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AGITATION in PILOT PLANTS

Everett

S. Bissell, Frank D. Miller,

and Harvey

J.

Everett

M I X I N G EQUIPMENT C O M P A N Y , INC., ROCHESTER, N. Y.

I?, FOR purposes of discussion, ~e

agitation is impaired, reduced, or misM o d i f y i n g effects of small containers on mixmay define agitation as a unit operaapplied, t h e consequent. chemical
ing action are given. Minimum dimensions are
tion, we are here concerned with the
change will be affected accordingly.
shown to be related to physical characteristics
application of a unit operation t o a
For simplifying the discussion,
of materials. The pilot plant for studying agitaunit process. To be successful, such an
the general physical effect,s of agitation is contrasted with the pilot plant requiring
installation must be capable of production can be divided into the six groups
agitation for carrying on the process. General
ing the predicted or expected chemical
of Table I. However, in even a simple
design data are given for vessel shape, dimenchange or changes in the unit proceds
case, such as hydrogenation of a,
sions, variable-speed drive, horsepower range,
itself, and must be able to be varied and
vegetable oil in the presence of a finely
impeller selection, method of supporting vessel.
controlled so as to enable the optimum
divided metallic catalyst, a t least three
Photographs show several typical designs of
points in the unit process t o be achieved.
of these functions of agitation are prespilot plant. Methods are also outlined for obThe characteristics and performance
ent-namely, gas dispersion, suspension
taining quantitative data and for extending
of the agitation equipment must
of catalyst in a uniform manner, and
Dilot Dlant to commercial scale operation.
be capable of being recorded quanthe mat,ter of heat transfer t o be imtitatively so that larger scale equipproved by the circulation of the liquid
ment, for commercial size installations, can be designed from the
in the tank against the side walls or coils.
Let us assume that we are t o consider a pilot plant for a btudy
data obtained from the pilot plant operation.
I n certain cases, before the pilot plant for the unit process is
of this kind. Because of the use of hydrogen gas, it might be
set up, it will be desirable or necessary to provide a pilot plant
arbitrarily decided that the vessel was t o be kept as small as
possible. I n considering the application of a n agitator, however,
for the at,udy of agitation as a unit operation so as t,o reduce the
it would be found that the dispersion of the hydrogen gas was the
number of variables which ~ ~ o i i otherwise
ld
be necessary in the
unit process pilot plant.
most difficult or controlling factor. h type of impeller would
have to be used which would produce refinement of gas bubbles
VESSEL SIZE
and also be capable of recirculation of the supernatant gas
R-hile commercial plants for a given unit process w-ill generally
throughout the entire vessel-in other words, of providin,: the
fall Tvithin relatively narrow limits of size, capacity, etc., this,
physical conditions necessary for the chemical change. Iuadeunfortunately, is not, true n i t h pilot plants. The greatest variaquate agitation a t this point would result either in incomplete
tion in pilot plant design a t present lies in the great range of
hydrogenation or prolonged time for hydrogenation, possibly conphysical size. The term pilot plant has acquired the connotacurrent with excessive amounts of catalyst required. Data derived
tion in some quarters of miniature so that any extremely small
from such results would lead to erroneous conclusions regarding
piece of equipment, made of metal, is apt to be considered pilot
the economic factors involved and, if translated t o a large scale,
plant, equipment. I t is not rare to encounter autoclaves and rewould result in a totally inefficient commercial process.
artion vessels as small as 4 inches in diameter and 6 inches in
MINIMUM VESSEL AND IMPELLER SIZE
height. I n the absence of any guide or data which illustrate t,he
I n the pilot plant unit, it is desirable to use an impellei v,hich
difficulties to be encountered in deriving information from reis geonietrically similar to that of the full scale plant in order to
sults obtained in such small vesels, it is not surprising that the
scale-up the pilot plant results successfully. The considerations
physical size of t,he reaction vessel is most frequently decided by
needed t o be given a n impeller are: (1) the circulation pattern
ot,her factors. Consideration of materials available, safety hazin the vessel, ( 2 ) discharge velocity, (3) discharge capacity, and
ards involved, amount of room available, and disposal of end(4) a Reynolds number relation.
and by-products play an important part in size determination of
Experience has indicated that the ratio of tank diameter to
the vessel.
impeller diameter should be between 3 and 4. This ratio leaves
The purpose of t,his paper is to set, fort!h a desirable minimum
a clearance of approximately 1 to 1.5 impeller diameters between
size of reaction vessel, together with the reasons involved in arthe impeller and tank wall. I n the usual solutions (under 400
riving a t this size and the handicaps t o be expected in dealing with
centipoises) a decreased clearance of impeller to tank wall would
smaller vessels. It will be shown that, while the function of mixcause a large energy loss a t the tank wall. More clearance would
ing or agitation is primarily to produce physical changes, these
result in an insufficient velocity to create turbulence throughout
physical changes are invariably associated tvith chemical changes
the tank.
inherent in a unit process; consequently, if the physical effect of

Table 1.

BLENDIXG
MISCIBLELIQUIDS

Simple mixing of sol. liquids,


as in reducing concn.

Grouping of Agitation Functions According to Physical Effect

MIXINGI m m CIBLE

LIQCIDS

Washing of liquids
Extraction
Contacting
Emulsifying

CRYSTAL
SIZE
CONTROL
Precipitation
Evaporation systems

426

GASABSORPTIOX
AND DISPERSIOX
Hydrogenation
Aeration
Gas scrubbing
Chlorination
Gas washing

SUSPENSION
OF SOLIDE
Slurries
Suspension of filter aid,
activated C, fullern
earth, crystals while
dissolving

HEAT
TRANSFER
Heating
Cooling

May, 1945

INDUSTRIAL AND ENGINEERING CHEMISTRY

427

to scale-up mixing operations. It is


therefore believed that a condition
exists (analogous to t h a t expressed by
the law of continuity of flow) wherein
the resulting fluid velocities a t the tank
walls are substantially the same for
both the small pilot plant vessel and
the selected commercial size, the ratio
of impeller diameter to tank diameter
being maintained as stated above.
The law of continuity of flow is generally stated in the following form for
flow in nozzles and Venturis:

A1Vl = AzV2
where A = cross section area of stream
V = velocity of stream

Again borrowing from the hydraulics


theory ( 2 ) ,we find that the discharge
rate of similar pumps is proportional t o
the product of the discharge area and
the discharge velocities. I n other
words, rate of discharge for similar impellers that operate a t constant peripheral speed varies as the impeller
diameter squared. Whereas the volume
of the tank in which a n impeller
operates varies as the tank diameter
cubed, then with fixed ratios of tank
to impeller diameters, smaller tanks
should have a decreased rate of circulation. For this reason i t is necessary to
set minimum tank and impeller diameters for pilot plant purposes. It
has been difficult to obtain satisfactory
COURTESY. PATTERSON-KELLEV COMPANY, INC.
scale-up results for impellers smaller
F i g u r e 1.
Integral U n i t
F i g u r e 2.
Pilot Plant
than
4 inches in diameter. Using the
for
High-pressure
Pilot
Agitator
Equipment
with
4-inch impeller as a minimum and alP l a n t Work, Equipped w i t h
C o u n t e r b a l a n c e d Vessel S u p lowing for a ratio of tank t o impeller
A g i t a t o r a n d Special Valve
p o r t a n d A g i t a t i n g Device
diameter of 3.5, a 14-inch-diameter
vessel is found to be the minimum. For
batch size convenience, a liquid level depth of 15 inches is
This discussion leads into t h e selection of tank proportions.
selected to give a 10-gallon batch. The pilot plant vessel
When tank proportions are selected with consideration for the
should have a space allowance for splashing, foaming, volume
agitator, the selection should be based on the stream paths t h a t
increase, and overflow connection. Three inches are allowed,
give the most uniform velocity distribution. For turbine impelwhich puts the minimum pilot plant vessel as 14 inches in diameter
lers, the flow is radial from t h e impeller to the tank wall, then
and 18 inches in depth.
vertical along the tank wall t o the liquid surface and the tank
Mechanical factors which also limit the impeller diameter are:
bottom, back to the tank center, and finally to the eye of the im(1) The shaft speed becomes a factor since impellers smaller
peller. With this general flow pattern, circular patterns have
than 4 inches would have a speed of 900 r.p.m. and above; the
the least flow resistance. Square patterns are a good compromise
speed would be limited where stuffing boxes are involved and also
between the least flow resistance and the use of change of direcwhere higher speeds introduce vibration problems. (2) It betion to create turbulence. The most desirable tank shape is incomes difficult to produce a dimensionally similar impeller in
dicated as one having liquid level height equal t o the tank disizes smaller than 4 inches.
ameter.
Finally, in order t o evaluate an impeller, we use the Reynolds
There are few factual data on the discharge velocity of imnumber function S N d 2 / p ,where S is specific
pellers. Using the centrifugal pump theory as a basis (a), the
gravity, N is impeller speed in r.p.m., d is
discharge velocities are proportional t o the peripheral velocities.
impeller diameter in inches, and p is visThus, with the lack of positive velocity data, 700 feet per minute
cosity in centipoises. SNd2/pis inconsistent
has been used as a desirable peripheral velocity applied t o probas far as units of measure are concerned, but
lems of mixing immiscible liquids, gas absorption and disnersion,
they do contain the necessary dimensions of
suspension of solids, and heat transfer where turbulence is dethe classical Reynolds number. This
sired throughout the solution.
formula is useful inasmuch as i t contains the
The tendency has often been to increase the peripheral velocidimensions usually measured. This functies of impellers with increase of vessel size. This has been found
tion has been checked by plotting it as log
unnecessary. By maintaining a fixed ratio of tank diameter to
XNd2/M against log of horsepower/SNW.
impeller diameter for similar radial flow turbines, the ratio of the
The practicability of this function has been
discharge area to the flow area at the tank wall is constant for
established by a large number of tests covany size tank and impeller. By maintaining this ratio and fixing
ering a wide range of impeller types, sizes
the peripheral velocity of the impeller, it has been found possible

428

INDUSTRIAL AND ENGINEERING CHEMISTRY

Vol. 37, No. 5

F i g u r e 3. Grease o r Paste M i x i n g K e t t l e w i t h Crank


M e c h a n i s m f o r Raising o r Lowering Head, a n d Provision f o r V a r y i n g Speed a n d F u l l Selection of M i x e r
Elements
COURTESY, BUFFALO FOUNDRY

MACHINE COMPANY

and speeds, viscosity and density of fluid, and tank sizes and
baffling. Our tests have shown that this Reynolds number
function is relatively independent of the tank diameter and is
remarkably consistent for changes of impeller diameter, speed,
density, and viscosity.
This function indicates only the flow in the impeller, and is affected by factors such as tank dimensions and baffles only as they
influence the flow through the impeller. For Reynolds number
in agitation, laminar flow occurs in numbers up to 2 , a transition
between 2 and 20, and turbulent flow from 20 up. We have obtained numbers in turbulent range as high as 1,000,000. The
Reynolds number alone is no more a measure of agitation than
any other factor. It is used in the selection of a favorable diameter and speed to perform the mixing operation.
These minimum sizes of impellers and vessels should be closely
adhered to. The reaction vessel need not, necessarily, have the
same capacity of preceding or following equipment. Material
may be accumulated or stored ordinarily so that smaller or
larger equipment may precede or follow the reaction vessel.
G E N E R A L M E C H A N I C A L REQUIREMENTS

The matter of access to the interior of the vessel is of prime importance. With the weight involved in the minimum size vessel
recorded, mechanical aids should be provided. It is possible t o
design t h e vessel so that it may alternately: (1) be raised, levered, or tipped for emptying or (2) support the vessel in a fixed
position, and raise and lower the head.

Where pressure vessels are involved, there is also the option of


utilizing a top-entering or a bottom-entering mixer. The topentering mixer is best supported in a cage construction which
carries the drive well above the operators level and thus frees the
head of the vessel for the installation of connecting nozzles, sight
glasses, thermometer wells, etc. Since there will normally be
more connections in the head of the vessel than in the body or
bottom, it is generally recommended that the head remain fixed
and that the vessel be raised or lowered for access.
Where heated vessels are involved, flexible tubing or flexible
joints can be used for connections to the bottom or body of the
vessel. Such items are commercially available and in common
use.
I t is also suggested that metal equipment (not glass-lined) be
used for the first setup so that additional nozzles and connections
may easily be welded in place if found desirable. This should be
undertaken even where corrosion rates are high, wherever the
process has not been fully studied, and where changes in the vessel
design must be developed as operation proceeds.
It is recommended also that the agitator be mounted centrally
for simple transfer of data to commercial scale. Off-center positioning of mixers is most critical in small vessels and should be
avoided in pilot plant work.
It is suggested that a variable-speed drive is essential for such
work. I t is desirable t o provide as wide a speed range as possible
with constant horsepower. This enables different types of impellers to be operated a t their optimum peripheral speeds, with
horsepower kept on a comparable basis. A satisfactory speed
reducer of this type is produced by the Master Electric Company, which has a speed ratio of approximately 9 to 1. At present this must be used with a separate bevel gear reducer of 2 to I
ratio. With the vessel sizes recommended, a one-horsepower
motor is satisfactory for the drive, and will permit the handling
of a wide range of viscosities and specific gravities in the liquids
to be agitated.
If the pilot plant is expected to produce actual studies of agitafion, provision for accurate power consumption measurements
must be made. This would normally involve either supporting
the vessel so as to measure the torque transmitted ( 1 ) or use of a
differential dynamometer (3). Various speeds and consequent
horsepowers may therefore be tested as affecting the unit process
itself, and the data thus obtained utilized in dimensioning the
commercial vessel and selecting the type, characteristics, and
horsepower of the commercial size agitator.
For many operations, however, the same results can be observed by securing calibrated impellers from the manufacturer
who would be expected to provide speed DS. horsepower curve5
for the impellers in water, together with formulas for correction
factors for viscosity and specific gravity. This would require
only t h a t the type of impeller and its diameter be recorded together with accurate measurement of actual r.p.m. which should
be obtained by tachometer.
TYPICAL CONSTRUCTIONS

Figures 1, 2, and 3 are illustrations of pilot plant apparatus


involving agitation.
Figure 1 is a high-pressure vessel with a fixed-speed stirrer.
This is a self-contained and complete element, but does not,
provide facilities for variable speed or for raising or lowering
either head or vessel, etc. A special valve which does not retain
dead pockets, as illustrated, is frequently a necessity i n small

May, 1945

INDUSTRIAL AND ENGINEERING CHEMISTRY

vessels for ease in cleaning and preventing contamination of succeeding batches.


Figure 2 shows a self-supporting unit with counterbalance arrangement so that position of vessel can be changed if desired.
Space has been gained in the vessel head by using a nozzle attached at an angle instead of the customary normal entry.
The design details shown in Figures 1 and 2 can, of course, be
combined in a n over-all design which would utilize structural steel
cage support, swing joints, and flexible tubing so that the head
may remain fixed while the vessel is lowered. The support of the
vessel should be at the most comfortable height for the most
difficult function involved, including the operations of loading,
draining, cleaning, temperature measuring, sampling, and visual
observation.
Figure 3 shows a complete assembly for handling materials
similar to paste, greases, etc. Provision for raising and lowering
the mixing head is built into the equipment, and extreme flexibility is obtained by interchanging mixing elements. Speed is
apparently vaned by changing flat belt pulleys. I n connection
with handling paste, greases, eto., the choice of the mixing elements themselves is very critical. A piece of equipment, as illustrated, is extremely valuable to anyone experimenting in the
paste range of materials. In fluid mixing, however, the type of
impeller is not critical, the choice most frequently being made on a
mechanical limitations basis. Therefore, in fluid mixing it is
generally possible to equip the pilot plant with only a single
type of impeller, provided this impeller type is capable of being
scaled up to the largest anticipated commercial size, and provided
the pilot plant is designed to develop the optimum conditions
for the impeller through proper selection of size, variable speed,
and other factors noted above.
A single type or, at most, two types of impellers can be selected
Q I ~the basis of final commercial size, physical characteristics of

429

material to be handled, and over-all duty requirements of the


agitator. Only when all of these factors are unknown at the time
of designing the pilot plant is it necessary to make provision for
trying out a wide variety of impellers.
It is suggested as important that the complete pilot plant for
any unit process include, wherever possible, actual equipment
representing each unit operation essential in the unit process itself. If a pilot plant is to produce complete.results, both as to
the chemical reactions involved ahd as to a study of the mechanical equipment and factors involved, greater attention must be
placed on the mechanical equipment than appears to be common
practice. For example, many times pumps are omitted from a
pilot plant because the quantities handled are small enough to be
transferred by buckets or by gravity. Consequently, no information is available for the engineers who design the commercial
siae plant.
It has also happened that mechanical methods for a unit operation are used in pilot plant work which are incapable of scaling
up to commercial size. For example, a rocking tank producing
agitation by shaking can hardly be scaled up beyond a relatively
small batch size, owing to the massive equipment that would be
involved.
The authors do not suggest complete standardisation of that
portion of the pilot plant involving agitation. They do believe,
however, that the factors presented here are important i n unit
process pilot plant design, and it is hoped that these factors will
provide a general guide for those approaching such problems.
LITERATURE CITED

(1) Cooper, C . M., Fernstrom, G . A., and Miller, S. A., IND.EN@.

CHEM.,36, 504-9 (1944).

(2) Gibson, A. H., Hydraulics and Its Application, 4th ed., 1930.

(3) Miller, F. D., and Rushton, J. H., IND.ENQ.CRBM.,36, 499


(1944).

OXIDATION of FERROUS SULFATE


SOLUTIONS with OXYGEN
Kenneth A. Kobe and William Dickey
HE oxidation of ferrous sulfate solutions by atmoepheric
oxygen has been studied considerably by analytical chemists, who have expressed surprise at the slowness of the reaction (6). They report a variety of conflicting results, probably
arising from the differences in experimental methods. I n a physiGal-chemical study of the activation of the oxygen electrode,
Lamb and Elder (6) studied a number of variables in this reaction
and corrected many of the erroneous conclusions of earlier workers. I n general, they determined the hours required for a n oxidation of 1% of the ferrous ion a t 30 C. Their results will be compared with those obtained in this work.

UNIVERSITY

OF TEXAS, AUSTIN, TEXAS

Industrial studies of this reaction were made by Reedy and


Machin (8) who state that the initial concentration of ferrous sulfate makes little difference in the velocity of the reaction. They
secured complete oxidation by circulating the solution five times
over crushed pyrolusite. Posnjak ( 7 ) determined the hours required for oxidation of 0.1 and 0.5 N ferrous sulfate solutions at
room temperature. Agde and Schimmel ( I )
bubbled air or oxygen through ferrous sulfate solutions at various temperatures a n d
pressures.
As discussed by previous workers (7, 8),

The factors controlling the oxidation of the ferrous iron in a solution OF ferrous sulfate, ferric sulfate, and sulfuric
acid have been studied, using both oxygen and air. The percentage oxidation of ferrous sulfate is shown
here graphically on curves with respect to time, partial press!re of oxygen, temperature, acid concentration, and catalyst
concentration. The oxidation OF ferrous sulFate in acid solution by oxygen is a very difficult reaction, and good
conversions to ferric sulfate occur only at quite high temperatures and pressures over a considerable time period.