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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 I?, FOR purposes of discussion, ~e


may define agitation as a unit opera-
tion, we are here concerned with the
application of a unit operation t o a
unit process. To be successful, such an
M o d i f y i n g effects of small containers on mix-
ing action are given. Minimum dimensions are
shown to be related to physical characteristics
of materials. The pilot plant for studying agita-
agitation is impaired, reduced, or mis-
applied, t h e consequent. chemical
change will be affected accordingly.
For simplifying the discussion,
the general physical effect,s of agita-
tion is contrasted with the pilot plant requiring
installation must be capable of produc- agitation for carrying on the process. General tion can be divided into the six groups
ing the predicted or expected chemical design data are given for vessel shape, dimen- of Table I. However, in even a simple
change or changes in the unit proceds sions, variable-speed drive, horsepower range, case, such as hydrogenation of a,
itself, and must be able to be varied and impeller selection, method of supporting vessel. vegetable oil in the presence of a finely
controlled so as to enable the optimum Photographs show several typical designs of divided metallic catalyst, a t least three
points in the unit process t o be achieved. pilot plant. Methods are also outlined for ob- of these functions of agitation are pres-
The characteristics and performance taining quantitative data and for extending ent-namely, gas dispersion, suspension
of the agitation equipment must Dilot Dlant to commercial scale operation. of catalyst in a uniform manner, and
be capable of being recorded quan- the mat,ter of heat transfer t o be im-
titatively so that larger scale equip- proved 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.
data obtained from the pilot plant operation. Let us assume that we are t o consider a pilot plant for a btudy
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
for the at,udy of agitation as a unit operation so as t,o reduce the possible. I n considering the application of a n agitator, however,
number of variables which ~ ~ o i i otherwise
ld be necessary in the it would be found that the dispersion of the hydrogen gas was the
unit process pilot plant. most difficult or controlling factor. h type of impeller would
VESSEL SIZE have to be used which would produce refinement of gas bubbles
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. Iuade-
unfortunately, is not, true n i t h pilot plants. The greatest varia- quate 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 con-
physical size. The term “pilot’ plant” has acquired the connota- current 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 met’al, 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 re- would result in a totally inefficient commercial process.
artion vessels as small as 4 inches in diameter and 6 inches in
height. I n the absence of any guide or data which illustrate t,he MINIMUM VESSEL AND IMPELLER SIZE
difficulties to be encountered in deriving information from re- I n the pilot plant unit, it is desirable to use an impellei v,hich
sults obtained in such small vesels, it is not surprising that the is geonietrically similar to that of the full scale plant in order to
physical size of t,he reaction vessel is most frequently decided by scale-up the pilot plant results successfully. The considerations
ot,her factors. Consideration of materials available, safety haz- needed t o be given a n impeller are: (1) the circulation pattern
ards involved, amount of room available, and disposal of end- in the vessel, ( 2 ) discharge velocity, (3) discharge capacity, and
and by-products play an important part in size determination of (4) a Reynolds number relation.
the vessel. Experience has indicated that the ratio of tank diameter to
The purpose of t,his paper is to set, fort!h a desirable minimum impeller diameter should be between 3 and 4. This ratio leaves
size of reaction vessel, together with the reasons involved in ar- a clearance of approximately 1 to 1.5 impeller diameters between
riving a t this size and the handicaps t o be expected in dealing with the impeller and tank wall. I n the usual solutions (under 400
smaller vessels. It will be shown that, while the function of mix- centipoises) a decreased clearance of impeller to tank wall would
ing or agitation is primarily to produce physical changes, these cause a large energy loss a t the tank wall. More clearance would
physical changes are invariably associated tvit’h chemical changes result in an insufficient velocity to create turbulence throughout
inherent in a unit process; consequently, if the physical effect of the tank.

Table 1. Grouping of Agitation Functions According to Physical Effect


BLENDIXG MIXINGI m m - SIZE
CRYSTAL GASABSORPTIOX SUSPENSION HEAT
MISCIBLELIQUIDS CIBLE LIQCIDS CONTROL AND DISPERSIOX OF SOLIDE TRANSFER
Simple mixing of sol. liquids, Washing of liquids Precipitation Hydrogenation Slurries Heating
as in reducing concn. Extraction Evaporation systems Aeration Suspension of filter aid, Cooling
Contacting Gas scrubbing activated C, fuller’n
Emulsifying Chlorination earth, crystals while
Gas washing dissolving

426
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 gen-
erally 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 im-
pellers that operate a t constant pe-
ripheral 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 circula-
tion. For this reason i t is necessary to
set minimum tank and impeller di-
ameters for pilot plant purposes. It
COURTESY. PATTERSON-KELLEV COMPANY, INC.
has been difficult to obtain satisfactory
“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
for High-pressure Pilot Agitator Equipment with
than 4 inches in diameter. Using the
P 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 - 4-inch impeller as a minimum and al-
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 lowing for a ratio of tank t o impeller
diameter of 3.5, a 14-inch-diameter
vessel is found to be the minimum. For
This discussion leads into t h e selection of tank proportions. batch size convenience, a liquid level depth of 15 inches is
When tank proportions are selected with consideration for the selected to give a 10-gallon batch. The pilot plant vessel
agitator, the selection should be based on the stream paths t h a t should have a space allowance for splashing, foaming, volume
give the most uniform velocity distribution. For turbine impel- increase, and overflow connection. Three inches are allowed,
lers, the flow is radial from t h e impeller to the tank wall, then which puts the minimum pilot plant vessel as 14 inches in diameter
vertical along the tank wall t o the liquid surface and the tank and 18 inches in depth.
bottom, back to the tank center, and finally to the eye of the im- Mechanical factors which also limit the impeller diameter are:
peller. With this general flow pattern, circular patterns have (1) The shaft speed becomes a factor since impellers smaller
* the least flow resistance. Square patterns are a good compromise than 4 inches would have a speed of 900 r.p.m. and above; the
between the least flow resistance and the use of change of direc- speed would be limited where stuffing boxes are involved and also
tion to create turbulence. The most desirable tank shape is in- where higher speeds introduce vibration problems. (2) It be-
dicated as one having liquid level height equal t o the tank di- comes difficult to produce a dimensionally similar impeller in
ameter. sizes smaller than 4 inches.
There are few factual data on the discharge velocity of im- Finally, in order t o evaluate an impeller, we use the Reynolds
pellers. Using the centrifugal pump theory as a basis (a), the number function S N d 2 / p ,where S is specific
discharge velocities are proportional t o the peripheral velocities. gravity, N is impeller speed in r.p.m., d is
Thus, with the lack of positive velocity data, 700 feet per minute impeller diameter in inches, and p is vis-
has been used as a desirable peripheral velocity applied t o prob- cosity in centipoises. SNd2/pis inconsistent
lems of mixing immiscible liquids, gas absorption and disnersion, as far as units of measure are concerned, but
suspension of solids, and heat transfer where turbulence is de- they do contain the necessary dimensions of
sired throughout the solution. the classical Reynolds number. This
The tendency has often been to increase the peripheral veloci- formula is useful inasmuch as i t contains the
ties of impellers with increase of vessel size. This has been found dimensions usually measured. This func-
unnecessary. By maintaining a fixed ratio of tank diameter to tion has been checked by plotting it as log
impeller diameter for similar radial flow turbines, the ratio of the XNd2/M against log of horsepower/SNW.
discharge area to the flow area at the tank wall is constant for The practicability of this function has been
any size tank and impeller. By maintaining this ratio and fixing established by a large number of tests cov-
the peripheral velocity of the impeller, it has been found possible ering a wide range of impeller types, sizes
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 Pro-
vision 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 a MACHINE COMPANY

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


utilizing a top-entering or a bottom-entering mixer. The top-
entering mixer is best supported in a cage construction which
carries the drive well above the operator’s 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 posi-
tioning 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 im-
pellers 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 Com-
pany, which has a speed ratio of approximately 9 to 1. At pres-
ent 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.
and speeds, viscosity and density of fluid, and tank sizes and
If the pilot plant is expected to produce actual studies of agita-
baffling. Our tests have shown that this Reynolds number
fion, provision for accurate power consumption measurements
function is relatively independent of the tank diameter and is
must be made. This would normally involve either supporting
remarkably consistent for changes of impeller diameter, speed,
the vessel so as to measure the torque transmitted ( 1 ) or use of a
density, and viscosity.
differential dynamometer (3). Various speeds and consequent
This function indicates only the flow in the impeller, and is af-
horsepowers may therefore be tested as affecting the unit process
fected by factors such as tank dimensions and baffles only as they
itself, and the data thus obtained utilized in dimensioning the
influence the flow through the impeller. For Reynolds number
commercial vessel and selecting the type, characteristics, and
in agitation, laminar flow occurs in numbers up to 2 , a transition
horsepower of the commercial size agitator.
between 2 and 20, and turbulent flow from 20 up. We have ob-
For many operations, however, the same results can be ob-
tained numbers in turbulent range as high as 1,000,000. The
served by securing calibrated impellers from the manufacturer
Reynolds number alone is no more a measure of agitation than
who would be expected to provide speed DS. horsepower curve5
any other factor. It is used in the selection of a favorable diam-
for the impellers in water, together with formulas for correction
eter and speed to perform the mixing operation.
factors for viscosity and specific gravity. This would require
These minimum sizes of impellers and vessels should be closely
only t h a t the type of impeller and its diameter be recorded to-
adhered to. The reaction vessel need not, necessarily, have the
gether with accurate measurement of actual r.p.m. which should
same capacity of preceding or following equipment. Material
be obtained by tachometer.
may be accumulated or stored ordinarily so that smaller or
larger equipment may precede or follow the reaction vessel. TYPICAL CONSTRUCTIONS
G E N E R A L M E C H A N I C A L REQUIREMENTS Figures 1, 2, and 3 are illustrations of pilot plant apparatus
The matter of access to the interior of the vessel is of prime im- involving agitation.
portance. With the weight involved in the minimum size vessel Figure 1 is a high-pressure vessel with a fixed-speed stirrer.
recorded, mechanical aids should be provided. It is possible t o This is a self-contained and complete element, but does not,
design t h e vessel so that it may alternately: (1) be raised, lev- provide facilities for variable speed or for raising or lowering
ered, or tipped for emptying or (2) support the vessel in a fixed either head or vessel, etc. A special valve which does not retain
position, and raise and lower the head. “dead pockets”, as illustrated, is frequently a necessity i n small
May, 1945 INDUSTRIAL AND ENGINEERING CHEMISTRY 429

vessels for ease in cleaning and preventing contamination of suc- material to be handled, and over-all duty requirements of the
ceeding batches. agitator. Only when all of these factors are unknown at the time
Figure 2 shows a self-supporting unit with counterbalance ar- of designing the pilot plant is it necessary to make provision for
rangement so that position of vessel can be changed if desired. trying out a wide variety of impellers.
Space has been gained in the vessel head by using a nozzle at- It is suggested as important that the complete pilot plant for
tached at an angle instead of the customary normal entry. any unit process include, wherever possible, actual equipment
The design details shown in Figures 1 and 2 can, of course, be representing each unit operation essential in the unit process it-
combined in a n over-all design which would utilize structural steel self. If a pilot plant is to produce complete.results, both as to
cage support, swing joints, and flexible tubing so that the head the chemical reactions involved ahd as to a study of the mechani-
may remain fixed while the vessel is lowered. The support of the cal equipment and factors involved, greater attention must be
vessel should be at the most comfortable height for the most placed on the mechanical equipment than appears to be common
difficult function involved, including the operations of loading, practice. For example, many times pumps are omitted from a
draining, cleaning, temperature measuring, sampling, and visual pilot plant because the quantities handled are small enough to be
observation. transferred by buckets or by gravity. Consequently, no informa-
Figure 3 shows a complete assembly for handling materials tion is available for the engineers who design the commercial
similar to paste, greases, etc. Provision for raising and lowering siae plant.
the mixing head is built into the equipment, and extreme flexi- It has also happened that mechanical methods for a unit opera-
bility is obtained by interchanging mixing elements. Speed is tion are used in pilot plant work which are incapable of scaling
apparently vaned by changing flat belt pulleys. I n connection up to commercial size. For example, a rocking tank producing
with handling paste, greases, eto., the choice of the mixing ele- agitation by shaking can hardly be scaled up beyond a relatively
ments themselves is very critical. A piece of equipment, as illus- small batch size, owing to the massive equipment that would be
trated, is extremely valuable to anyone experimenting in the involved.
paste range of materials. In fluid mixing, however, the type of The authors do not suggest complete standardisation of that
impeller is not critical, the choice most frequently being made on a portion of the pilot plant involving agitation. They do believe,
mechanical limitations basis. Therefore, in fluid mixing it is however, that the factors presented here are important i n unit
generally possible to equip the pilot plant with only a single process pilot plant design, and it is hoped that these factors will
type of impeller, provided this impeller type is capable of being provide a general guide for those approaching such problems.
scaled up to the largest anticipated commercial size, and provided
the pilot plant is designed to develop the optimum conditions LITERATURE CITED
for the impeller through proper selection of size, variable speed, (1) Cooper, C . M., Fernstrom, G . A., and Miller, S. A., IND.EN@.
and other factors noted above. CHEM.,36, 504-9 (1944).
A single type or, at most, two types of impellers can be selected (2) Gibson, A. H., “Hydraulics and Its Application”, 4th ed., 1930.
(3) Miller, F. D., and Rushton, J. H., IND.ENQ.CRBM.,36, 499
Q I ~the basis of final commercial size, physical characteristics of (1944).

OXIDATION of FERROUS SULFATE


SOLUTIONS with OXYGEN
Kenneth A. Kobe and William Dickey UNIVERSITY OF TEXAS, AUSTIN, TEXAS

HE oxidation of ferrous sulfate solutions by atmoepheric Industrial studies of this reaction were made by Reedy and
oxygen has been studied considerably by analytical chem- Machin (8) who state that the initial concentration of ferrous sul-
ists, who have expressed surprise at the slowness of the re- fate makes little difference in the velocity of the reaction. They
action (6). They report a variety of conflicting results, probably secured complete oxidation by circulating the solution five times
arising from the differences in experimental methods. I n a physi- over crushed pyrolusite. Posnjak ( 7 ) determined the hours re-
Gal-chemical study of the activation of the oxygen electrode, quired for oxidation of 0.1 and 0.5 N ferrous sulfate solutions at
Lamb and Elder (6) studied a number of variables in this reaction room temperature. Agde and Schimmel ( I )
and corrected many of the erroneous conclusions of earlier work- bubbled air or oxygen through ferrous sul-
ers. I n general, they determined the hours required for a n oxida- fate solutions at various temperatures a n d ’
tion of 1% of the ferrous ion a t 30” C. Their results will be com- pressures.
pared with those obtained in this work. 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.