCE FOR 3-TOWER PLANT WITH 2 PARALLEL TOWERS


ADSORBING FOR 12 HOURS AND 1 TOWER REGENERATING IN 6 HOURS
TOWER 1 Adsorbing Heating Cooling Adsorbing
TOWER 2 Adsorbing Heating Cooling Adsorbing
TOWER 3 Heating Cooling Adsorbing Heating Cooling

12 M 3 AM 6M 9M 12 N 3 PM 6 PM 9 PM 12 M

MOLECULAR SIEVE DEHYDRATION PROCESS


SWITCHING VALVE OPERATION 21

Problem 3
A 2-tower plant has a 12-hour adsorption time cycle. Regeneration phases are 7
hours of heating and 5 hours of cooling. Tower switch occurs at midnight. Tower 1 switches
to adsorbing, and Tower 2 is regenerating. Indicate the service of each tower at times
shown. Service is either adsorbing, heating or cooling.

TIME SERVICE
Tower 1 Tower 2
12 M Adsorbing Heating
8 AM __________ __________
1 PM __________ __________
9 PM __________ __________

F. Switching Valve Operation towers in the plant. In most plants, switch-


Switching valves are operated periodi- ing valves are operated by an electro/pneu-
cally to divert the flow of process fluid and matic system triggered by a clock or timer
regeneration gas into or out of the various as shown in the drawing below.
TIMER
TIMER
0
0
18 6 1 18 6
12 At 0800, clock
1 12
trips switch in
circuit to ralay. At 1600, clock
trips switch in
2 circuit to relay.
RELAY RELAY
Relay closes switch 12 or 24
12 or 24
that completes cir- DC Volts 2 DC Volts
cuit to solenoid. Relay opens switch
that breaks circuit
INSTR to solenoid. INSTR
AIR AIR

4-WAY 4-WAY
3 SOLENOID 4 SOLENOID 4
VALVE 3 VALVE
Solenoid energizes When 4-way valve When 4-way valve
opens, air pressure Solenoid deenergizes
and moves 4-way closes, air pressure
above piston actuator and moves 4-way
valve to open position. below piston actuator
is vented, and air valve to closed position.
VENT is vented, and air
pressure is diverted VENT
pressure is diverted
below the piston, above the piston,
which moves upward which moves down-
and opens the switch- ward and closes the
ing valve. switching valve.

SWITCHING SWITCHING
VALVE VALVE
SWITCHING VALVE OPERATION

MOLECULAR SIEVE DEHYDRATION PROCESS


22 SWITCHING VALVE OPERATION

Switching valves are often ball valves bers on a keyboard located on the control-
equipped with pneumatic piston actuators ler panel. The pneumatic actuated switch-
that require air pressure on top of or below ing valves and 4-way solenoid valves are
the piston in order to change the position still used.
of the valve. It is obviously necessary to Plants that remove close to 100% of a
vent air from one side of the piston in order contaminant from a fluid stream must be
for air pressure on the opposite side to force thoroughly regenerated. One way of assur-
it to move. This is accomplished with a 4- ing adequate heating during regeneration
way solenoid valve that diverts the flow of is to use a temperature switch located in
air to one side of the piston and simulta- the heating gas outlet line to switch from
neously vents air from the other side. heating to cooling. If the bed must be
The switching lugs shown on the Timer heated to 260°C [500°F] to completely strip
in the opposite drawing at 8 and 16 hours adsorbed material, the temperature switch
are adjustable so that the cycle can be in- is set at that point, and the heating phase
creased or reduced. The drawing shows will continue until that temperature is
only 2 lugs, whereas additional lugs are reached. The temperature switch will then
required for by-passing the heater, and for trip and by-pass the heater so that cooling
switching towers at midnight. will begin.
The switching control in plants built Another temperature switch may be
after 1980 may include a micro-computer located in the cooling gas outlet line to pre-
and micro-switches instead of a timer and vent the tower from switching to adsorp-
relay. With this type of control, the cycle time tion service until the bed is cooled to the
is changed by entering a series of num- set point of the temperature switch.

Problem 4

Match items in the two columns:

_______ 1. Switching valves a. One tower adsorbing, one tower regenerat-


ing.

_______ 2. 2-tower plant b. Two towers adsorbing one tower regenerat-


ing.

_______ 3. 3-tower plant c. Divert gas flow from one tower to another.

MOLECULAR SIEVE DEHYDRATION PROCESS


IV. REGENERATION OF ADSORBENT 23

A. Principles of Regeneration as much material from the process stream


Regenerating the adsorbent is the at a high temperature.
most important and least understood Refer to the flow diagram for the 2-
phase of an adsorption plant operation. It tower plant shown below. Tower 2 is
is the most expensive part of the opera- adsorbing and Tower 1 is regenerating.
tion because fuel is consumed in heating During the heating phase of regeneration,
the regeneration gas. the regeneration gas flows through the
Regeneration consists of a heating heater prior to entering Tower 1. During the
phase to boil out the adsorbed material, cooling phase, the heater is by-passed and
and a cooling phase to lower the adsor- the regeneration stream flows directly to
bent temperature to approximately that of Tower 1. This gas flow should cool the ad-
the process inlet stream. Cooling is essen- sorbent to within about 20°C [35°F] of the
tial because the adsorbent will not remove temperature of the process inlet fluid.

REGEN PROCESS
GAS INLET FLUID LINE SHADING LEGEND
OUTLET PROCESS FLUID
REGENERATION GAS

REGENERATION
GAS COOLER REGEN
REGENERATION GAS
GAS SEPARATOR TEMP
RECORDER

LIQUID TO
DISPOSAL

TOWER 1
REGENERATING TOWER 2
ADSORBING
TEMP
CONTR

FUEL
GAS
REGENERATION TEMP PROCESS
GAS HEATER RECORDER OUTLET FLUID
REGENERATION
GAS FROM
OUTSIDE SOURCE

2-TOWER DEHYDRATION

MOLECULAR SIEVE DEHYDRATION PROCESS


24 REGENERATION OF ADSORBENT

To simplify our discussion on regen- The heating phase of regeneration in-


eration, let’s consider a gas dehydration cludes 3 parts:
plant. The regeneration principles which
1. Heat the adsorbent to the boiling tem-
apply to it will also apply to other types of
perature of water.
adsorption plants. During the adsorbing
phase, the adsorbent removes moisture 2. Add enough heat to vaporize most of
from the gas passing through it. The mois- the water. About 90% of the water will
ture is in the form of steam in the gas, but it boil off at this point.
changes to a liquid when it is adsorbed. At
3. Heat the adsorbent to drive off the re-
the conclusion of the adsorbing period, the
maining 10% of the water.
adsorbent is saturated with water. The wa-
ter will be boiled out of the adsorbent dur- The last step is the most important and
ing regeneration. most difficult. Any adsorbed material that
Water boils at 100°C [212°F] at atmo- remains on the adsorbent after regenera-
spheric pressure. Its boiling point is higher tion obviously reduces the capacity of the
as the pressure is raised. At the operating adsorbent. It also lowers the efficiency of
pressure of most adsorbers, its boiling tem- the adsorbent, which results in a higher dew
perature is about 150°C [300°F]. The heat point of treated gas in a dehydration plant.
of vaporization for water is 2264 kJ per kg About 25% of the total heater fuel is re-
[970 Btu per lb]. This heat must be added quired to drive off the last 10% of adsorbed
to water when it is at its boiling tempera- material, so it is the most expensive part of
ture in order to boil the water. regeneration.

TYPICAL PROCESS REQUIREMENTS FOR


DEHYDRATION PLANTS
REGEN GAS REGENERATION HEAT
MOISTURE DEW FLOW TEMP TO HEAT
ADSORBENT REMOVED POINT OF SOURCE DIRECTION ADSORBENT HEATER FUEL GAS
CAPACITY FROM INLET TREATED OF IN m3/kg of cu ft/lb of
TYPE Wt% GAS % GAS GAS TOWER °C °F ADSORBENT ADSORBENT
Mol 10.0 99.9% Below Treated Up 232° 450° 0.062 1.0
Sieve -62°C Gas
[-80°F]

MOLECULAR SIEVE DEHYDRATION PROCESS


REGENERATION OF ADSORBENT 25

Regeneration heat is provided with hot adsorber at a temperature of 260°C


gas which flows through a heater. The heat- [500°F]. At the start of the heating phase,
ing gas is a heat transfer fluid. It is trans- the temperature of the adsorbent and pip-
ferring heat from the heater to the adsor- ing is 38°C [100°F]. The adsorbent in the
bent. We would prefer to have the adsor- bottom of the tower heats very quickly at
bent flow through the heater, but this is not the start of the regeneration, because it is
practical. A secondary function of the re- contacting the hottest regeneration gas. It
generation gas is to sweep out adsorbed approaches the maximum temperature
material as it boils off the adsorbent. approximately 4 hours after heating starts.
We said that the first step in the heat- The plateau in the temperature trace at
ing phase is to heat the adsorbent to the 127°C [260°F] is due to water boiling off
boiling temperature of water or other the adsorbent.
adsorbed material. At the time regenera- By the time heating gas gets to the
tion starts, the piping, adsorbent, and middle of the tower, it has given up some
adsorber tower are at the temperature of of its heat in the lower portion, so that it is
the process inlet fluid. In order to heat the at a lower temperature. It takes about 5
adsorbent to the boiling temperature of hours for the adsorbent temperature in the
water, it is also necessary to heat the pip- middle of the tower to reach the same tem-
ing and steel in the adsorber tower. In fact, perature that the bottom of the tower
about 1/3rd of the total heater duty is to heat reached in 3 hours.
the steel in piping and the adsorber ves- The top portion of the tower is the last
sel. Another 1/3rd is used in raising the tem- portion to be heated. It reaches its peak
perature of the adsorbent, and the final 1/ temperature at the end of the heating
3rd is the heat of vaporization required to phase, and cooling commences.
boil off the adsorbed material. When the temperature of the adsor-
During the heating phase of regenera- bent in the bottom of the tower reaches
tion, hot gas from the heater flows through 127°C [260°F], the water starts to boil out.
the adsorbent, and some of the heat in the However, the temperature of adsorbent in
gas transfers to the adsorbent. The figures the upper part of the tower is below the
on the following pages indicate tempera- boiling point of water, so most of the water
ture profiles in a tower during an 8 hour that boils out at the bottom condenses in
regeneration cycle. The bottom and top the upper section. If you could see inside
profiles are gas temperatures entering the tower during the heating phase, you
and leaving the tower. The 3 middle pro- would observe rain falling in the upper part
files are adsorbent temperatures. as water condenses from the gas.
Hot gas enters the bottom of the The temperature plateau in the top of

MOLECULAR SIEVE DEHYDRATION PROCESS


26 TEMPERATURE PROFILES IN ADSORBER
DURING REGENERATION - SI UNITS
300

REGENERATION
200
GAS OUTLET

100
OUTLET GAS
TEMP
0
0 1 2 3 4 5 6 7 8
300

200

100
TOP
ADSORBENT
TEMP 0
0 1 2 3 4 5 6 7 8
300

200

100
MIDDLE
ADSORBENT
TEMP 0
0 1 2 3 4 5 6 7 8
300

200

100
BOTTOM
ADSORBENT
TEMP 0
0 1 2 3 4 5 6 7 8

300

200

100
INLET GAS
TEMP
REGENERATION
0
GAS INLET 0 1 2 3 4 5 6 7 8
HEATING COOLING
ELAPSED TIME, HOURS

MOLECULAR SIEVE DEHYDRATION PROCESS


TEMPERATURE PROFILES IN ADSORBER 27
DURING REGENERATION - ENGLISH UNITS
500

REGENERATION
400
GAS OUTLET

300

OUTLET GAS
200
TEMP
100
0 1 2 3 4 5 6 7 8

500

400

300

TOP
ADSORBENT 200
TEMP
100
0 1 2 3 4 5 6 7 8
500

400

300

MIDDLE 200
ADSORBENT
TEMP 100
0 1 2 3 4 5 6 7 8
500

400

300

BOTTOM 200
ADSORBENT
TEMP 100
0 1 2 3 4 5 6 7 8
500

400

300

INLET GAS 200


TEMP
REGENERATION 100
0 1 2 3 4 5 6 7 8
GAS INLET HEATING COOLING
ELAPSED TIME, HOURS

MOLECULAR SIEVE DEHYDRATION PROCESS


28 REGENERATION OF ADSORBENT

the tower and in the outlet gas is more temperature is 235°C [455°F]. The differ-
prominent than that in the middle or bot- ence in the inlet and outlet gas tempera-
tom because more water boils out of the ture at the end of the heating cycle is 25°C
top adsorbent due to the condensation. The [45°F]. The significance of this is that of the
outlet gas temperature often drops off a few total heat in the regeneration gas, only 25°C
degrees before it reaches the water boil- [45°F] or 11% transfers to the adsorbent at
off plateau. This drop is due to water con- the end of the heating cycle. The other 89%
densing from gas flowing up the tower. of heat is in the regeneration gas leaving
As we previously said, only 90% of the the tower. To put it another way, only 11%
water boils out of the adsorbent when it is of the fuel burned in the Regeneration Gas
heated to the water boiling point. About Heater is utilized during the last 20 - 60
10% of the water remains on the adsorbent minutes of the heating phase.
because the adsorbent still has some attrac- After 5 hours of heating, the cooling
tion for water. This attraction diminishes as phase commences. The regeneration gas
the temperature is raised. It approaches zero by-passes the heater and flows directly into
at a temperature of 232°C [475°F]. the regenerating tower. Its temperature is
At the end of the heating period, the 38°C [100°F].
adsorbent in the lower part of the tower is During the cooling phase, the adsor-
heated to a temperature of 246°C [475°F], bent at the bottom of the tower is cooled
whereas the peak temperature at the top more than that in the middle or top. This, of
of the tower is 218°C [425°F]. The average course, is because it is contacting the cool-
temperature to which the adsorbent is ing gas first. As the cooling gas cools the
heated is 232°C [450°F]. The peak outlet bottom part, the gas is warmed so that it
temperature of gas leaving the tower is does not cool the upper portion of the tower
232°C [455°F], which is 3°C [5°F] above as much as it does the bottom. The lower
the average temperature to which the ad- part of the tower is cooled to a tempera-
sorbent is heated. ture of 52°C [125°F], whereas the top por-
The peak temperature of gas leaving tion is cooled to only 79°C [175°F]. The av-
the adsorber is the primary means for indi- erage temperature of adsorbent after cool-
cating the completeness of regeneration. ing is 66°C [150°F] which is 28°C [50°F]
However, the average temperature to which higher than the temperature of the cooling
the adsorbent is heated is 3 - 6°C [5 - 10°F] gas that enters the tower.
below the peak outlet gas temperature dur- The adsorbent at the bottom of the
ing the heating phase. tower gets heated more and cooled more
The heating gas inlet temperature is than the adsorbent in the top of the tower.
260°C [500°F], and the peak outlet gas Consequently, it will have more adsorbed

MOLECULAR SIEVE DEHYDRATION PROCESS


REGENERATION OF ADSORBENT 29

material boiled out of it, and since it is the temperature of the regeneration gas as
cooler, it will adsorb more than that at the it enters the tower (approximately heater
top of the tower. To put it another way, the outlet temperature) and another recorder
adsorbent at the end of the tower that the showing the temperature of gas that leaves
regeneration gas enters will be the purest the tower. Quite often, a single instrument
and have the greatest capacity of any of with two pens is used to record the inlet
the adsorbent in the tower. and outlet temperatures.
At the conclusion of the cooling cycle, Typical 2-pen regeneration tempera-
the tower switches to adsorption. The tem- ture charts are shown below. Of course,
perature of the adsorbent is higher than different types of recording charts provide
that of the process gas passing through it, different kinds of plots. The plots shown are
so it will heat the process gas a few de- for a 2-tower plant with an 8-hour re-
grees for 15 - 30 minutes. At the end of generation period… 5 hours of heating,
that time, the process gas stream will cool and three hours at cooling. The regen-
the adsorbent so that both are at the same eration gas enters the bed at 300°C
temperature. The dew point of treated gas [575°F] during heating, and 30°C [86°F]
may rise a few degrees during this period. during cooling.
Most plants have recorders showing

300 600
PEAK OUTLET
TEMPERATURE PEAK OUTLET
TEMPERATURE OF TEMPERATURE OF TEMPERATURE
REGENERATION GAS 500 REGENERATION GAS
TO TOWER TO TOWER
TEMPERATURE, °C

TEMPERATURE, °F

WATER 400
200 BOIL OFF
WATER
BOIL OFF

300

100 200

TEMPERATURE OF TEMPERATURE OF
REGENERATION GAS 100 REGENERATION GAS
OUT OF TOWER OUT OF TOWER

HEATING PHASE COOLING PHASE HEATING PHASE COOLING PHASE

0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
ELAPSED TIME IN REGENERATION PERIOD, HOURS ELAPSED TIME IN REGENERATION PERIOD, HOURS

TEMPERATURE RECORDING CHARTS FOR REGENERATION GAS


ENTERING AND LEAVING A TOWER

MOLECULAR SIEVE DEHYDRATION PROCESS


30 REGENERATION OF ADSORBENT

In the outlet gas temperature trace, The exception to this is in sulfur removal
you can see a plateau at about 150°C plants, where additional sulfur compounds will
[300°F]. This is quite typical in dehydrator boil out after the peak temperature is reached.
temperature profiles. It is the result of the In these plants, the peak temperature should
water boiling off the desiccant. If a slug of occur 30 minutes to 1 hour before the con-
water enters the plant, the plateau will be clusion of the heating phase.
more prominent when the tower that re- B. Heat Transfer During Regeneration
ceived the slug is regenerated. Sometimes, As we said previously, the heating gas
in rich gas systems, there will be other pla- is a heat transfer fluid. It receives heat in
teaus where various hydrocarbon fractions the heater, and transfers some of it to the
are leaving the adsorbent. adsorbent. Only 35 - 40% of the heat re-
Temperature traces are individual leased by the heater actually transfers to
characteristics of each tower. They are al- the tower. The other 60 - 65% remains in
most as exclusive as fingerprint. Tempera- the regeneration gas that leaves the tower
tures in towers being regenerated may vary being heated. During the first part of the
from one tower to another at the same point heating cycle, the adsorbent is cool and
in each tower’s cycle. One tower may heat about 90% of the heat in the regeneration
to a temperature of 205°C [401°F] after 3 gas transfers to the adsorbent. However
hours, whereas another tower in the same during the latter part of the heating phase,
plant heats to only 190°C [374°F]. Conse- the adsorbent temperature approaches the
quently, temperature data must be com- regeneration gas temperature and only 15
pared with prior readings on the same - 20% heat transfer occurs.
tower at the same time in the cycle. The amount of heat that transfers from
The temperature trace of gas leaving the hot regeneration gas to the adsorbent
the tower near the end of the heating phase depends upon the difference in tempera-
is one of the best means of determining if ture between the gas and the adsorbent.
the regeneration gas flow rate and the heat- More heat will transfer when there is a
ing time period are properly set. The peak greater temperature difference. For ex-
outlet temperature should occur 15 - 30 ample, if the temperature of regeneration
minutes before the end of the heating pe- gas out of the heater is raised 5°C [9°F],
riod. Once the bed is heated to the peak 6% more heat will transfer from the regen-
temperature, no additional water will boil eration gas to the adsorbent. This means
out. However, most operators hold peak that he adsorbent can be heated to the
temperature to insure 100% regeneration. same temperature in 6% less time. Rais-

MOLECULAR SIEVE DEHYDRATION PROCESS


HEAT TRANSFER DURING REGENERATION 31

ing the temperature of gas out of the heater will be required.


by 5°C [9°F] will increase the heater fuel
about 3%. However, the heating time pe- C. Optimizing Regeneration
riod is reduced by 6%, so the net heater Fuel consumed in the Regeneration
fuel saving is 3%. Gas Heater is the major operating expense
If the regeneration gas heater is firing of an adsorption plant. Significant savings
at its maximum rate, it will be necessary to in heater fuel are often achievable by opti-
reduce the regeneration gas flow rate in mizing the process operating conditions.
order to raise the temperature of gas leav- The 3 process variable in the regeneration
ing the heater. A 2.5% reduction in flow rate system are:
will allow you to raise the heater outlet tem- 1. Regeneration gas flow rate.
perature 5°C [9°F] with the same fuel rate
2. Regeneration gas heater outlet tem-
to the heater. Lowering the flow rate and
perature.
raising the temperature will allow you to
regenerate the tower to the same tempera- 3. Heating and cooling time.
ture in 3.0% less time. The net heater fuel The goal in optimizing is to satisfacto-
savings is also 3.0%. The table below sum- rily regenerate the towers with the lowest
marizes the methods of heating the tower fuel rate to the heater. Satisfactory regen-
at a lower heater fuel rate. eration is that which boils off all of the
Either of the below methods will allow adsorbed material so that when the tower
you to heat the tower in a shorter period of switches to adsorbing service, the treated
time, so the heating time period should be process fluid is slightly better than specifi-
lowered. If you raise the heater outlet tem- cation limits.
perature without lowering the heating time The procedure to optimize involves
period, heater fuel consumption will in- changes in the regeneration gas flow rate,
crease. In addition, more heat will be trans- heater outlet temperature and heating time.
ferred to the tower, so more cooling time Changes are made in steps, and the effect

MEANS OF HEATING TOWER WITH LESS HEATER FUEL


WHEN REGEN CHANGE REGEN RAISE HEATER LOWER HEATER
HEATER FIRING GAS FLOW OUTLET TEMP HEATING FUEL
RATE IS RATE °C °F TIME SAVING
Below Max No change 5° 9° 6% 3.0%
Maximum Lower 2.5% 5° 9° 3.0% 3.0%

MOLECULAR SIEVE DEHYDRATION PROCESS


32 OPTIMIZING REGENERATION

of each step change is determined by ob- not meet specifications (has a high water
serving the quality of treated gas when the content) regeneration process changes
tower switches to adsorbing service. are first made which produce treated
For example, suppose the step change gas of acceptable quality. Optimizing
is to lower the heating time period in 5 can then proceed.
minute steps. The heating cycle time is re- There are 2 factors that determine the
duced 5 minutes for each tower, and the procedure to optimize:
quality of treated gas is observed for each 1. The quality of treated gas — it does not
tower for several cycles. If treated gas qual- meet specification, it just meets speci-
ity is okay, another 5 minute reduction is fication, or is better than specification.
made, and treated gas quality is observed
2. The temperature of regeneration gas
again for several cycles. The step changes
leaving the tower during the heating
continue until treated gas quality reaches
phase — it peaks before the end of the
its specification limit. At this point, back up
heating phase, or it peaks after the end
1 step (add 5 minutes to the heating time)
of the heating phase, or it peaks at the
and proceed to the next process step
end of or a few minutes after the end of
change.
the heating phase.
In order to optimize, you must have
instruments to continuously measure the The procedure to optimize for each of
quality of treated gas. In addition, the qual- the above cases is shown on the following
ity of treated gas must meet specification pages. It is a good operating practice to
limits before optimizing. If treated gas does calibrate instruments before optimizing.

Problem 5
List the first corrective action to take in each of the following situations to optimize
heater fuel.

DEW POINT TEMPERATURE OF


OF HEATING GAS OUT OF
TREATED GAS REGENERATING TOWER FIRST ACTION TO TAKE
a. Does not meet Rising at end of ___________________
specification. heating cycle.
b. Better than Peaks 30 min. before ___________________
specification. end of heating cycle.

MOLECULAR SIEVE DEHYDRATION PROCESS


PROCEDURE TO OPTIMIZE REGENERATION WHEN PEAK 33
OUTLET TEMPERATURE OCCURS
BEFORE THE END OF THE HEATING PHASE
TREATED
GAS CORRECTIVE ACTION TO PRODUCE TREATED GAS OF ACCEPT-
QUALITY DIAGNOSIS ABLE QUALITY AT MINIMUM REGEN GAS HEATER FUEL GAS

Bad - 1. Regen gas flow is OK or high. If flow 1. Raise heater outlet temp in 5°C [9°F] steps until treated gas quality is
High rate was low, peak temp would not oc- OK. If heater fires at max rate before treated gas reaches acceptable
Water cur before end of heating phase. quality, cut regen flow in 2.5% steps and maintain maximum firing rate.
Content 2. Heating time is too long. Peak temp Gas temp out of heater should rise 5°C [9°F] at each flow reduction
occurs before end of heating phase. step. Continue temp increase steps until treated gas quality is OK.
3. Since peak temp occurs before end of 2. If peak outlet temp after step 1 still occurs before end of heating phase,
heating phase, tower is heated to max cut heating time in 5 min. Steps until treated gas quality goes off - spec
temp possible with heating gas. Temp then add 5 min to heating time.
is not high enough to boil out all the 3. If heater is not firing at max rate after step 2, raise outlet temp 5°C
water, and treated gas quality is bad. [9°F] again. The peak outlet temp of heating gas should be 5°C [9°F]
Heating gas temp must be raised to boil above the peak temp at step 2 in 6% less time. Treated gas quality
out more water. should improve.
4. After step 3, if peak outlet temp is at least 4°C [7°F] above peak temp
at step 2, and treated gas quality is OK, cut heating time in 5 min steps
until treated gas quality goes off-spec. Add 5 min to heating time.
5. Repeat steps 3 and 4 until heater is firing at max rate, or heating outlet
temp is raised.
OK 1. Regen gas flow is OK or high. If flow 1. Lower heating time in 5 min steps until treated gas quality goes off-
rate was low, peak temp would not oc- spec. Then add 5 min to heating time. Peak outlet temp should occur
cur before end of heating phase. near end of heating phase.
2. Heating time is too long. Peak temp 2. After step 1, if heater is not firing at max rate, raise outlet temp 5°C
occurs before end of heating phase. [9°F]. The peak outlet temp of heating gas should be 5°C [9°F] above
3. Heating gas temp out of heater is OK the peak temp at step 1 in 6% less time. Treated gas quality should
because treated gas quality is OK. improve.
3. After step 2, if the peak outlet temp is at least 4°C [7°F] above the peak
temp at step 1, and treated gas quality is OK, cut heating time in 5 min
steps until treated gas quality goes off-spec. Add 5 min to heating time.
4. Repeat step 2 and 3 until heater is firing at max rate, or heating time
cannot be cut at least 3% when heating gas temp is raised.
Too 1. Since treated gas quality is better than 1. Lower heating time in 5 min steps until treated gas quality just meets
Good - necessary, tower is being heated too spec. Then add 5 min.
Moisture much. 2. After step 1, if heater is not firing at max rate, raise outlet temp 5°C
Content 2. Regen gas flow is too high, or heating [9°F]. The peak outlet temp of heating gas should be 5°C [9°F] above
Less time is too long, or gas temp is too high. the peak temp at step 1 in 6% less time. Treated gas quality should
Than 3. Max fuel saving is achieved by lower- improve.
Spec. ing heating time. 3. After step 2, if the peak outlet temp is at least 4°C [7°F] above the peak
temp at step 1, and treated gas quality is OK, cut heating time in 5 min
steps until treated gas quality goes off-spec. Add 5 min to heating time.
4. Repeat steps 2 and 3 until heater is firing at max rate, or heating time
cannot be cut at least 3% when heating gas temp is raised.

500
ENGLISH UNITS
TEMP OF REGENERATION GAS
LEAVING TOWER, °F
TEMP OF REGENERATION GAS

300 400
SI UNITS
LEAVING TOWER, °C

200 300

100 200

HEATING PHASE COOLING PHASE HEATING PHASE COOLING PHASE


0 100
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
ELAPSED TIME DURING REGENERATION CYCLE, HOURS ELAPSED TIME DURING REGENERATION CYCLE, HOURS

TEMPERATURE TRACES OF REGENERATION GAS LEAVING TOWER WHEN THE


PEAK TEMPERATURE OCCURS BEFORE THE END OF THE HEATING PHASE

MOLECULAR SIEVE DEHYDRATION PROCESS


34 PROCEDURE TO OPTIMIZE REGENERATION WHEN PEAK
OUTLET TEMPERATURE OCCURS
AFTER HEATING PHASE CONCLUDES
TREATED
GAS CORRECTIVE ACTION TO PRODUCE TREATED GAS OF ACCEPT-
QUALITY DIAGNOSIS ABLE QUALITY AT MINIMUM REGEN GAS HEATER FUEL GAS

Bad - 1. Since treated gas quality is bad, tower 1. If regen heater is not firing at max rate, raise regen flow rate in 2.5%
High is not heated enough to boil out all the steps until treated gas quality is OK, or regen heater is firing at max
Water water. rate.
Content 2. Since outlet temp is still rising at the 2. After step 1, if regen heater is firing at max rate and treated gas quality
end of the heating phase, the heating is still bad, increase heating time in 5 min steps until treated gas qual-
gas temp is probably OK, but the heat- ity if OK.
ing time is too short, or the regen gas 3. If the quality of treated gas meets specification during step 1, and the
flow is too low to heat the tower enough heater is not firing at max rate, raise heater outlet temp 5°C [9°F] again.
to boil all the water out. The peak outlet temp of heating gas should be 5°C [9°F] above the
3. If the heating time is increased, the peak temp before raising the temp in 6% less time. Treated gas quality
cooling time will be lowered, which will should improve.
result in a higher temp of treated gas 4. After step 3, if peak outlet temp is at least 4°C [7°F] above peak temp
when tower switches to adsorption. before raising heater temp, and treated gas quality is OK, cut heating
4. Raising regen flow rate will raise the time in 5 min steps until treated gas quality goes off-spec. Add 5 min to
tower temp and boil out more water heating time.
without increasing the heating time, 5. Repeat steps 3 and 4 until heater is firing at max rate, or heating time
providing the regen gas temp out of the cannot be cut at least 3% when the heater outlet is raised.
heater remains the same. If heater is
not firing at max rate, regen gas flow
can be increased and held at the same
temp.
OK 1. Since treated gas quality is OK, regen 1. If heater is not firing at max rate, raise outlet temp 5°C [9°F]. The peak
flow, temp and heating time are OK. outlet temp of heating gas should be 5°C [9°F] above the present peak
2. Heater fuel can be lowered if heater is temp in 6% less time. Treated gas quality should improve.
not firing at max rate. 2. After step 1, if peak outlet temp is at least 4°C [7°F] above its present
temp, and treated gas quality is OK, cut heating time in 5 min steps
until treated gas quality goes off-spec. Add 5 min to heating time.
3. Repeat steps 1 and 2 until heater fires at max rate, or heating time
cannot be cut at least 3%.
Too 1. Since quality of treated gas is better 1. Lower heating time in 5 min steps until treated gas quality just meets
Good - than necessary, tower is being heated spec. Then add 5 min.
Moisture too much. 2. After step 1, if heater is not firing at max rate, raise outlet temp 5°C
Content 2. Regen gas flow is too high, or heating [9°F]. The peak outlet temp of heating gas should be 5°C [9°F] above
Less time is too long, or gas temp is too high. the peak temp at step 1 in 6% less time. Treated gas quality should
Than 3. Max heat fuel saving is achieved by improve.
Spec. lowering heating time. 3. After step 2, if the peak outlet temp is at least 4°C [7°F] above the peak
temp at step 1, and treated gas quality goes off-spec. Add 5 min to
heating time.
4. Repeat steps 2 and 3 until heater is firing at max rate, or heating time
cannot be cut at least 3% when heating gas temp is raised.

500
ENGLISH UNITS
TEMP OF REGENERATION GAS
LEAVING TOWER, °F

400
TEMP OF REGENERATION GAS

300
SI UNITS
LEAVING TOWER, °C

200 300

100 200

HEATING PHASE COOLING PHASE HEATING PHASE COOLING PHASE


0 100
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
ELAPSED TIME DURING REGENERATION CYCLE, HOURS ELAPSED TIME DURING REGENERATION CYCLE, HOURS

TEMPERATURE TRACES OF REGENERATION GAS LEAVING TOWER WHEN


TEMPERATURE IS RISING AT THE END OF THE HEATING PHASE

MOLECULAR SIEVE DEHYDRATION PROCESS


COOLING PHASE OF REGENERATION 35

D. Cooling Phase of Regeneration enough of the bed to adsorb for 15 - 30


Most of our discussion so far has em- minutes. During this period, the remainder
phasized the importance of heating the of the bed will be cooled by the main pro-
adsorbent during regeneration. However, cess stream.
cooling the adsorbent after the heating Cooling of the bed by the main pro-
phase is also important. When the cooling cess fluid results in a temperature rise in
phase is completed, the tower switches to the outlet process fluid. It may be only a
adsorption service. If the bed is hot at the few degrees, or it may be as much as 25°C
time of switching, it will have a low adsorp- [45°F], depending upon how hot the bed is
tion capacity, and may not remove enough when it switches to adsorbing. The tem-
material from the main process stream. perature rise will occur immediately after a
The dew point of treated gas will rise. tower switches to adsorption, and will tail
Cooling gas flows through the entire off, usually in less than an hour. This tem-
bed, so it is not possible to cool only a part perature rise generally has little effect on
of it. However, the portion of the bed that the adsorption plant, but it may adversely
the cooling gas contacts first will cool more effect a downstream process plant… par-
than the portion the cooling gas contacts ticularly if the gas enters a low tempera-
last. The cool end will usually be 25 - 36°C ture plant.
[45 - 65°F] cooler than the other end. Thus, if the temperature of outlet gas
In most adsorption plants, flow of re- from an adsorption plant must remain fairly
generation gas —heating and cooling — constant, the cooling phase must be length-
is only a fraction of the main process flow. ened, or flow of cooling gas increased, so
Consequently, when a tower completes its that very little heat remains in the bed when
cooling phase and switches to adsorbing, cooling is completed.
the gas flow rate through the adsorber is We previously said that about !/3rd of
much higher. The higher flow rate of pro- the heat input to the bed during heating is
cess gas will cool the tower faster than the to boil out adsorbed material. The remain-
fractional flow of cooling gas. The process ing @/3rds is to heat the adsorbent and steel
fluid will be heated by the adsorbent, and in piping and the adsorber tower. The cool-
it may not meet quality specification. This ing phase only has to remove the heat that
condition lasts until the process fluid cools transferred to the adsorbent and steel.
the bed. Thus, if the flow of cooling gas is the same
It is not always necessary to com- as the flow of heating gas, the cooling time
pletely cool the entire adsorbent bed. In is about @/3rds that of the heating time.
fact, sometimes it is only necessary to cool Regardless of how long the cooling

MOLECULAR SIEVE DEHYDRATION PROCESS


36 COOLING PHASE OF REGENERATION

time is, we will never be able to completely cooling time will have to be increased, or
cool the entire bed during the cooling phase the flow of cooling gas will have to be raised.
unless the cooling gas temperature is be- Lengthening the cooling time will shorten
low the process fluid temperature. This the heating time. If the heating time cannot
means that there will always be some tem- be shortened, flow of cooling gas must be
perature rise in the outlet process fluid af- increased. This requires another flow con-
ter a regenerated tower switches to troller and selector valve in the regenera-
adsorbing. tion flow control system.
The length of the cooling period will The dual flow control system is seldom
vary with the type of plant, number of installed in adsorption plants. However, it
adsorber towers in service, and the num- is a relatively inexpensive way of indepen-
ber of towers in regeneration service. If dently controlling heating and cooling. If
there are two towers regenerating, one more heating time is required, cooling can
cooling and one heating, the cooling time be accomplished in less time by increas-
is the same as the heating time. Thus the ing the flow rate.
length of the cooling period is of primary The question at this point is: how do
concern in plants that have only one tower we know when we have the proper cooling
in regeneration service. In this case, the time and/or flow rate? The answer is: when
cooling period will equal the total regen- the outlet process fluid meets quality and
eration time less the time for heating. If the temperature limits right after a tower
regeneration time is 8 hours, and 5 hours switches from cooling to adsorbing.
are required for heating, then the cooling E. Source of Regeneration Gas
period will equal 8 - 5 = 3 hours.
The source of regeneration gas may be:
Suppose 3 hours is not long enough.
When the tower switches to adsorbing, it 1. Process outlet gas.
is hot, and the process fluid is off-spec and 2. Gas from an adjoining process facility
also has a high temperature. This condi- such as residue gas from a cryogenic
tion may be tolerable if there are two paral- plant.
lel towers in adsorption service. Half the In mole sieve plants, 99 - 100% of
product is warm and off-spec, but the total water vapor is removed from the gas, and
mixture from the two towers may be within regeneration efficiency must be 99 - 100%.
acceptable temperature and specification This requires pure gas for regeneration, so
limits. process outlet gas or pure gas from an
If the outlet process gas does not meet outside source must be used.
specifications after tower switching, the When process outlet gas is the source

MOLECULAR SIEVE DEHYDRATION PROCESS


SOURCE OF REGENERATION GAS 37

of regeneration gas, the gas leaving the or downward.


Regeneration Separator must either be dis- When a tower is regenerated, it is
posed of, or a compressor must be installed heated to boil out the adsorbed material
to boost the pressure to that of the pro- and then cooled. If regeneration gas en-
cess inlet. The pressure drop in the regen- ters at the bottom of the tower and flows
eration system is approximately 170 kPa upward, the adsorbent at the bottom of the
[25 psi]. A blower will provide this magni- tower will be the hottest, and more
tude of pressure rise when regeneration adsorbed material will boil out than from
gas from the Regeneration Separator flows the adsorbent at the top of tower. During
to the inlet gas stream. The adsorber tow- cooling, the adsorbent at the end of the
ers must contain enough adsorbent to tower that cooling gas enters will be cooled
handle the process fluid plus the flow of to a lower temperature than the adsorbent
regeneration gas, which is usually 5 - 10% at the other end.
of the process inlet stream. If the adsorption plant must remove
close to 100% of an impurity or impurities,
F. Flow Direction of Regeneration Gas
we want the process fluid to contact the
In most mole sieve plants, the main
purest adsorbent in the tower just before it
inlet gas flows downward; it enters the top
exits. Since the process fluid flows down-
of an adsorber and exits at the bottom. If
ward, the purest adsorbent should be a the
process fluid flow is upward, the adsorbent
bottom of the tower so that it can remove
might fluidize and carry out the top of the
any components that remain in the process
tower with the process outlet gas.
fluid before it exits. Regeneration gas flow
The volume of regeneration gas is
is upward in such plants.
usually a fraction of the process inlet gas
In most plants, flow of regeneration
so that it is highly unlikely that the adsor-
gas during heating and cooling is upward.
bent will fluidize from regeneration gas
However, some plants have upward flow
flowing upward through it, unless there is
of heating gas, and downward flow of cool-
surge in the regeneration gas flow rate.
ing gas.
Thus, regeneration gas can flow upward

Problem 6
During the heating phase of regeneration:
a. ______ % of the heat in regeneration gas is used to heat steel.
b. ______ % of the heat is used to heat mol sieve.
c. ______ % of the heat is used to boil water.

MOLECULAR SIEVE DEHYDRATION PROCESS


38 REGENERATION GAS FLOW CONTROL

Regeneration gas flow in plants hav- ever, it requires an additional discharge


ing a regeneration gas compressor is regu- pressure of 175 - 200 kPa [25 - 30 psi] for
lated with a flow controller on the compres- the entire outlet gas stream.
sor discharge line as shown in the flow Regeneration gas flow rate is 7.5 to
sheet on page 16. 10% of main gas flow in a 2-tower plant;
Another method of flow control is that and 5 to 7.5% in a 3-tower plant. The rea-
shown below. Gas is withdrawn from the son for the difference is that the weight of
cryogenic plant outlet gas stream. A but- adsorbent per tower in a 3-tower plant is
terfly valve in the outlet line is pinched off less than that in a 2-tower plant when each
enough to force regeneration gas to flow remove the same weight of water from a
through the plant. This eliminates the need process fluid.
for a regeneration gas compressor. How-

OUTLET GAS
TO SALES
INLET GAS

C O
O C

REGENERATION
GAS COOLER
REGENERATION
GAS SEPARATOR
3-way valve moves to VENT
position during tower switch. Liquid
to
FLOW Disposal
CONTR

F.O.
VENT

REGENERATION GAS

TOWER 1 TOWER 2
O REGEN DRYING
CRYOGENIC C
PLANT OUTLET GAS
C O
REGENERATION
GAS HEATER
FC OUTLET
Temp
Fuel Contr
Gas

MOLE SIEVE DEHYDRATOR

MOLECULAR SIEVE DEHYDRATION PROCESS


REGENERATION GAS CHANNELING 39

H. Regeneration Gas Channeling salt remains, and can cement an entire bed
When channeling occurs, the regen- into one huge lump. These lumps eventually
eration gas flows through only a portion of break down and provide big cracks, or chan-
the adsorbent. Since it is not contacting all nels, for the gas to flow through, by-passing
of the adsorbent, it will not give up as much virtually all the adsorbent.
heat as normal, and the regeneration gas Another cause of channeling is that of
outlet temperature will reach its peak be- plugging parts of the adsorbent bed with
fore its normal time. The effect of channel- adsorbent dust or fines. Some fines are
ing is that the bed will be only partially re- continuously produced as the adsorbent
generated. When it switches to adsorbing expands and contracts during its normal
service, it will not remove as much mate- heating and cooling cycle. Additional break-
rial from the process fluid, so the outlet age may occur as a result of a sudden pres-
process fluid will not meet specification, sure change, or from a sudden surge of
probably throughout all or most of the upflowing gas, or from a slug of liquid en-
adsorbing cycle. tering with the inlet gas stream. The fine
If heavy hydrocarbons enter the plant, particles can accumulate in the spaces
such as lube oil from a gas compressor, or between adsorbent particles, or they may
glycol enters from upstream treaters, coke build up on the support screen and outlet
may form during the heating phase which nozzle at the bottom of the tower. Regen-
will cement large lumps of adsorbent to- eration gas will by-pass the plugged por-
gether. As gas flows through the bed on tion of the bed.
regeneration, it by-passes the lumps, so it The effect of a bed caking or becoming
does not regenerate the adsorbent in them. plugged with fines is to isolate those portions
During adsorbing, the flow is greater, and of the bed from the flow of regeneration gas.
more gas will pass into and through the Since those portions are not being heated,
lumps. Gas that was dried in the upper the regeneration gas temperature out of a
section of the bed can actually pick up tower during the heating phase will reach its
water and become wet in passing through maximum before its normal time period. This
such lumps in the bottom of the bed that shows up on the regeneration outlet gas tem-
were not properly regenerated. perature recorder.
Salt brine can do the same thing to a One way of partially compensating for
bed. Systems that process fluids coming from gas channeling during regeneration is to
areas where there is salt water are subject increase the flow of regeneration gas. This
to carryover of the brine. During regenera- may reduce the degree of channeling, and
tion, the water in the brine boils out, but the increase the volume of adsorbent that is

MOLECULAR SIEVE DEHYDRATION PROCESS


40 OPERATION

regenerated. However, it will obviously not and remove the caked or plugged material
eliminate the cause of channeling. The per- and replace it with new adsorbent.
manent solution is to dump the adsorbent

Problem 7
Channeling is indicated by __________________________________________
_______________________________________________________________
_______________________________________________________________

V. OPERATION
A. Start-Up After Adsorbent siderable air in the pores of the adsorbent.
Replacement This can be removed by putting each bed
After towers are filled with new adsor- through a gentle regeneration. The normal
bent, the entire system will be full of air, regeneration system is used, but the heater
including the pores of the adsorbent, all of temperature controller is set to hold the
which should be removed. The individual outlet gas temperature at about 100°C
piping arrangements of each plant make [212°F]. This is hot enough to force most of
the exact air removal procedure difficult to the air out of the adsorbent, without pro-
specify. Usually, there will be several vents moting the deposit of coke resulting from
or pressure relief valves on the various hydrocarbon-oxygen reactions in the pores.
vessels in the adsorption plant. The plant During this reactivation, the regeneration
should be pressurized to 300 - 400 kPa [45 gas should be sent to the flare. This should
- 60 psi] by slowly introducing feed gas. be followed by a regeneration at normal
Then the various vent valves should be temperature.
opened in a sequence starting at the plant The exception to this type of bed de-
inlet. It will be necessary to keep introduc- aeration is if the feed gas or regeneration
ing more feed gas to maintain the pressure gas contains H2S. In that case it will be
as the various vessels are vented. necessary to find an alternate source of
When most of the air has been re- sweet gas, or purchase an inert gas to
moved, the system pressure can be al- purge the system and provide the initial
lowed to build to the operating level at a regeneration flow. This is because H2S will
rate of about 350 kPa [50 psi] per minute. react with oxygen on the surface of most
Then, the inlet line can be opened com- adsorbents. The reaction produces elemen-
pletely. At this point there will still be con- tal sulfur which will partially plug the pores,

MOLECULAR SIEVE DEHYDRATION PROCESS


START-UP 41

thus reducing the adsorbent’s capacity of a fresh bed. If these apply, they should
right from the beginning. be incorporated in the start-up procedure.
As soon as one bed has been regen- During the first few weeks, the pres-
erated it can be switched to adsorbing ser- sure drop across the outlet line filter should
vice. If the plant has 2 or more parallel be watched closely. It will probably show a
adsorbers, it will be possible to run at re- much higher than normal increase, as bits
duced flow as soon as one bed is ready. of adsorbent and dust created during the
When successive towers are regenerated, loading come through the line. It may be
inlet flow is increased. necessary to change the filter elements two
Many of these steps in start-up will or three times during the first few days.
require alteration to the normal sequenc- Then if the pressure continues to build rap-
ing for valve switches. The way this will be idly it may be a sign of failure in the bed
accomplished is dependent on the type of support system.
control system in the plant, and whether Another pressure drop measurement
the valves are manual or are automatically which should be made shortly after start-
controlled through electric or pneumatic up is that across each adsorber tower. An
drives. There are too many possible sys- increase in the pressure drop is one of the
tems to attempt a complete description in most positive means of identifying plugging
this manual. It is quite obvious, with all the or caking of adsorbent. However, in order
necessary sequencing and temperature to know if an increase has occurred, pres-
modifications involved, that an instrument sure drop measurement with new adsor-
man will be involved in any start-up. bent is necessary as a basis for compari-
If the plant is equipped with automatic son for future pressure drop readings.
valves, each one should be closely B. Routine Operation
watched during the first few cycles. Start-
One of the virtues of solid bed sys-
up seems to be the time when all the as-
tems is their ability to operate unattended
sorted junk that has been in the pipe sys-
for long periods. This tells you something
tem for years decides to settle in the valves.
about the need for routine operating
The result can be valves that do not seat
checks. However, their reputation notwith-
properly, and, if allowed to progress
standing, all plants are subject to the
through several cycles the result can be
variations in supply rate, temperature,
permanently damaged seats.
etc. The solid bed plants also have a large
Some adsorbent manufacturers have
number of valves that operate several
special precautions for the first few cycles
time each day.

MOLECULAR SIEVE DEHYDRATION PROCESS


42 ROUTINE OPERATION

1. Visual Inspection tures, pressures, flows, etc. — is of little


Following are some of the visual value unless that data is interpreted as it
checks to make: is observed. The main thing that the opera-
1. After each tower switch, check positions tor looks for is a change from the previous
of switching valves to see that each reading.
moved fully to its proper position. Valve This is not as simple as it sounds, be-
stem indicators show the position of the cause each tower in the plant operates
valve. Failure of a valve to move to its slightly differently from the others. Thus,
full open or full closed position should operating conditions on a tower must be
be corrected by stroking the valve a few compared with the conditions on that same
times. If this does not correct the con- tower during the same time in the previous
dition, the valve should be repaired or cycle in the same service.
replaced. Furthermore, if a problem develops
2. Check the heater fuel system for proper during regeneration, the effects of that prob-
pressures and reset regulators if nec- lem will not show up until that tower
essary. If a scrubber is installed in the switches to adsorption service. Thus, de-
fuel system, check the level in it to see termining the cause for a change in pro-
that liquid is dumping. cess data may require an examination of
3. Check the flame pattern in the heater data prior to the last tower switch. This
and adjust the burner air setting if nec- points out the importance of process re-
essary. corders, and of properly maintaining them.
When a change in process data is ob-
4. Check levels in the inlet scrubber and
served, the cause should be determined
regeneration gas separator to see that
and corrected before the condition wors-
liquid is dumping. Clean sight glasses
ens. Refer to Chapter VII for troubleshoot-
if they are dirty.
ing the causes of operating problems.
2. Gathering and Interpreting
Process Data
Collecting process data — tempera-

MOLECULAR SIEVE DEHYDRATION PROCESS


SUMMARY OF CAUSES OF PROCESS CHANGES 43

Following is a list of process conditions most common causes for changes in the
which should be routinely observed and the conditions.

SUMMARY OF CAUSES OF PROCESS CHANGES


CAUSE OF CHANGE IN
PROCESS CONDITION PROCESS CONDITION
Regeneration Gas Flow Rate. 1. Faulty flow control system.
2. Failure of switching valves.
Temperature of Regeneration Gas 1. Change in heater fuel gas pressure.
out of Heater. 2. Improper air setting in burners in
heater.
3. Change in regeneration gas flow.
Temperature of Regeneration Gas 1. Change in temperature of gas entering
out of Tower (heating or cooling). tower. See above.
2. Change in regeneration gas flow rate.
3. Gas is channeling in adsorbent. Adsor-
bent has broken, shifted, or solidified
from coke or salt.
4. Pressure drop is up.
Temperature of Regeneration Gas 1. Change in flow of regeneration gas.
out of Cooler. 2. Leak in cooler.
3. Cooler is plugged with adsorbent dust.
4. Change in flow of cooling fluid (air or
water).
5. Cooler is fouled on cooling fluid side.
Pressure drop through plant. Increase may be due to:
(Process fluid inlet pressure minus 1. Adsorbent breakage.
outlet pressure.) 2. Adsorbent has caked from salt or coke.
3. Switching valves plugged or partially
closed.
Decrease may be due to:
1. Bed support failure.
2. Low inlet gas rate.
Pressure drop across filter. Sudden increase indicates adsorbent
breakage which may be due to:
1. Failure of bed support.
2. Slug of liquid entered plant.

MOLECULAR SIEVE DEHYDRATION PROCESS


44 SHUT DOWN

CAUSE OF CHANGE IN
PROCESS CONDITION PROCESS CONDITION
Level in inlet gas and regeneration gas 1. Failure of level control system.
separators. 2. High level may be due to plugged or
stuck level control valve.
Fuel gas pressure to heater. 1. Faulty pressure controllers.
2. Faulty temperature control system on
heaters.
Fuel gas flow rate to heater. 1. Faulty heater temp control system.
2. Change in regeneration gas flow rate.
3. Change in temperature of gas out of
heater.
Time of tower switch. 1. Switching timer failure.
2. Switching cams on timer have moved.
Time of regeneration switch from 1. Switching cams on timer have moved.
from heating to cooling.
Quality of outlet process fluid. 1. Loss of capacity.
(Dew point, moisture content, etc.) 2. Loss of efficiency. See Chapter VII.

C. Shut Down two, it will be possible to start up again at


With the possible exception of the re- the same point in the cycle. During the down
generation gas heater, there is nothing in time the adsorbers should be isolated, by
an adsorption plant that can be harmed by closing both inlet and outlet valves. This will
sudden shut down. To make an emergency prevent moisture or other adsorbed mate-
shut down simply block in the process inlet rial from migrating from a partially loaded
fluid. If the regeneration heater is running bed to other beds in the system.
at the time of shutdown, its burner should If the shut down is to be for a longer
be shut down, or reduced to maintain a time, it should come just as the towers are
molten bed if it is a salt bath type. In some ready to switch. This way the tower that was
units, the sudden shutdown of a heater can regenerated will be fresh for the first cycle
cause damage to the refractory, so flow of of the next start up. If possible, the loaded
regeneration gas should be maintained bed should be regenerated right after the
until a safe temperature is reached. shutdown. Otherwise it should be isolated
If an adsorption plant is to shutdown during the down period to prevent migra-
for a relatively short period, like a week or tion of its adsorbed load to other towers.

MOLECULAR SIEVE DEHYDRATION PROCESS


SHUT DOWN 45

When an adsorption plant is shut of the adsorbent, some of the highly


down to dump the adsorbent, each of the toxic H2S may leave the particles very
beds should be regenerated just prior to slowly, making the area around the
shut down. This is true whether the old dumped adsorbent extremely danger-
adsorbent is to be discarded, or removed ous, or, the H2S will react with oxygen
for screening, or for maintenance on the in the air and deposit elemental sulfur
internals of the vessel. It may seem strange on the adsorbent. This will ruin the ma-
to regenerate a bed and then expose it to terial for any future use. If there is a lot
the atmosphere or throw it away. There are of H2S, there will be considerable heat
however, several good reasons for this generated by the reaction, and this in
practice: itself can create a dangerous situation.
1. Adsorbents are physically weaker when 4. Even after the regeneration, the adsor-
they are full of water. If a bed of adsor- bent from a sweetener should be
bent is dumped, and then put back in handled with extreme care. There is
the towers, it will suffer less breakage usually a considerable amount of iron
if it does not contain moisture. sulfide scale and dust in such a bed. It
2. Adsorbents will hold some heavy hy- originated in the lines and accumulated
drocarbon in their pores. When a bed in the adsorbers, which act as a filter.
is dumped without regeneration, there This material can spontaneously ignite
will be a considerable amount of hydro- when exposed to air. It not only creates
carbons which will diffuse from the par- a fire hazard, but the fumes generated
ticles over a fairly long period of time. are toxic. If this type situation develops,
During this period, the adsorbent is a the dumped adsorbent must be soaked
fire hazard. By regenerating prior to with water to reduce the danger. This
dumping, the heavier hydrocarbons are will probably mean that adsorbent from
removed and the adsorbent will hold such a system cannot be returned to
only light gases, such as methane and service, even if it was not dumped be-
ethane. These leave the particles very cause it has lost its capacity.
rapidly when the pressure is released, When an adsorber must be opened,
so the danger of fire or explosion is the unit will be depressured from line pres-
greatly reduced. sure to atmospheric pressure. This should
3. In systems that use adsorbents for sul- be done in a controlled manner, so that the
fur removal, there is a similar problem reduction is not too fast. A rate of about
with H2S. Depending on the condition 350 kPa [50 psi] per minute is usually a

MOLECULAR SIEVE DEHYDRATION PROCESS


46 BREAKPOINT TEST PROCEDURE

safe depressureing rate. If an adsorbent the adsorbed load can flash inside the ad-
that is loaded with hydrocarbons is sorbent particles and actually cause them
depressured too rapidly, the light ends in to break.

Problem 8
a. The adsorbers in a dehydration plant operate at 4200 kPa and 30°C [600 psi and
86°F]. The plant must be shut down for the replacement of the adsorbent. What is the
minimum time that should be allowed for depressuring? __________ min.
b. Why should the adsorbent in a gas dehydration plant be regenerated before it is dumped?
___________________________________________________________________

D. Breakpoint Test Procedure the hottest part of the day when the mois-
Breakpoint tests should be run on ture content of the gas is at its peak.
each tower periodically, and the adsorbing In order to run a breakpoint test, you
cycle time changed as indicated by the must be able to continuously monitor the
breakpoint test. The purpose of the moisture content of the outlet gas, and have
breakpoint test is to determine how long a the means for manually controlling the
tower can remain in adsorbing service and switching cycle.
still produce treated fluid that meets qual- The procedure to run a breakpoint test
ity specifications. Breakpoint tests must be is to allow the plant to go through its nor-
run on each tower in the plant. Although mal cycle until the heating phase is com-
each tower contains the same weight of ad- pleted. After the cooling phase commences,
sorbent and is made identically, there will lock out the tower switching mechanism so
usually be some difference in the that the towers remain in adsorbing and
breakpoint time from one tower to another. cooling service until you manually trip a
Furthermore, a breakpoint test run during switch. Suppose your plant has two towers
the night when the gas temperature and on an 8 hour cycle. The heating phase of
moisture content is lower, should give a regeneration is five hours, and the cooling
longer adsorbing time than a test run dur- phase is 3 hours. After 5 hours the heating
ing the day, when the gas temperature and phase has completed, and the regenerat-
moisture content are higher. It is best to ing tower has switched to cooling. The cycle
run breakpoint tests on each tower during switching mechanism is taken out of ser-
the same time of the day, preferably during vice so that the tower adsorbing will remain

MOLECULAR SIEVE DEHYDRATION PROCESS


BREAKPOINT TEST PROCEDURE 47

in that service until you manually trip the test the other tower to see if its breakpoint
switching cycle. The tower cooling will ob- time is also at least 10 !/2 hours.
viously remain in that service also. The breakpoint test on the other tower
After the normal 8 hour adsorbing time or towers is run when they begin adsorbing
has elapsed, you watch the moisture indica- at about the same time of the day as that
tor on the outlet gas stream until it starts to of the first tower. When all towers have been
rise. At that time, you put the switching de- tested, the adsorbing time cycle should be
vice back in service so that the towers switch changed so that it is about 0.5 hour less
in their normal procedure. You note the time than the lowest breakpoint time of all
the test started, and the time that the towers. If one tower in a 2-tower plant
breakpoint occurred. Suppose that this time tests 9.5 hours, and the other 10 hours,
period was 10 !/2 hours. At this point it ap- the 9.5 hour tower will be the control-
pears that you can increase the adsorbing ling one. The adsorbing cycle should be
time from 8 to 10 !/2 hours. However, you must set for 9.5 - 0.5 = 9.0 hours.

REGEN PROCESS
GAS INLET FLUID LINE SHADING LEGEND
OUTLET PROCESS FLUID
REGENERATION GAS

Note time tower


1 switch occurred.
REGENERATION
GAS COOLER REGEN
REGENERATION GAS Determine breakpoint time.
TEMP 4 Subtract time at step 1
GAS SEPARATOR
RECORDER from time at step 3.
LIQUID TO Repeat procedure for the
DISPOSAL 5 other tower.
When tower regenerating begins
2 cooling phase, deactivate tower
switching mechanism. TOWER 1
REGENERATING
TOWER 2
TEMP ADSORBING
CONTR
Continuously monitor moisture
3 content of treated gas. When it
starts to rise, activate tower
FUEL switching mechanism. Note time.
GAS
REGENERATION TEMP PROCESS
GAS HEATER RECORDER OUTLET FLUID
REGENERATION
GAS FROM
OUTSIDE SOURCE

BREAKPOINT TEST PROCEDURE

MOLECULAR SIEVE DEHYDRATION PROCESS


48 VI. CONTROL OF ADSORPTION PLANT

Ideal control of an adsorption plant is 3. Test at 100 cycle intervals for the next
that which results in producing an outlet 600 cycles (400 - 1000 cycles).
process fluid of specified quality at the low- 4. Test at 250 cycle intervals thereafter.
est operating cost.
The procedure for setting the
The main operating expenses of an
adsorbing time cycle after replacing adsor-
adsorption plant are:
bent is as follows:
1. The cost of periodically replacing ad-
1. Run a breakpoint test on each tower
sorbent in the towers.
after a few cycles, and set the adsorbing
2. Fuel to the regeneration gas heater.
cycle time 45 minutes less than the
The life of adsorbent will depend on tower with the shortest breakpoint time.
the number of cycles that it goes through. We previously said that the adsorbing
Each time it is heated and cooled, it loses time cycle should be 30 minutes less
some of its capacity. Consequently, the than the lowest breakpoint time. How-
longest life is obtained by minimizing the ever, during the first 250 generations,
frequency of regeneration. This is accom- the capacity of adsorbent drops rapidly.
plished by operating with the maximum The drop in capacity of new adsorbent
adsorption time period, which will reduce is equivalent to 1 - 2 minutes of
the number of regeneration periods. adsorbing time for each regeneration.
The capacity of new adsorbent is usu- After 20 regenerations, the breakpoint
ally about twice that of material that has time will be 20 - 40 minutes less than
been in service for a year or more. Refer to that of new adsorbent.
the capacity curves in Manual P-6. Thus, 2. Run breakpoint tests at the frequency
the adsorption time period for new adsor- shown above. Set the adsorbing time
bent can be twice as long as that for used cycle 45 minutes less than the lowest
material. breakpoint time during the first 250 re-
The adsorption time cycle is deter- generations. Thereafter, set the
mined from breakpoint tests. The frequency adsorbing time 30 minutes less.
of testing new adsorbent is as follows:
As the adsorbent capacity declines
1. Test at 25 cycle intervals for the first 100 with age, less material is adsorbed, so less
cycles. regeneration heat is required. Conse-
2. Test at 50 cycle intervals for the next quently, when the adsorbing time is low-
300 cycles (100 - 400 cycles). ered the heating time should be lowered.

MOLECULAR SIEVE DEHYDRATION PROCESS


CONTROL OF ADSORPTION PLANT 49

The effect of lowering the adsorbing adsorbed material, and the other @/3rds is
time cycle will be that the bed will contain used to heat the steel and adsorbent. Thus,
less moisture or other adsorbed material the heat reduction for regenerating a bed
at the conclusion of the adsorbing cycle. that contains less adsorbed material is only
Since the bed has less adsorbed material that heat required to boil out the material.
on it, less heat will be required during the The net reduction in the heating time pe-
heating phase of regeneration. You recall riod will be !/3rd of the percent reduction in
we previously said that of the total regen- the adsorbing time period.
eration heat, about !/3rd is used to boil out

Example

Adsorbent has been in service 500 cycles on a 12 hour adsorbing cycle. Regenera-
tion includes 7 hours of heating and 5 hours of cooling. Breakpoint tests after 600 cycles
indicate the adsorbing time should be lowered 1 hour to 11 hours. Determine the heating
time period at the lower adsorbing cycle time.

Present adsorbing time 12 hours

Change in adsorbing time 1 hour

1’
% change in adsorbing tine 12 x 100 = -8.25%

Present heating time 7 hours

Present heating time to boil off water 7 x !/3 = 2 !/3 hrs or 2 !/3 x 60 = 140 min

Present heating time 7 hours

8.25
Reduction in heating time 140 x 100 = 11.55 min, call it 12 min

New heating time (7 hrs) - (12 min) = 6 hrs 48 min

The above calculation is confirmed by reducing the heating time in 5 minute steps
until treated gas quality fails to meet specification. Then add 10 minutes for safety.

MOLECULAR SIEVE DEHYDRATION PROCESS


50 CONTROL OF ADSORPTION PLANT

Most plants do not optimize their lowest breakpoint time.


adsorbing time period. They have operated When the adsorbing time period is in-
on a fixed adsorbing time period since start- creased after breakpoint tests are run, the
up. Significant regeneration fuel savings are towers will contain more adsorbed mate-
often possible in such plants, particularly if rial when they switch to regeneration. More
the process inlet gas flow rate is down. regeneration heat will be required to boil
The procedure to maximize the out the additional adsorbed material. The
adsorbing time is to run breakpoint tests regeneration hating phase should be in-
on each tower; and set the adsorbing time creased !/3 of the % increase in adsorp-
!/2 hours less than the tower that had the tion time.

Example
A 2-tower plant is on an 8-hour switching cycle. Regeneration consists of 5 hours heating
and 3 hours cooling. Breakpoint tests indicated the adsorbing cycle can be increased to 12
hours. Determine the additional heating time required at the longer adsorbing cycle.
New adsorbing time cycle 12 hours
Previous adsorbing cycle 8 hours
Difference 4 hours
4
% Difference 8 x 100 = 50%
% increase in heating time 50 = 16.7%
(!/3rd % increase in adsorbing time) 3
Present heating time period 5 hours
16.7
Increase in heating time at 12 hr cycle 5 x 100 = 0.84 hrs or 50 min

Length of heating phase on 12 hr cycle 5 hrs + 50 min Call it 6 hrs


Length of cooling phase on 12 hr cycle 12 - 6 = 6 hrs

Problem 9
A 3-tower plant operates with 2 towers adsorbing for 10 hours each, and one tower
regenerating in 5 hours. Regeneration includes 3 hours of heating and 2 hours of cooling.
Breakpoint tests are: Tower 1 = 13 hrs Tower 2 = 13.5 hrs Tower 3 = 12.5 hrs
(a) Adsorbing time should be _____ hrs, (b) Heating time should ______ hrs, (c)
Cooling time cycle should be ______ hrs.

MOLECULAR SIEVE DEHYDRATION PROCESS


CONTROL OF ADSORPTION PLANT 51

The adsorbing cycle time should be flow rate is higher.


changed when there is a significant change When the adsorption time is changed
in the weight of adsorbed material enter- because of a change in gas flow rate or
ing the plant. An increase in gas flow rate moisture content, no change in the heat-
will obviously result in an increase in the ing phase of regeneration is necessary
weight of moisture or other components to because the weight of adsorbed material
be removed. However, a reduction in gas in each tower remains the same. For ex-
temperature will reduce the weight of mois- ample, if the gas temperature is reduced
ture in the gas at the same flow rate. so that the gas contains 25% less water,
An inlet gas temperature drop of a few the adsorbing time can be increased 25%
degrees in the winter months may result in and still remove the same weight of water
a reduction in moisture content of as much as it did before the gas temperature was
as 25 - 50%. The adsorbing time cycle reduced. The heating phase of regenera-
should be increased by the percentage tion will remain the same because the
reduction in the moisture content of inlet weight of water to boil off remains the same.
gas. Refer to pages 23 and 24 of Manual The other phase of ideal control is that
P-6, for the moisture content of gas at vari- of minimizing heater fuel during each re-
ous temperatures. generation cycle. A detailed procedure for
In many plants, the gas flow rate in- minimizing fuel was covered on pages 33
creases during the winter months. How- and 34. Following the procedure will result
ever, the gas is usually at a lower tem- in minimum heater fuel to boil off a fixed
perature, and the weight of moisture en- weight of water or other adsorbed material
tering the plant is lower, even though the from the bed.

Problem 10
a. The adsorbent in a 2-tower plant is replaced after 3 years. Tower switching time prior to
replacement was 8 hours. After plant start-up with new adsorbent:
1. The adsorbing time period should increase / decrease / remain the same.
2. The heating time period should increase / decrease / remain the same.
3. The cooling time period should increase / decrease / remain the same.
b. The main operating expense of an adsorption plant is ________________________..

MOLECULAR SIEVE DEHYDRATION PROCESS


52 VII. TROUBLESHOOTING

A problem occurs in an adsorption sition on the face.


plant when it does not produce a process 4. The heater is not performing as it
fluid that meets quality specification. Most should. Gas temperature out of the unit
mole sieve plants are in dehydration ser- may be below normal because fuel
vice to remove moisture from gas to a cer- pressure is low, or the burners may be
tain dew point or moisture content. The plugged. Flameouts are usually infre-
plant is not performing its job when the quent, but possible. Check the air ad-
outlet gas dew point or moisture content is justment on the burners to see that they
more than the specified point. are firing with the proper fuel-air mix-
The most obvious cause of off-spec ture.
process fluid is a problem in an adsorber 5. The regeneration gas cooler is not func-
tower. However, there are a number of tioning properly. Temperature of gas out
mechanical failures and other process of the cooler is above normal. The prob-
problems that will cause off-spec product. lem will depend on the type of cooler. If
These must be checked before the it is an aerial type, fan failure or plug-
adsorber towers are examined. They in- ging of the fins on the outside of the
clude the following: tubes should be checked. If water flows
1. The most obvious thing, and most fre- through the cooler, check its flow rate
quently overlooked, is to be sure the and temperature.
quality of outlet process fluid is off-spec, Regeneration gas flowing through the
and not a failure of the quality measur- cooler usually comes directly out of an
ing device. adsorber tower, so it will contain some
2. Tower switching valves do not fully open adsorbent dust. This will accumulate in
or close. Most valves have position in- the cooler over a period of time. An up-
dicators which show if the valve is fully set in the switching system may result
open or closed. Failure to close may be in a slug of dust entering the cooler and
caused by an accumulation of dirt or plugging it.
adsorbent in the valve. This can often 6. Flow of regeneration gas has changed.
be blown out by stroking the valve a few It may be higher or lower than normal.
times. Check the flow controller and the entire
3. Cycle controller is not functioning system for partially open switching
properly. The controller is often a clock valves.
with cams attached to the face that 7. The regenerating gas separator is not
trip a switch when the time reaches draining liquid properly. This results in
the cam. Be sure the cams have not liquid carry-over in the regeneration gas
come lose or moved to a different po- stream. If this stream flows to an

MOLECULAR SIEVE DEHYDRATION PROCESS


TROUBLESHOOTING 53

adsorber tower, it will overload it. Most normal adsorption period. The product from
of the liquid that enters the separator the plant meets specification during the first
will flow about @/3rds of the way through few hours of adsorbing, and then it goes
the heating phase. This is the time the off specification during the latter part.
separator dump system must be Sometimes the product from an
checked. If the level controller is set for adsorber will be off specification from the
a low dumping rate, the liquid level may beginning of an adsorption period. The
appear normal most of the time, when amount of contaminant removed from the
there is little or no flow of liquid to the stream is less than required. It may hap-
separator. During the short period that pen when only one particular tower is on
liquid enters at a high rate, the level will stream, or it may happen with all towers.
rise because of the restricted dumping This type of problem is the result of a loss
rate. This is when the separator must of efficiency.
be observed to see the high level, and An adsorption bed will slowly lose ca-
take corrective measures. pacity as it ages. The time when the ca-
8. Visually check for leaks or insulation fail- pacity is too low for satisfactory operation
ures, particularly on adsorber towers. is usually several years after the bed is put
After you have eliminated the above in service. There are situations when this
items as the cause for producing off-spec time may be as short as a year, but those
product, you are ready to look at the special plants are aware of the rapid aging
adsorbers to find the cause. problem, and anticipate it. As a bed of ad-
A loss of capacity is indicated when sorbent ages it does not usually lose effi-
the breakpoint occurs before the end of the ciency. Its efficiency should remain about

15 END OF NORMAL Bed with high efficiency


ADSORPTION CYCLE and capacity. Treated gas
Bed with low efficiency and high capacity. moisture content is below
Treated gas moisture content is above specified limit for the
entire adsorbing cycle; and
OF TREATED GAS, PPM

specified limit for the entire adsorption


MOISTURE CONTENT

cycle. Breakpoint occurs after normal the breakpoint is one hour


10 longer than the normal
adsorption period.
adsorbing cycle time.

Bed with high efficiency and low


5 capacity. Treated gas moisture
content is below specified limit, but
TREATED GAS SPECIFICATION the breakpoint occurs before the
end of the normal adsorption cycle.

0
0 1 2 3 4 5 6 7 8 9 10
ADSORPTION TIME, HOURS

OPERATING CURVES SHOWING EFFECT OF EFFICIENCY & CAPACITY

MOLECULAR SIEVE DEHYDRATION PROCESS


54 LOSS OF CAPACITY

the same during its entire life. bination of wells that are being produced,
So, if the capacity of a plant, or one even when all are in the same field.
tower seems to fall suddenly, or if the effi- There is usually competition for the
ciency falls off, some troubleshooting is adsorption space in the adsorbent, so that
needed. a change in capacity can occur if there is a
A. Loss of Capacity change in concentration of some mate-
Loss of capacity is indicated by the rial other than that which is being removed.
breakpoint occurring before its normal time. Methanol that is injected to prevent hydrate
When an adsorbent bed loses capacity it formation in gathering systems will com-
may be a real loss, resulting from contami- pete with water in most desiccants. So, if
nation or damage to the adsorbent; or, it the dehydrator starts to lose capacity as
may be a temporary situation which results the weather gets cold, it is a good idea to
in an apparent capacity loss. The latter is check the methanol content of the feed. The
the most common, and fortunately is the same thing can happen if the CO2 content
easiest problem to cure. Remember: increases in a system designed for H2S
adsorbents slowly lose capacity with age. removal. In either of these cases the effec-
In our discussion, we are talking about a tive useful capacity of the adsorbent has
loss of capacity before the normal loss due been reduced, but only as long as the com-
to age. peting material is present in greater than
design concentration. As soon as the com-
1. Overloading the Bed position goes back to normal the bed ca-
If it appears that a plant has lost ca- pacity should also return to normal.
pacity rapidly, particularly if the loss occurs In order to correct an overload situa-
suddenly, it may be the result of increased tion, flow of process inlet fluid must be re-
loading. Make sure the inlet gas composi- duced, or the adsorbing cycle time must
tion, or flow rate, have not increased. A rise be lowered. When the adsorbing time pe-
in inlet temperature of a few degrees can riod is reduced, the regeneration time is
result in a large increase in water content also reduced. Reducing the regeneration
of gas. Also, if the system pressure has time period will probably require raising the
been reduced, there will be an increase in flow of regeneration gas so that it will heat
the water load. Changes in temperature or and cool the bed in a shorter period of time.
pressure do not affect the H2S or CO2 con-
2. Two Phase Flow
tent. So, if the plant is removing acid com-
Adsorbers are almost always designed
ponents, the inlet gas composition should
to operate in either gas or liquid systems. It
be checked by analysis. Sometimes, the
is difficult to design a system which can
level of H2S or CO2 changes with the com-
handle mixed flow. This can be a good clue

MOLECULAR SIEVE DEHYDRATION PROCESS


LOSS OF CAPACITY 55

if the capacity in a gas treater seems to In extreme cases it may be necessary to


decline in cold weather. Check the feed insulate and heat trace the main feed line
composition and the hydrocarbon dew to prevent hydrocarbons from condensing
point. If the feed enters the adsorber at a during cold weather.
temperature below the hydrocarbon dew
3. Inadequate Regeneration
point, there will be liquid, as well as gas,
contacting the adsorbent. When this hap- Most gas dehydrators operate with an
pens the particles are coated with a layer effective capacity of 6 - 12 %. An increase in
of the liquid, and act as if they are in a liq- the residual content of the bed after regen-
uid system. eration lowers the capacity of the beds. Nor-
One of the big differences between a mal regeneration is not perfect, so there will
gas and liquid system is the rate at which usually be some residual left on the bed. It is
material is adsorbed. It is much slower in a anticipated in the design of the system, and
liquid system. If the adsorption rate slows the useful capacity is based on adsorption
down, the length of the mass transfer zone over and above the residual. If for some rea-
increases. Sometimes this increase can be son, the residual increases, it reduces the
as much as two or three meters [6 - 10 ft]. useful capacity of the adsorbent.
Such a situation can easily put most of the The regeneration system is designed
bed in the mass transfer zone and leave to provide the amount of energy to strip the
no adsorbent to remove impurities from the design load from the bed, and usually has
process fluid. The overall useful capacity little excess. Therefore, if there is a load
of the adsorbent is reduced, which results above design, as when the bed is slugged
in very short breakthrough times. This, of with liquid, or when some unanticipated
course, makes it appear as if there is a loss compound in the feed is adsorbed, the re-
in real capacity. generation may not be adequate. This can
If there is a lot of liquid in the inlet gas, result in a residual buildup, and fast capac-
it can overload the inlet separator and en- ity decline. The results of occasional slug-
ter the beds. Some plants are built with low ging will usually straighten themselves out
spots in the feed manifold. If there is a small in a few cycles. If the plant has the flexibil-
amount of condensation it will accumulate ity of control, it is wise to give such beds
in these low spots. Then, when a tower an extra high temperature regeneration or
change occurs, it will be swept into the bed. increased time on heating for a few cycles
When this is a problem, it is necessary to after the slugging.
drain the low spots just prior to each tower If the overload, and resultant inad-
change. Or, Condensation may occur in equate regeneration, is the result of co-
piping between the separator and the beds. adsorption of some compound from the

MOLECULAR SIEVE DEHYDRATION PROCESS


56 LOSS OF CAPACITY

stream, it may be necessary to perma- contaminating material from the process


nently change the regeneration conditions, stream before it enters the adsorption plant.
or even install a larger heater. This may require installation of high effi-
An increase in the residual content ciency separators to remove traces of
occurs because the bed is not heated heavy hydrocarbon or glycol mist from the
enough during the heating phase of regen- gas entering the plant. Another method for
eration to boil out adsorbed materials. The removing contaminants is to install a layer
temperature of heating gas leaving the of charcoal on top of the adsorbent to re-
tower during the heating phase of regen- move contaminating materials from the
eration will be below its normal peak tem- stream.
perature. This condition is corrected by one Once caking or plugging has occurred,
or more of the following means: it is necessary to dump the adsorbent and
1. Lengthen the time of the heating cycle. screen out the fines and/or caked portion
before reusing the balance.
2. Raise the temperature of heating gas.
3. Raise the flow of regeneration gas. a. Pressure Drop Across Adsorber
One of the best means for determin-
4. Uneven Flow of Gas Through
Adsorbent ing whether or not obstruction has occurred
is that of measuring the pressure drop
If the adsorbent becomes caked or
across the adsorber tower. The pressure
plugged, the process fluid will by-pass the
drop will obviously increase as the adsor-
obstructed portion, and the breakpoint will
bent becomes obstructed. However, a pres-
occur before its normal time. This situation
sure drop measurement is of little value
can occur from the first day of operation if
unless it can be compared with a prior pres-
the adsorbent is not properly loaded into
sure drop measurement made at the time
the tower.
new adsorbent was added to the tower.
The net effect of gas channeling is that
The pressure drop in a tower will in-
only a portion of the adsorbent actually
crease 10 - 20% a few months after filling
contacts the gas. For example, if 25% of
due to adsorbent packing. It will then level
the adsorbent is obstructed, the inlet pro-
off if no breakage or plugging occurs. Pres-
cess stream will flow through the remain-
sure drop measurements should be made
ing 75%, and will reach its breakpoint at
weekly after adsorbent is changed out un-
75% of its normal adsorbing time period.
til the pressure drop levels off. After the
Adsorbent obstruction due to caking,
pressure drop stabilizes, it should be re-
coking, or plugging usually worsens over
corded, along with the gas flow rate and
an extended period of time. The permanent
pressure in the log book or other perma-
solution to this problem is to remove the
nent records for future use.

MOLECULAR SIEVE DEHYDRATION PROCESS


LOSS OF CAPACITY 57

The pressure drop is affected by a used for calculating the pressure drop at
change in gas flow rate and/or change in various flow rate and pressures from a prior
gas pressure. The following equation is pressure drop measurement:
2
(Present Gas Flow Rate)(Prior Gas Pres)
Present Pressure Drop = (Prior Gas Flow Rate)(Present Gas Pres) (Prior Pres. Drop)

Example
The pressure drop through an adsorber after 3 months operation was 55 kPa at a gas
flow rate of 1 million m3/d and a pressure of 6.0 MPa [8 psi at a flow rate of 35 MMcf/d and
pressure of 870 psi]. A year later the gas flow rate is 1.1 million m3/d at a pressure of 5.45
MPa [flow rate is 38.5 MMcf/d at a pressure of 790 psi]. Calculate the pressure drop.

SI UNITS ENGLISH UNITS


Prior Gas Pressure 6.0 MPa 870 psi
Prior Gas Flow 1 million m3/d 35 MMcf/d
Prior Pressure Drop 55 kPa 8 psi
Present Gas Pressure 5.45 MPa 790 psi
2 2
(1.1) (6) (38.5)(870)
Subst. in Pres. Drop Equation (1.0) (5.45) (55) (35)(790) (8)

= (1.21)2 x (55) = (1.21)2 x (8)


Calculated Present Pres. Drop = 80.5 kPa = 11.7 psi

If the observed pressure drop is significantly more than the calculated pressure drop,
plugging or caking is indicated.

Problem 11
The breakpoint in a gas dehydrator occurs 1 hour before the end of the normal
adsorbing cycle. The gas flow rate is 2 million m3/d at a pressure 5 MPa [70 MMcf/d at 720
psi]. Pressure drop across the adsorber is 75 kPa [10.5 psi]. Pressure drop measurement
a year ago was 50 kPa at a gas rate of 2.2 million m3/d and a pressure of 5.5 MPa [7 psi at
a flow rate of 77 MMcf/d and a pressure 792 psi].
a. Calculated pressure drop is __________.
b. What has apparently happened? _______________________________________.

MOLECULAR SIEVE DEHYDRATION PROCESS


58 LOSS OF EFFICIENCY

B. Loss of Efficiency for the first half the adsorbing cycle, and it
Loss of efficiency in a dehydrator is goes up for the last half. This indicates part
indicated by an increase in the moisture of the adsorbent has been properly regen-
content of treated process fluid. The in- erated, and the other part has not.
crease may occur throughout the entire Regeneration of only part of a tower
adsorbing cycle, or during the latter part of occurs when:
the cycle. It may occur on one tower or all 1. The heating time cycle is not long
towers. enough.
2. Flow of regeneration gas is not high
1. Incomplete Regeneration
enough.
As we said previously, incomplete re-
3. Part of the bed of adsorbent is ob-
generation results in a loss of capacity. It
structed so that regeneration gas chan-
also reduces the efficiency of the adsor-
nels through part of the bed.
bent. In other words, the adsorbent will not
pick up as much material from the process The temperature trace of heating gas
fluid during the adsorbing cycle, and the leaving the tower during regeneration will
breakpoint will occur before its normal time indicate which of the above conditions is
period. In a dehydration plant, the moisture present. If the heating gas outlet tempera-
content of outlet gas will be high during the ture is rising at the end of the heating phase,
adsorbing cycle, and the breakpoint will and treated gas quality is bad, regenera-
occur before normal tower switch. tion gas flow rate is low, or heating time is
The loss of efficiency may be for the not long enough. Raise regeneration gas
entire adsorbing cycle or for the latter part flow in 2.5% steps, or raise the heating time
of the cycle. For example, the moisture in 5 minute steps until treated gas quality
content of treated gas meets specification is OK.

500
ENGLISH UNITS
TEMP OF REGENERATION GAS
LEAVING TOWER, °F

400
TEMP OF REGENERATION GAS

300
SI UNITS
LEAVING TOWER, °C

200 300

100 200

HEATING PHASE COOLING PHASE HEATING PHASE COOLING PHASE


0 100
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
ELAPSED TIME DURING REGENERATION CYCLE, HOURS ELAPSED TIME DURING REGENERATION CYCLE, HOURS

TEMPERATURE TRACES OF REGENERATION GAS LEAVING TOWER


WHEN HEATING TIME IS NOT LONG ENOUGH
OR REGENERATION GAS FLOW IS LOW

MOLECULAR SIEVE DEHYDRATION PROCESS


LOSS OF EFFICIENCY 59

When channeling occurs, heating gas adsorbent removes. Treated gas is the
outlet temperature rises faster than normal. source of regeneration gas in these plants.
Treated gas quality may be bad for the en- However, if the gas used for regeneration
tire adsorbing cycle. It is confirmed by high contains oxygen, even in very small
pressure drop across the tower during the amounts, it can react with hydrocarbons
adsorbing cycle. Adsorbent must be and produce water and carbon dioxide. This
dumped. reaction takes place on some adsorbents,
When the peak outlet temperature oc- which act as catalysts, and also in the tubes
curs before the end of the heating phase, of the heater, where the iron oxide cata-
and treated gas quality is bad, the tempera- lyzes the reaction. Thus it is possible to start
ture of heating gas is not high enough. with a perfectly dry regeneration gas
Raise heating gas temperature in 5°C [9°F] stream, and find that the hot gas out of the
steps until treated gas quality is OK. heater is partly wet. In most systems, there
The regeneration gas must not con- is a threshold temperature above which this
tain any moisture or other components the reaction occurs. The exact temperature will

500
ENGLISH UNITS
TEMP OF REGENERATION GAS
LEAVING TOWER, °F

400
TEMP OF REGENERATION GAS

300
SI UNITS TEMP TRACE
WHEN GAS CHANNELS
LEAVING TOWER, °C

TEMP TRACE 300


200 WHEN GAS CHANNELS NORMAL
TEMP TRACE

NORMAL 200
100 TEMP TRACE

HEATING PHASE COOLING PHASE


HEATING PHASE COOLING PHASE 100
0 0 1 2 3 4 5 6 7 8
0 1 2 3 4 5 6 7 8
ELAPSED TIME DURING REGENERATION CYCLE, HOURS ELAPSED TIME DURING REGENERATION CYCLE, HOURS

TEMPERATURE TRACES OF REGENERATION GAS LEAVING TOWER


WHEN CHANNELING OCCURS
500
ENGLISH UNITS
TEMP OF REGENERATION GAS
LEAVING TOWER, °F

400
TEMP OF REGENERATION GAS

300
SI UNITS
LEAVING TOWER, °C

200 300

100 200

HEATING PHASE COOLING PHASE HEATING PHASE COOLING PHASE


0 100
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
ELAPSED TIME DURING REGENERATION CYCLE, HOURS ELAPSED TIME DURING REGENERATION CYCLE, HOURS

TEMPERATURE TRACES OF REGENERATION GAS LEAVING TOWER


WHEN TEMPERATURE OF HEATING GAS IS NOT HIGH ENOUGH

MOLECULAR SIEVE DEHYDRATION PROCESS


60 LOSS OF EFFICIENCY

vary with the composition of the gas and indicators or by feeling piping around the
the system pressure, but it is usually above valves that are supposed to be closed. If a
260°C [500°F]. So, if this is a problem, it valve in a hot gas line is leaking, the tem-
may be necessary to hold regeneration perature of the piping on the outlet end of
temperatures in the range of 230°C [450°F] the valve will obviously be hot.
to avoid the effects of the reaction. This may If a leaking valve is discovered, it
have an adverse influence on capacity, and
should be stroked a few times to see if it
also on adsorbent life, so it should be thor-
will seat. If this does not correct the leak,
oughly studies before a lower regeneration
the valve will have to be repaired or re-
temperature is adopted.
placed.
2. Leaking Switching Valves
3. By-Passing the Adsorbent
If pressure in the regeneration system One of the most common causes of
is higher than that in the adsorption sys- loss of efficiency is that of by-passing the
tem, a leaking switching valve will result in adsorbent by some of the process stream.
some regeneration gas flowing through the It does not take much of a by-pass to result
valve into the process stream. The most in a real problem. The treated process fluid
critical leaking valve is that in the line in will be off specification for the entire cycle
which hot regeneration gas leaves the that the affected tower is adsorbing.
tower. If some of this gas leaks into the The usual cause of by-passing is that
main process line, it may result in the out- of plugged or caked adsorbent. This condi-
let process fluid not meeting quality speci- tion usually occurs over a period of time
fications. and gradually worsens. You will eventually
Leaking switching valves can usually have to dump the adsorbent and screen out
be detected by observing valve position the fines or remove caked material.

MOLECULAR SIEVE DEHYDRATION PROCESS


TROUBLESHOOTING 61

TROUBLESHOOTING CHART
PROBLEM CAUSE OF PROBLEM CORRECTIVE ACTION
Breakpoint occurs A. Bed overloaded during adsorption Shorten adsorbing cycle
before end of cycle. or reduce flow of process
normal adsorbing 1. Increase in process fluid flow. fluid.
cycle (Loss of 2. Increase in concentration of
Capacity) adsorbed component in
process fluid.
3. Increase in quantity of
competing component in
process fluid.
B. Liquid in process inlet gas stream.
1. Inlet separator not dumping Correct inlet separator
properly. level control system.
2. Condensation occurs in Heat trace inlet piping.
inlet piping.
C. Adsorbent is obstructed.
1. Adsorbent coked from glycol 1.Confirm obstruction with
or heavy hydrocarbons in pressure drop measure-
inlet gas. ment.
2. Adsorbent caked from salt 2.Dump adsorbent &
water in inlet gas. screen fines or remove
caked portion.
3. Adsorbent plugged from
fines.
D. Inadequate Regeneration
1. Heating gas temp is down. Raise gas temp out of
heater.
2. Regen gas flow is low. Raise regen flow.
3. Heating time is low. Lengthen heating cycle.
4. Regen gas contains oxygen, Lower heater outlet temp.
which reacts in heater to form
water and CO2.
Treated Process A. Inadequate Regeneration. Refer to item D above.
Fluid is off B. Leaking switching valve. Stroke valve. Repair if it
specification for will not close.
part or all of C. Process fluid by-passes some Refer to item C above.
adsorbing cycle adsorbent. Adsorbent is
(Loss of Efficiency) obstructed.

MOLECULAR SIEVE DEHYDRATION PROCESS


62 TROUBLESHOOTING CHART

Problem 12
List the symptoms of each of the following operating problems in a gas dehydration
plant.
PROBLEM SYMPTOMS
a. Slug of liquid enters with inlet gas. 1. ________________________________
________________________________
b. Bed is coked. 1. ________________________________
________________________________
2. ________________________________
________________________________
c. Temperature and moisture content 1. ________________________________
of inlet gas rises. ________________________________
________________________________

MOLECULAR SIEVE DEHYDRATION PROCESS


MANUAL P-5 VALIDATION - SI UNITS 63
MOLECULAR SIEVE
DEHYDRATION PROCESS Trainee _________________________
Operating conditions in a dehydration plant are 32° 4800 kPa
REGEN
as shown. The plant has been in service for 750 GAS
PROCESS
INLET FLUID
OUTLET 1.4 million m /d
3
days with an adsorbing cycle time of 10 hours. Heat- Moisture Content = 900 kg/million m3

ing time is 6 hours, and cooling is 4 hours. The dew 245° max

point of treated gas is -75°C. REGENERATION


GAS COOLER REGEN
1. The dew point of treated gas has been below REGENERATION GAS
TEMP
GAS SEPARATOR
the specified point. It suddenly rises 7 hours after RECORDER
Pres Drop =
LIQUID TO 60 kPa
a tower switch. What has apparently happened? DISPOSAL

–––––––––––––––––––––– TOWER 1 275°


TOWER 2
What should you do? (List 2 items) REGENERATING during
heating ADSORBING
TEMP
______________________ CONTR phase

______________________
2. A tower switch just occurred and towers are FUEL GAS

operating as shown above. Regeneration gas REGENERATION


GAS HEATER
TEMP
RECORDER
PROCESS
OUTLET FLUID
pressure is 5300 kPa. The switching valve in REGENERATION
GAS FROM
Dew Point Spec = 60
OUTSIDE SOURCE
the process gas outlet line from Tower 1 did not
fully close. How is this condition discovered?
____________________________________________________________________________________
What should you do? ____________________________________________________________________
3. The temperature of regeneration gas out of the heater drops to 250°C. List 2 effects it will have _________
____________________________________________________________________________________
4. When adsorbent is replaced in a plant,
(a) The adsorbing cycle time should be increased / reduced / remain the same.
(b) The heating cycle time should be increased / reduced / remain in the same.
(c) The cooling cycle time should be increased / reduced / remain the same.
5. During the winter, the inlet gas temperature is 24°C. Gas flow and pressure are unchanged.
(a) The adsorbing cycle time should increase / reduce / remain the same.
(b) The heating cycle time should increase / reduce / remain the same.
(c) The cooling cycle time should increase / reduce / remain the same.
6. Treated gas dew point is -75°C. During the heating phase of regeneration, the maximum temperature of gas
out of the tower occurs 1 hour before the end of the heating cycle. The regeneration gas heater is firing at 75%
of its maximum. List the sequence of steps to perform in order to minimize heater fuel.
____________________________________________________________________________________
____________________________________________________________________________________
____________________________________________________________________________________
7. How do you detect channeling during regeneration?
____________________________________________________________________________________
____________________________________________________________________________________
8. The dew point of treated gas rises to -50° for the entire adsorbing cycle on both towers. List 3 possible causes:
1. ___________________________________________________________________________________
2. ___________________________________________________________________________________
3. ___________________________________________________________________________________
9. The gas flow rate rises to 1.54 million m3/d at a pressure of 4400 kPa. The pressure drop across the towers
should be ________ kPa.
10. Breakpoint tests should be run more / less / the same frequency during the first 6 months after adsorbent
replacement than after 2 years of service.
11. Breakpoint tests show 12 hours on Tower 1 and 12.5 hours on Tower 2. Cycle times should be changed as
follows:
(a) The Adsorbing time _____ hrs, (b) The Heating time _____ hrs, (c) The Cooling time _____ hrs

MOLECULAR SIEVE DEHYDRATION PROCESS


64 SOLUTIONS TO PROBLEMS - SI UNITS

1. d 1 2. d 1 3. Time Service ’ 4. c 1
c 2 f 2 Tower 1 Tower 2 a 2
f 3 a 3 8 am Adsorbing Cooling b 3
e 4 g 4 1 pm Heating Adsorbing
b 5 e 5 9 pm Cooling Adsorbing
a 6 b 6
c 7
5. a. Raise regen heating time in 5 min steps until treated gas quality of OK.
b. Lower heating time in 5 min steps until treated gas quality just meets specification.
6. 33 a 33 b 33 c
7. Heating gas outlet temperature peaks before its normal time. High ∆P on tower. High
dew point of treated fluid.

4200
8. a. 350 = 12 min b. To boil out heavy hydrocarbons
9. a. Tower 3 has lowest breakpoint time - 12.5 hrs.
Set adsorbing cycle 1/2 hr less than it. 12.5 - 0.5 = 12 hrs
b. Percent change in heating time is 1/3rd % change in adsorbing time.
New adsorbing time = 12 hrs
Old adsorbing time = 10 hrs
Diff 2 hrs

2’
% Diff = 10 x 100 = 20%
20
% Change in heating time = 3 = 6.67%
Hrs change in heating time = 3 x 6.67 = 0.2 hrs
New heating time = 3.0 + 0.2 = 3.2 hrs
12
c. Total regen time = 1/2 of adsorbing time = 2 = 6 hrs
Cooling time = 6 - 3.2 = 2.8 hrs
10. a. 1. Increase
2. Increase
3. Increase
b. Fuel to regeneration gas heater
2 x 5.5 2
11. a. Pres. drop = 2.2 x 5 x 50 = 50 kPa
b. Observed pressure drop (75 kPa) is 50% more than that calculated. Adsorbent is
obstructed from caking, coking, or fines.
12. a. 1. Breakpoint occurs before normal time. 2. High ∆P. 3. Takes longer to heat.
b. 1. Breakpoint occurs before normal time.
2. Regen gas channels - peak temp occurs before normal time.
3. High pressure drop in tower.
c. 1. Breakpoint occurs before normal time.

MOLECULAR SIEVE DEHYDRATION PROCESS


MANUAL P-5 VALIDATION - ENGLISH UNITS 65
MOLECULAR SIEVE
DEHYDRATION PROCESS Trainee _________________________
Operating conditions in a dehydration plant 90° 800 psi
are as shown. The plant has been in service for REGEN
GAS
PROCESS
INLET FLUID
750 days with an adsorbing cycle time of 10 OUTLET 50 MMcf/d
Moisture Content = 50 lb/MMcf
hours. Heating time is 6 hours, and cooling is 4 475° max
hours. The dew point of treated gas is -100°F.
REGENERATION
1. The dew point of treated gas has been be- GAS COOLER REGEN
GAS
REGENERATION
low the specified point. It suddenly rises 7 GAS SEPARATOR TEMP
RECORDER
Pres Drop =
hours after a tower switch. What has appar- LIQUID TO 8 psi
DISPOSAL
ently happened?
–––––––––––––––––––––– TOWER 1
REGENERATING
525°
during TOWER 2
ADSORBING
What should you do? (List 2 items) TEMP heating
CONTR phase
______________________
______________________ FUEL
2. A tower switch just occurred and towers are GAS
REGENERATION TEMP PROCESS
operating as shown above. Regeneration GAS HEATER RECORDER OUTLET FLUID
REGENERATION Dew Point Spec = 80°
gas pressure is 850 psi. The switching valve GAS FROM
OUTSIDE SOURCE
in the process gas outlet line from Tower 1
did not fully close. How is this condition discovered?
____________________________________________________________________________________
What should you do? ____________________________________________________________________
3. The temperature of regeneration gas out of the heater drops to 475°F. List 2 effects it will have __________
____________________________________________________________________________________
4. When adsorbent is replaced in a plant,
(a) The adsorbing cycle time should be increased / reduced / remain the same.
(b) The heating cycle time should be increased / reduced / remain in the same.
(c) The cooling cycle time should be increased / reduced / remain the same.
5. During the winter, the inlet gas temperature is 24°C. Gas flow and pressure are unchanged.
(a) The adsorbing cycle time should increase / reduce / remain the same.
(b) The heating cycle time should increase / reduce / remain the same.
(c) The cooling cycle time should increase / reduce / remain the same.
6. Treated gas dew point is -100°F. During the heating phase of regeneration, the maximum temperature of gas
out of the tower occurs 1 hour before the end of the heating cycle. The regeneration gas heater is firing at 75%
of its maximum. List the sequence of steps to perform in order to minimize heater fuel.
____________________________________________________________________________________
____________________________________________________________________________________
____________________________________________________________________________________
7. How do you detect channeling during regeneration?
____________________________________________________________________________________
____________________________________________________________________________________
8. The dew point of treated gas rises to -60° for the entire adsorbing cycle on both towers. List 3 possible causes:
1. ___________________________________________________________________________________
2. ___________________________________________________________________________________
3. ___________________________________________________________________________________
9. The gas flow rate rises to 57 MMcf/d at a pressure of 760 psi. The pressure drop across the towers should be
________ psi.
10. Breakpoint tests should be run more / less / the same frequency during the first 6 months after adsorbent
replacement than after 2 years of service.
11. Breakpoint tests show 12 hours on Tower 1 and 12.5 hours on Tower 2. Cycle times should be changed as
follows:
(a) The Adsorbing time _____ hrs, (b) The Heating time _____ hrs, (c) The Cooling time _____ hrs

MOLECULAR SIEVE DEHYDRATION PROCESS


66 SOLUTIONS TO PROBLEMS - ENGLISH UNITS

1. d 1 2. d 1 3. Time Service ’ 4. c 1
c 2 f 2 Tower 1 Tower 2 a 2
f 3 a 3 8 am Adsorbing Cooling b 3
e 4 g 4 1 pm Heating Adsorbing
b 5 e 5 9 pm Cooling Adsorbing
a 6 b 6
c 7
5. a. Raise regen heating time in 5 min steps until treated gas quality of OK.
b. Lower heating time in 5 min steps until treated gas quality just meets specification.
6. 33 a 33 b 33 c
7. Heating gas outlet temperature peaks before its normal time. High ∆P on tower. High
dew point of treated fluid.

600
8. a. 50 = 12 min b. To boil out heavy hydrocarbons
9. a. Tower 3 has lowest breakpoint time - 12.5 hrs.
Set adsorbing cycle 1/2 hr less than it. 12.5 - 0.5 = 12 hrs
b. Percent change in heating time is 1/3rd % change in adsorbing time.
New adsorbing time = 12 hrs
Old adsorbing time = 10 hrs
Diff 2 hrs

2’
% Diff = 10 x 100 = 20%
20
% Change in heating time = 3 = 6.67%
Hrs change in heating time = 3 x 6.67 = 0.2 hrs
New heating time = 3.0 + 0.2 = 3.2 hrs
12
c. Total regen time = 1/2 of adsorbing time = 2 = 6 hrs
Cooling time = 6 - 3.2 = 2.8 hrs
10. a. 1. Increase
2. Increase
3. Increase
b. Fuel to regeneration gas heater
70 x 792 2
11. a. Pres. drop = 77 x 720 x 7 = 7 psi
b. Observed pressure drop (10.5 psi) is 50% more than that calculated. Adsorbent is
obstructed from caking, coking, or fines.
12. a. 1. Breakpoint occurs before normal time. 2. High ∆P. 3. Takes longer to heat.
b. 1. Breakpoint occurs before normal time.
2. Regen gas channels - peak temp occurs before normal time.
3. High pressure drop in tower.
c. 1. Breakpoint occurs before normal time.

MOLECULAR SIEVE DEHYDRATION PROCESS


PLP TRAINING MANUALS
NUMBER TITLE

F-1 Basic Units of Measurement


F-2 Measurement of Energy
F-3 Hydrocarbons
F-4 Fluid Flow

E-1A Centrifugal Compressors Part 1


E-1B Centrifugal Compressors Part 2
E-2 Piston Type Compressors
E-3 Centrifugal Pumps
E-4 Reciprocating Pumps
E-5 Gas Engines
E-6 Fractionators
E-7 Heat Exchangers
E-8 Indirect Fired Heaters
E-9 Pneumatic Process Instruments
E-10 LACT Units
E-11 Lean Oil Absorbers
E-12 Separators

P-1 Cryogenic Gas Plants


P-2 Glycol Dehydration Process
P-3 Contactor in Dehydration Plant
P-4 Stripper in Dehydration Plant
P-5 Molecular Sieve Dehydration Process
P-6 Adsorber in Dehydration
P-7 Crude Oil Emulsion Treating
P-8 Hydrate Inhibition
P-9 Mechanical Refrigeration
P-10 Amine Sweetening Process
P-11 Contactor in Sweetening Process
P-12 Stripper in Sweetening Process
P-13 Stabiblizing Crude Oil & Condensate

M-1 Flow Measurement


M-2 The Gas/Oil Well
M-3 Oilfield Safety

305 WELLS FARGO DR., SUITE 4 • HOUSTON, TEXAS 77090 • (281) 444-7632 • FAX: (281) 586-9876
E-MAIL: PetroLearning@aol.com

MOLECULAR SIEVE DEHYDRATION PROCESS

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