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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

stricted flow of solid particles-Le., 5 t o 10 particle diameters.


I n this instance if the gas should start to flow more rapidly
through one side of the tower than the other, the fast-flowing gas
will not be cooled as quickly by the solids. Therefore, it will have
a higher viscosity and a greater resistance to flow and will be
self-correcting for uniform flow. If the process is reversed and
the hot solids are cooled by means of a cold gas, any nonuniformity of gas flow aggravates itself because the more rapid flow of gas
through one vertical section will develop a cool path through which
abnormally large quantities of gas will flow. For the latter type
of operations, the diameter of the pilot plant should be as near
commercial size as possible.
I n a process in which a bed of granular solids is heated or cooled
by means of a li uid, the conclusions would be reversed because
the viscosity of t i e li uid decreases with increasing temperature,
the cooling step wou18 be self-correcting, and heating would give
nonuniform flow.

A parallel case can be drawn for a granular solid extraction


process with a liquid flow rate sufficiently low that pressure drop
is negligible. If the solvent becomes more dense as i t flows
through the bed the solvent automatically seeks uniformity of
density at all points at any given level in the extractor. A downflow of solvent will give uniform flow, and a very small diameter
pilot plant reactor is sufficient. If an upward flow of solvent is
used in this operation, the denser solvent at the higher level in
the extractor attempts to return to the bottom, and internal recycling and mixing result, particularly in large diameter vessels,
and pilot plant data cannot be extrapolated.
Suppose we have a process in which heats of reaction are involved. An example would be a reaction in a fixed bed of catalyst.
The magnitude of the heat effects should be estimated, and a
probable commercial design should be calculated. A pilot plant
with an adiabatic shell need encompass only one representative
full-length element of the commercial design. The pilot plant
may indicate the necessity of more or less heat transfer surface,
but when the final surface-volume relationship is established,
the diameter can be expanded to commercial size without the
necessity of building a larger pilot plant.
Most of these examples illustrate types of processes in which
one phase does not adversely affect the physical movement of a
second phase that is involved in the process. I n such processes
the equipment can usually be arranged so that either there is positive control of movement or random nonuniformity is selfcorrecting. In these processes a full-height, small-diameter, adiabatic-shell pilot plant is sufficient.
There are also many processes in which one phase adversely
influences the movement of a second phase. Examples of this
type are contact of liquid with liquid as in solvent extraction, gas

Vol. 45, No. 8

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.

An Approach to Pilot Plant Studies


J. B. MAERKER AND J. W. SCHALL
Houdry Process Corp., Marcus Hook, Pa.

HE great strides which have been made in the chemical and


petroleum industries today and which are continuing a t a
rapid pace are the result of new and improved processing methods.
These changes are brought about by demands for new products,
upgrading of existing products, and improving yields and quality
of existing products. I n addition, the motivation for improving
existing processing methods in many cases is the necessity for de-

creasing new plant investment and operating costs. Economic


pressure forces reliable proof of the feasibility of new or improved
processes and processing methods. This proof is one of the
principal functions of the pilot plant.
There are many misconceptions of the role of pilot plant studies
in the development of new or improved processes. Pilot plant
studies are carried out to obtain the necessary product yield and

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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unitized approach, one of the first steps concerns the planning


of the pilot plant design. In order to accomplish this, the problems to be solved in the pilot plant studies are divided into groups.
Each group should contain those problems that can be solved
by a single step or relatively few processing steps. Pilot plants
should be designed so that each group of problems can be studied
independently of the others, This may result in several pilot
plants, each for a different part of the process. However, this
plan results in simplification of pilot plant design, operation, and
analysis of the results. Moreover, the individual pilot plants
may be designed for greater flexibility since the design will not
be limited by the piloting operations of the other parts of the
process.
Examples Point Up Effective Use of Each Method

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

1624

INDUSTRIAL AND ENGINEERING CHEMISTRY

features of the lifting or regeneration portions of the process.


This same unitized approach was carried further in the separation
of reactor products into gas, gasoline, and gas oil cuts. Whenever
possible, the reactor effluent was not fractionated on the tower
system associated with the cracking reactor. Instead, separation
was accomplished in auxiliary distillation apparatus designed to
handle only the quantity of material necessary to obtain the required yield and quality data. This resulted in considerable
simplification of the pilot unit operation.
The reactor was designed for a relatively low throughput of
1 to 4 barrels per day. This permitted the use of small equipment and reduced the cost of the pilot plant installation. The
pilot unit was designed for a wide range of flexibility. This enabled the determination of the effects of the process variables
on the process results over ranges even beyond those contemplated for the commercial unit. The design of the pilot plant was
predicated on precise control. Accurate material balances were
essential in order to develop reliable correlations between process
variables, product yields, and product quality. The design was
also considered in the light of probable continued pilot plant
operation even aftel: the desired correlation of process data had
been accomplished. Thus, the pilot plant was available for
evaluations of different charge stocks, catalysts, or processing
schemes as required.
The pilot unit was operated at a number of conditions of space
rate, catalyst to oil ratio, temperature, and recycle ratio, The
resulting data were empirically correlated to show the interrelationships existing among the products from the cracking reaction
as well as the relationship between the process variables and
product distribution and product quality (4-6). Although the
data were obtained only with one charge stock and one catalyst,
the correlations were devised so that they would be applicable
to other charge stocks and/or catalysts b y determining the cracking characteristics of the stock or catalyst from a small number
of properly chosen pilot plant runs. These correlations not only
assist the process engineer in the design of commercial units but
also provide a basis for adjusting the operation of commercial
units to meet the individual refiners requirements.
The piloting of the regeneration step was considered from an
entirely different viewpoint from that of the cracking reaction.
As indicated, the regeneration of catalyst for the cracking unit was
accomplished in a service unit. The fundamental information
concerning catalyst regeneration characteristics which were required for kiln design were obtained more efficiently in a small
pilot unit operated independently of the cracking pilot unit.
This represented a further manifestation of the unitized philosophy of approach to pilot plant studies and resulted in a type of
study that could not have been accomplished in a unit designed to
operate in conjunction with the cracking pilot plant.
Basically, the problems in kiln design concern the amount of
regeneration gas, temperature, pressure, and kiln volume required
to effect catalyst regeneration. Consideration of the regeneration
problem indicated that the more important variables might include initial carbon content of the catalyst, initial hydrogen content, regeneration temperature, pressure, oxygen concentration
in the regeneration gas, gas velocity, and catalyst pellet diameter.
The reactions involved are simple and concern only the reaction
of oxygen with carbon and hydrogen. These considerations indicated that a fundamental study of reaction kinetics might be
used as the approach t o this pilot plant problem.
A small regeneration pilot unit operable under a wide range of
conditions was designed to determine the effect of the primary
process variables on catalyst regeneration. The unit was designed to operate under essentially isothermal conditions. Operations were conducted to establish the relationship between carbon content and burning time. The effect of each process variable was determined. Analysis and correlation of the results indicated that the primary variables in regeneration were instantaneous carbon content, reaction temperature, and oxygen partial

Vol. 45, No, 8

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

Au+

1953

INDUSTRIAL AND ENGINEERING CHEMISTRY

program was carried out on pilot unite up to 12 inches in dismeter


and 175 feet high and resulted in the evolution of reliable design
methods, the development of a nuitable control system, and the
attsinment of sttrition ratas wiihin acceptable limits.

162s

losophy of approach to pilot plant studies r d t s in the maximum


quantity of useful procese design data in a minimum of time and
with a minimum cost.
Conclusion

Visual Models Help Solve Flow Problems

As indicated before, many other problems occurred during the


development of the Houdriaow catalytic cracking process. For
example, problems relating to catalyst flow and the disengaging
of vapors from beds of solids had to be solved. Solutions to
problema of this type were developed in visual model pilot
units which were designed to scale to represent a segment of a
commercial unit. In another example, heat of cracking and regeneration values were required for the design of commercial
cracking reactors and kilns. Determination of these heat quanti&~ by actual heat balance around pilot units resulted in large
errors becsuse the heat of reaction is obtained by ditlerence from
heat quantities which have mors that rue large in relation to the
heat of reaction. Therefore, u8e was made of modem calorimetric apparatus and techniques of proved high precision to determineexperimentallytheheatof combustionof thechargeandproducte from catalytic cracking. By combining these data with
accurate sensible heat data, the heat of cracking and regeneration
were calculated directly (8). The basic approach used in planning these development programs was the same aa that hereinbefore deemibed. Experience has shown that the use of this phi-

In planning pilot plant development work, considerationshould


be given to the method of attack to obtain the solution of the
problems. Three m e t h c d e - d y , fundamental, e m p i r i d ,
and a combination fundamental-empirical-can be uaed. The
unitized concept ahould be followed in execUting pilot plant design and operation. Expdence has shown that this approach to
pilot plant studies will result in the maximum quantity of useful
infomationper unit of time or cost.
Litarotun Cited

T.A,. Dart, J. C.. Kirkbride. C. G.. Peapy. C. C.. C h .


E&?. Prov., 45, No. 2. 97 (1949).
(2) Dart, J. C., Obiad, A. G., M . ,45, No. 2. 110 (1948).
13) Dart. J. C.. S a w
- . R. T.. Kirkbride. C. G.. M . .45. No. 2. 103
(1) Burtis.

..

rn94-J).

.-__
W,

(4) Maerker.

I1 (1.51
.,I .

J. B., Sohall, J. W.. Dart, J. C:,

Bid.. 47, No. 2, 95

J. W.. Dart. J. C., Pdrolmm Refinei. 31. No.3, 101; No.


4.173 (19621.
(6)Schall. J. W.. Dsrt, J. C., Kirkbride, C. G..C h . Eng. Picm.,
45. No. 12.746 (1949).
(5)

R~mxrroforreview Anpril 15, 1953.

ACCSPTEDMay 21. 1963.

basic Factors
A. 1. CONN
Standard Oil Co. (Idhm), Whiling, I d .

ILOT plant work may be defined as small d e experimental


work &ed
out to simulate projected conditions of a commercial p r o m . The work provides information for design and
economic evaluation of a new proceas or for investigstion of
troubles or proposed changes in an existing operation. The product is manufactured only in amounts d c i e n t for evaluation.
A pilot plant is thus dktmguiihed from a memiworks unit, which
can produce quantities large enough for initial marketing. It also
differs from a bench scale unit, which is too small to simulate all
the conditions of a commercial p r o m .
The continued increase in she and cost of commercial unit8
has required more p r e c k definition of all the factors involved in
d&
and operation. As a rasult, pilot p h t work has aswmed
a role of inneasing importance in the petroleum and chemical
industries. The apecialined techniques of construction and operation have received much a h u t i o n . Very little has been written,
however, about the more basic decisions that must be faced in
every development program. when is pilot plant work warranted? What are the objectives of the work? How long should
the work be continued? Because pilot plant workisitself costly,
such basic questions must be carefully considered by all those
concerned with the tschnioal details of a project.
The major purpoee of pilot plant work is to reduce the area
of uncertainty in the design and operation of commercial unite.
The larger the area of uncertainty, the greater is the meentive
forthework Beforeanypilotplantpmgramisundert9ken,these
incentives must be weighed against the probable costs. Because

forward and as the area of uncartainty is reduced, the program


must be r d n e d at frequent intervals to determine whether
the work should continue as planned or whether emphasis should
be s i f t e d .
Pilot plant work is a v i b l connecting link between bench scale
research and manufacturing, as shown in Figure 1. To be effective, pilot plant work mnst be continually coordinated with
research, economic evaluation, procem design, engineering design,
and manufacturing. I n large industrial research organiaations,
each of these functions is usually handled by a separate group.
The pilot plant group must have a thorough underatanding of
the broad aspects of the project at all stages of the development to
e n m e proper coordination.
When Should Work Be
Undemked on Pilot Plant Scale?

certainly the most impatant decision in pilot plant work is


whether or not the project should he studied on this s d e at all.
Projects that require pilot plant work fall into two p u p : thoee
that rue desirableon the basis of current knowledge and those that
show promiee on the basis of predictions of the future. In most
cases, the time required to develop a new process through the
pilot plant, de&,
and coostruction stggeg is measured in years.
Consequently, if the need is obvious M o r e the development work
is started, the pro*
may have been started tao lata.
The most profitable ideas for development work are, there-