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I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY
with liquid as in fractional distillation, gas with solids as in fluidized catalytic cracking, or liquid with solid as in contact decolorization. I n such processes countercurrent operation cannot
be obtained directly, so we must either be content with one contact, often at a low degree of effectiveness, or resort to stage operation in which the phases are contacted, separated, and recontacted
in a countercurrent sequence, as in a bubble tray fractionation
tower or in many of the well-known liquid-liquid solvent extraction processes.
Most of these latter processes give good countercurrent operation in small diameter vessels (up to a few inches) but as vessel
diameter gets larger the results get poorer, and we begin to add
internals to direct flow. What we should realize is that a material flowing through a vessel likes to follow the easiest path, and
two phases never flow countercurrently if both have freedom of
movement; they start internal cycling or by-passing each other.
If it is decided that stage contact, separation, and recontact
will be practiced commercially, then a small pilot plant is ample.
But if for economic reasons it is desirable to build a commercial
unit in which random flow will take place, then the bigger the
pilot plant the better, because only a full commercial size will
give the final answer.
Enough examples have been given to illustrate types of processes that require only a small pilot plant and also those for which
a pilot plant can only indicate how the next larger should be built.
There is one fairly common fallacy regarding pilot plants:
this is that the pilot plant vessels should have the shape of the
proposed commercial unit. The fact that a commercial vessel,
for design reasons, might have a diameter one half its height
should have no influence whatever in establishing the shape of
the pilot plant vessels. The pilot plant vessels should be designed to duplicate commercial velocities, heat transfer coefficient, contact (residence) times, and heating or cooling surface
distribution. This does not imply that the size and shape of a
commercial vessel has no effect on the type of contact obtainable.
I n processes in which there is random movement and in which
one phase adversely affects the uniform flow of another phase,
the size and shape of a commercial vessel are very important, and
the nearest approach to countercurrent cortact or uniform contact can be obtained with tall thin vessels. However, a pilot plant
with the same shape factor must sacrifice either flow velocity,
transfer coefficients, contact time, or other critical factors, which
invalidate the data for use in commercial design.
I n summary, i t is usually good economy to build pilot plants;
and for developing a new process, a careful study of process
characteristics will reveal the size that should be built.
RECEIVED
for review April 15, 1953.
.iCCIPTED
M a y 21, 1953.
August 1953
I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY
quality data, to develop the optimum processing steps and conditions, and to obtain engineering design data applicable to
commercial plants, Pilot plants are not necessarily small replicas of the entire proposed commercial installation nor are they
necessarily replicas of individual parts of the commercial unit.
There may be many parts of a process which either cannot be or
need not be studied in a pilot plant. Some parts of a process
can be developed adequately only on a commercial scale. Careful study of the proposed process will indicate where pilot plant
work is applicable. I n the parts of the process that require
pilot plant work, the engineer should determine exactly what
individual points need clarification and design the pilot plant
specifically to obtain that information.
In this discussion it is assumed that the justification, need for,
and scope of the pilot plant work have already been established.
This discussion is directed primarily to the how of pilot plant
work. One method of approach to pilot plant studies is presented. Consideration of this and other approaches should enable industry to realize the greatest benefits from pilot plant
studies.
The approach to pilot plant studies described herein can be
termed the unitized approach, This means that the pilot
plant development work is divided into a number of basic parts or
units. Each unit is then studied individually with no interference from the other parts of the process. This philosophy is
maintained during the planning stages of development work as
well as during the design and operation of the pilot plants.
The subject matter of this presentation is made in two sections.
In the first section the methods for attacking problems which are
to be solved in pilot plant studies are described. The manner in
which both the problems and the methods used for solving them
can affect pilot plant design is discussed. The second section
presents a practical application of this approach to pilot plant
studies. The Houdriflow moving bed catalytic cracking process
has been selected to exemplify the discussions.
The Approach to Pilot Studies
M a y Be Fundamental, Empirical, or Both
Pilot plant studies can be carried out using two general methods
of attack-namely, fundamental and empirical. Certain of the
problems that mkst be solved may lend themselves readily to a
theoretical solution. If so, the pilot unit is designed to facilitate
obBining fundamental data regarding material balance, energy
balance, static equilibria, and the rates of transfer and transformation of mass and energy. The data are then correlated using
these fundamentals as a basis. However, in many instances the
mechanism of the process is so complex that pilot plant results
cannot be correlated readily solely on the basis of fundamentals.
Then, an empirical attack is often the best method of reaching a
solution to the problems, and the basic pilot plant material and
energy balance data are correlated on an empirical basis. A
third attack t o pilot plant studies comprises a combination of the
empirical and fundamental methods. I n using this combination,
the pilot plant results might first be correlated on an empirical
basis. This correlation is then modified by the application of
the fundamental attack. The result is a correlation that is
basically empirical but supported and checked by theory.
In many instances the method of attack to a specific problem
may be selected before the design of the pilot plant is started.
In some cases, however, the possibility of theoretical interpretation of the pilot plant results is not realized until after correlation
of the data has started. For this reason pilot plants should be
designed to provide as large an amount of fundamental data as
is practicable. If this is done, information will be available for
the application of any of the three methods in the correlation
of the pilot plant results.
These considerations lend themselves to the philosophy of a
unitized approach to pilot plant studies. I n executing the
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This approach to pilot plant studies can be more readily understood by considering a practical application. The following paragraphs exemplify the approach by applying it to the development
of the Houdriflow moving bed catalytic cracking process (1).
This process is applicable to the processing of all petroleum
distillate fractions for the production of high octane number
motor and aviation fuels. The processing is accomplished by
catalytically cracking the oil charge in a bed of downwardly
gravitating catalyst particles. The catalyst is regenerated with
air in a second position of the processing vessel, the kiln. Regenerated catalyst is transported to the top of the catalytic
cracking reactor vessel by means of a gas lift. It follows, then,
that the Houdriflow process can be divided conveniently into
three principal parts-namely, the catalytic cracking step, the
catalyst regeneration step, and catalyst transportation. Each of
these parts will be considered from the standpoint of pilot unit
studies.
The problems concerning the catalytic cracking step may be
divided into several classes. One phase concerns the effects of
the process variables such as space rate, catalyst to oil ratio, and
temperature on product distribution and product quality. The
effects of variables such as catalyst type and source and boiling
range of the charge stock on the process results are included in
this phase. Other classes of problems concern heat of reaction,
catalyst flow, disengaging of vapors from catalyst, distribution
of charge to the catalyst, and seal leg operation. I n line with
the unitized approach previously outlined, each of these classes
of problems was investigated in separate pilot units. For the
purposes of the present discussion only the effects of process
variables will be considered.
A considerable background of information concerning the
effects of process variables on the process results was available
from previous commercial and pilot plant operations in the
general category of catalytic cracking. However, correlations of
these data were of limited value primarily because the data did
not cover a wide range in process variables on any one particular
stock and catalyst. Therefore, a study was initiated to obtain
these data for use in the design and operation of commercial catalytic cracking units. Consideration of the complexity of the reactions involved in catalytic cracking indicated that a theoretical
attack of this part of the process would not be practical. Therefore, an empirical method was used.
The design of the pilot plant was planned to segregate the
study of the cracking reactions from studies of the regeneration
and catalyst transportation parts of the process. Regeneration
of spent catalyst from the pilot unit was handled in a separate
service unit kiln. The only data taken during regeneration
were those necessary to ensure that the catalyst was regenerated
and that temperatures in excess of those permitted for the catalyst
were not reached. The catalyst was transported to the top of the
reactor and the kiln by means of a simple lift system or hoist.
No data were taken for this operation. I n this way the study of
the catalytic cracking step was not limited by design or operating
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pressure. Burning rates were found to have second order dependency on carbon content and first order dependency on oxygen
partial pressure. The effect of temperature was found to follow
the Arrhenius equation. Comparison of the energy of activation
for the carbon-burning reaction with that for a diffusional controlled step indicated that the rate controlling step in regeneration
was actually the rate of chemical reaction. These data provided
a sound fundamental basis for the design of the kiln section of
Houdriflow catalytic cracking units ( 3 ) .
The third section of the Houdriflow process concerns solids
transportation. I n early moving bed units catalyst was transported b y elevators. This limited the quantity of catalyst that
could be circulated. It was recognized that the elimination of
the elevator limitations on catalyst circulation would result in
tremendous added flexibility to the process and in considerable
simplification to both the process and mechanical design. Consequently, the development of a simple pneumatic lift for circulating catalyst was started.
The problems involved in this development included those of
determining methods for introducing catalyst and lifting medium
to the lift and separating these materials after the required lifting
had been accomplished. A fundamental understanding of the
principles involved in gas lift transportation was needed to apply
the basic engineering data to design. I n addition, information
concerning attrition of catalyst and erosion of the materials of
construction was required. These considerations indicated that
a combination of empirical and theoretical methods in pilot plant
work probably would be necessary to develop pneumatic lifting
techniques.
It was anticipated that the lift development would progress
through several sizes of pilot units. This fact plus the consideration that circulation rates considerably in excess of those required
for the pilot unit cracking reactor and kiln would be investigated
indicated that the lift techniques should be developed in units
entirely independent of other parts of the Houdriflow system.
Thus, the unitized concept of pilot plant studies resulted in a
considerable reduction in pilot plant costs since cracking and kiln
pilot units t o utilize the catalyst circulated in the lift studies were
entirely unnecessary.
As a result of these considerations a 11j2-inchdiameter glass
lift was built and operated to study the vertical lifting of catalyst
and to develop methods for introducing catalyst into the vapor
lift and separating the catalyst from the vapor stream a t the top
of the lift. Later a 3-inch diameter lift, 30 feet in height, was
constructed. Operation of these pilot units indicated that lifting
performance was satisfactory. Sufficient information was obtained during the operation of these units to permit the design of
a larger sized pilot unit. Preliminary attempts were made to
relate the basic variables affecting the performance of gas lifts.
Preliminary catalyst attrition values were obtained and correlated
with the operating variables.
The development program was extended by the design and
operation of a pilot unit utilizing a 6-inch diameter lift which
was 175 feet high. This unit also operated satisfactorily.
Theoretical correlations based on fundamental concepts of fluid
dynamics were developed. The experimental data correlated
well with the theoretical concepts. Therefore, these correlations
formed a sound and fundamental basis for commercial lift design.
These operations extended the empirical correlation between catalyst attrition and operating variables. Additional development
work included the design and operation of a 175-foot, 12-inch
diameter lift. Results from the operation of this unit at both
ambient and elevated temperatures indicated that the d$gn
methods developed from previous work were satisfactory for the
design of commercial lifts. Catalyst attrition correlations were
extended and design changes were developed to reduce catalyst
attrition. Lift pipe erosion was found to be within acceptable
limits for commercial operation. Methods for the control of circulation rate were developed. Thus, the gas lift development
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basic Factors
A. 1. CONN
Standard Oil Co. (Idhm), Whiling, I d .