Scale Formation on Laborator
Evaporator
F. 31. HILDEBRANDT AND IC. H. TC'_.IRREN
1'. S . Industrial Chemicals, Inc., Baltimore, Md.
Figure 1. Laboratory Evaporator Arranged for Natural
Circulation
K E of the most serious problems to be solved in the evapora-
tion of many materials is the drop in the coefficient of
heat transfer because of the fouling of heat,ing surfaces by scale
and occluded matter. Webre and Robinson ( I ? ) give data which
show that in a n extreme case the over-all coefficient dropped,
owing t o scale formaeion, from 1550 to 900 in less t h m 2 hours
and then less rapidly to about 700. Other dat,a showing t h e
heat transfer t o boiling liquids under varied conditions may be
found in the literature ( 7 , 9, 10, 12, 16). The majority of these
studies have been confined to plant scale equipment,. Labora-
tory data are difficult t o find arid are, in general, limited t o t'he
investigation of a specific factor such as the film coefficient.
This is due in part t,o the fact t h a t small scale equipment for
evaporation studies is specialized for t,he study of these specific
factors and in part to t,he feeling that laboratory apparatus is too
far removed in size and operating conditions t,o give data valid
for t,he larger evaporators. To experiment with full scale
evaporators, however, is costly. illso such eyuiprrienl lacks
flexibility, the machine is difficult to examine after use, and ex-
perimentation under production conditions is hard to interpret,
a,s the uncontrollable factors of t h e larger operation affect the
results erratically.
JVith those things in mind attention vas turned t o the setting
up of a small evaporator for laboratory studies of scale formatmion.
Certain requirements for such an apparalus have been suggested
by other workers ( 2 , 3,11, 18, 1 4 ) among which are the following:
The apparatus should be designed t o evaporate small amounts
of material under controlled conditions with t'he heat transfer
tube constructed so that t,he scale forms on the outside where it
can be observed readily.
It should be taken apart easily for ohsrivation or nieaiurement
of the scale on t h e tube surface.
Xeasurenient of scale formation by change in evaporation rate
should be made easily.
DESCRIPTIO\ O F APPARATUS
;1photograph of the appaiatub is shown in Fiyurc I il is t h e
body of the evaporator constructed froin a 500-ml. Kjeldahl
flask by adding a section to the neck and providing an outlet in
the bulb and another outlet in thc neck about 1 inch from the
bottom. B is another 500-ml. Kjeldahl with a tangential inlet,
two outlets, one foi a thermonietei and the other near the top
for vapor. The nccli of this flaqk is shortened and drawn down t o
a reduced diameter for attachment of rubber tubing. C is a
glass manifold with four outlets, interchangeably usrd for in-
coming feed, E , down-leg connection from B , or draining the
apparatus. A , B, and C are connected by rubber tubing. G
is a graduated receiver for water from R. condensed by bulb
condenser, D. F is a graduated separatory funriel lor holding
the feed and maintaining a supply at constant level in pump
reservoir iV. Steam a t constant pressure enters the apparatus
through regulator H . T h e gage, I , gives the pressure on the
heater tube, and the condensate is removed by steam trap, K .
The temperature of the steam is measured by a Weston thermom-
eter, L. J1 is a braided metallic hose which admits steam t o
the 0.5-inch brass evaporator tube, T . X is a rubber stopper
fitted over tube T and into the neck of A . 0 is a steam trap
connected t o a 0.125-inrh copper capillary tube within tube T,
and drained by condensate discharge line P. Details of the oon-
struction of the heater are shown in Figure 2. The con-
struction and operation of feed pump R arc described in a pre-
vious publication (6). It consists of a rubber tube provided
with stainless steel ball check valves. Pumping action is ob-
tained by compressing the tube with a bar moved by means of ek
motor-driven cam.
OPERATION O F EVAPORATOR
In actual operation, the evaporator is filled to the desired levd
and the steam inlet valve opened. I n about 1 minute the liquid
boils and circulation starts through the apparatus. From B,
the catchall, the vapor goes to the condenser, D,and the oon-
densate is caught in a 100-ml. graduated cylinder. I n these
experiments readings of the amount of condensate were made
a t 5-minute intervals and the data obtained were used for plot-
ting curves shown later in this paper. The liquid level is main-
tained relatively constant in the catchall (within about I inch)
simple and easily constructed laboratory apparatus
designed for the study of evaporator scale formation is
described. Results are presented graphically to show the
decrease in the rate and amount of water cvaporated under
controlled conditions as a coating of scale is formed on the
heater tube, Experiments with calcium sulfate solutions
and molasses stillage are described, and some of the more
important factors affecting scale formation are empha-
sized. The apparatus is used to produce small amounts
of evaporated material experimentally in the laboratory,
in addition to its principal use as a tool for the investiga-
tion of the effect of various factors on scale fortnation.
April 1949 INDUSTRIAL AND ENGINEERING CHEMISTRY
~‘O.D.COPPERTUBNG
RUBBER STOPPER
BRASS HEX. NUT BRAZED
T O B R A S S TUBE
COPPER CAPILL
BRAZED TO BUS OSE
/ BRA% TEE
CONDENSATE
T O SEWER
Figure 2. Heater Cross Section Showing Tube Assembly
and Steam Connections
by regulating the output of the feed pump. Saturated plant
steam previously reduced to 15 pounds is fed to the regulating
valve and a temperature of 238” F. is maintained on the steam
side of the heater tube by adjustment of t h e steam pressure
regulator. Steam enters the tube at the bottom apd the con-
densate leaves the system through t h e copper capillary tube
shown in Figure 2 connected with a steam trap. During t h e
course of the runs, as scale forms, the amount of water dis-
charged from the condenser decreases. The most marked drop i n
evaporation rate occurs when scale can be seen crystallizing on
the tube surface. At the end of each run the evaporating tube is
removed by disconnecting the rubber tubing from the outlets of
the evaporator body A , and unscrewing the tube from the tee
in which it is held. hleasurements of scale formed and observa-
tion at close range with the naked eye or under a stereoscopic
microscope can be made readily.
r , I I I
. . RUN Nl NG
Figure 3. Left. Typical Curve Obtained by Evapora-
tion of Calcium Sulfate Solutions. Right. Decrease in
Initial Evaporation Rate with Ethyl Stillage from High
Ash Molasses
Stillage from fermentation maah : 1, without acid and backslopping;
2, with eiilfiiric acid and n o hackalopping; 3, with hnckslopping
but no acid; 4, duplicate of 3 with 100 p.p.m. tetrnphoaphoqluco-
sate ndded to stillage
755
OPERATION OF EQUIVMEVT
This type of evaporator has a number of advantages. It is
constructed of standard material readily obtainable by any
laboratory. T h e glass body permits visual observation of t h e
tube with lightly colored solutions and scale formation can be
observed a t t h e moment deposition starts. T h e evaporator
can be readily taken apart for cleaning and inspection of the tube
surface. With minor changes, it c a n be converted t o the forced
circulation type. The apparatus is sinal1 enough t o be sup-
ported on a rack on the laboratory table. T h e feed may be
introduced a t any one of several places t o give thorough mixing
of the cold feed before i t reaches the tube surface. K i t h slight
modifications it lends itself t o orthodox methods of heat transfer
study. A further advantage is its use for evaporating small
amounts of solutions experimentally under conditions which
make for a minimum of heat injury. T h e unit can also be used
for continuous evaporation.
DETERMINATION O F EVAPORATION CAPACITY OF CLEAN TUBE
As a preliminary t o the study of evaporator performance,
tests were made on the clean tube with water. Other investi-
gators have shown that it is difficult t o clean a scaled tube surface
so as t o bring its heat transfer capacity back t o the original
value (16). Tubes for the experiments described here were
cleaned by several methods such as bufing with a scratch wheel
and hand polishing with emery cloth (size 3/0). The latter
method gave results which checked closest when water was
evaporated and this was chosen as a standard procedure. JVith
water the rates of evaporation of the tubes used in these experi-
ments varied between 16.2 and 17.6 ml. of water per minute
under the test conditions.
Figure 4. Typical R u n with Calcium Sul-
fate Solution Showing Formation of Scale
on Brass Heater Tube
PRELIMINARY STUDIES OB CALCIUM SULFATE
T o throw light on the basic problems of scale formation and
prevention, experiments were first carried out with calcium SUI-(
fate solutions, this salt being chosen because it is one of t h e
prime scale formers in the evaporation of many solutions. T h e
solution also permits visual observation of the tube surface and
the low solubility of the salt minimizes the effect of viscosity.
Likewise, calcium sulfate has a n inverted solubility curve which is
a n essential requirement for scale formatiol! ( 2 , 4 ) . Solutions were
made by dissolving 2 grams of desiccated calcium sulfate in
1 liter of water at room temperature, shaking the flasks about .
every E, minutes for half a n hour, and then filtering.
The evaporator was started on water, and calcium sulfate
solution was then fed a t such a rate that a constant level in t h e
catchall was maintained, keeping steam pressure and tempera-
ture constant. Figure 3 (left) is a graphic representation of a
typical run. When 1000 ml. of calcium sulfate solution had been
fed, scale could be seen forming on the tube, this point corre-
sponding t o 60 minutes of running time. A sharp drop in evapora-
tion rate occurs a t this time and continues for another 60 minutes,
a t which point the rate continues to fall off more slowly. In such
 756 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
Figure 5 . Tatal Condensate Collected O + ~ I
4-Ilour Kunning Time
Aboae. 1, Cas04 solution untreated: 2, C a s 0 1feed
with 100 p.p.m. cornstarch; 3, CaSOa feed with 100
p.p.m. Calgon; 4 CaSOa feed, tubc coated with a
resin. Below. 1, ' CaSOa solution untreated; 2,
Cas04 feed treated 100 p . p . m . Tetrafosforg; 3.
Cas04 feed treated with 100 p.p.m. tetraphospho-
glucosate; 4, CaSOi feed, tube precoated with ran-
delilla wax and feed treated with 100 p.p.m. tetra-
phosphogluooaate
experiments, the tube removed a t the end of 4 iiouiq iilvaliabl)
shows a heavy coating of scale, ab can be seen by Figure 4.
Figure 3 (left) shows the result graphically in terms of evapora-
tion rate. In this curve evaporation rate is exprewed as per-
centage of the initial rate on water.
METHOD Ok EXI'HESSING TEST RESULTS
- Results have been expressed graphically in two J I L ~ J Yusing
data obtained from the amount of water evaporated over 5-
minute intervals, Since the principal criterion for evaporator
performance is the amount of water evaporated from a given
solution in a definite period ( I ) , the cumulative quantity for e:tch
half-hour or hour has been plotted against running time. This
type of graph has been used in Figure 5 (above). Ordinarily
this method gives an easily interpreted graph. Hon-ever, with
some solutions containing large amounts of dissolved solids, in-
crease in viscosity and rise in boiling point, as the solution con-
centrates, lower the amount of Rater evaporated, if steam pressure
Vol. 41, No. 4
on the heater is maintained constant. This gives curves in which
the control and experimental values lie close together, By
raising the steam pressure or using a tube of larger area the
points can be separated arid coildensate values obtained which
correlate with the observed scale formation on the tube surface.
A second method of expressing results, based on the water
evaporated, s h o m the rate a t which evaporation falls off. 111
this case, t.he amounts of condensate collected in successivc.
d a,s percentage of initial evaporation rate
et'hod takes into account the initial condition
of the tube and shows the progress of scale forniation during the
course of t'he run. This type of graph is shown in Figure 3 (left),
C,urve 1, Figure 6 (above) is characteristic of thc cvaporatiori
rate of an untreated calcium sulfate solution, while the bent?-
ficial results of adding starch or Calgon are illustrated by curves
2 and 3. Thcre is a slight decrease in the evaporation shown t)y
n 60 and 90 minutes of running time which 00-
incided n-ith heavy scale forrriat,ioii, but the period betrvertn 90
arid 120 minutes shows an increase in rate owing to a desc:diirg
effect of the starch (8). While it vias hoped that the tube wvoiald
become completely descaled, t,his did not occur and simultarirou$
scaling and descaling continued with less descaling as the run
progressed. The data for curve 4 were obt,ained from a tube
coated with a resin. This tube showed a scaling and descaling
effect as when starch was present and the run vas contiiiued for
10 hours, during which time the rate of evaporation would first
fall off as scale formed and then rise again as descaling took place
(results from only the first 4 hours arc shown on the graph).
Thrce coats of Bakelite varnish were used t o coat this tube and
consequently its rate of evaporation was less than half of a normal
average. As the scale was sloughed off, the tube maintained its
rate of evaporation. Curve 1 of Figure 5 (below) shows the con-
densate produced during a 4-hour run from a calciuni sulfate
solution. Curves 2 arid 3, Figure 5 (below) show results of
adding commercial scale preventives to calcium sulfate solutioris.
Curve 4 shows a remarkable increase in the amount' of water
evaporated by coating the tube with wax before introducing
liquid and then adding 100 p.p,m, of tetraphosphoglucosate to
the calcium sulfate. h preliminary experiment with wax alone
showed little or no improvenfeiit except t o give a n easily reniov-
able scale. Scale observed visually on t,he tube a t the end of
r u n after removal from t8he npparatus showed that starch and
c~aritlelillawax coatings with or without tetraphosphoglucosate
(6) gave a nonadherent scale easily removed by light fingor
pressure. Results from t,he other tests gave a n adherent scale
which had t o be sanded off with emery cloth. R7hi1r visu:ti
Figure 6. Comparison of Clean Tube with
Lightly Scaled Tube after 4-Hour Run w-ith
High Ash Stillage from Fermentation with
N o 4cid arid No Bacldopping
April 1949 INDUSTRIAL AND ENGINEERING CHEMISTRY
Figure 7. R u n with High Ash Stillage
Where Sulfuric Acid Had Been Used i n
Wash Make-up
Figure 8. Comparison of Clean Tube with
Tube Scaled Heavily by Evaporation of High
4sh Stillage from Fermentation Where
Stillage Had Been Used as Part of Mash
Make-Up
observation of the amount and thickness of the scale coating
tallied with the results as expressed graphically, t h e weight of
the scale could not be correlated with these results. This is no
doubt a result in part of the type of crystals formed. Examina-
tion of t h e coatings under a stereoscopic microscope showed that
various treatments changed the crystal size and shape and also
altered the amount of unscaled tube area between crystals.
EVAPORATION O F STILLAGE FROM. YEAST FERMENTATION OF
BLACKSTRAP MOLASSES
The evaporation of stillage from dealcoholized fermentation
solutions presents many problems, and the hope of casting some
light on these was one of the principal reasons this work was
undertaken. Variation in rate of evaporation, not explainable
by any obvious condition in the evaporators, is a common ex-
perience in distilleries. When malasses is the raw material,
very serious operational difficulties arise with certain shipments.
.4t such times frequent cleaning is necessary, which is expensive
and results in loss of operation time. I n extreme cases the evap-
orator heads have t o be removed and the hard scale drilled out
of tubes in t h e heater section of the evaporator.
Experimentation on the factors responsible for scale formation
could be oriented t o some extent by drawing on experience with
plant evaporators. It was known t h a t the scale is primarily a
calqium sulfate deposit, sometimes also a mixed calcium-potas-
sium salt; t h a t the amount deposited is affected by the ash con-
tent of the molasses, being greater when the ash content is high;
and i t was ,suspected t h a t there might be some aggravation of
scale formation b y physical conditions in the heater section of the
evaporator. Experiments were set up, therefore, t o answer the
following questions on the effect of chemical and physical condi-
tions on scale formation.
1. .Could scaling be produced by adding a soluble calcium
salt to a nonscaling stillage?
2. Does the sulfate radical affect scaling?
3. Does scaling increase when stillage is used as a mash
ingredient? (This is the common practice of backslopping.)
4. Does forced circulation decrease scaling?
5. Is foam in t h e heater section related t o scale formation?
757
EFFECT O F ADDING SOLUBLE CALCIUM SALT
h sample of stillage found in plant operation t o be nonscaling
was evaporated in the apparatus and no scale was formed after
4 hours of operation. Calcium chloride was added and the
experiment repeated. I n both cases there was a gradual de-
crease in rate which was due t o the increase in viscosity of the
solution. However, t h e heater tube remained clean in both
experiments. Potassium chloride was then added t o t h e same
stillage and again the tube remained clean. These experiments,
which were repeated several times, showed t h a t t h e soluble
calcium salt did not increase scaling and also t h a t an increase in
the potassium ion was without effect.
ADDITION OF SULFATES
Stillage giving no scale in plant operation was saturated with
potassium sulfate at 25" C. Evaporation of the untreated
stillage showed no scale formation, but t h e same material con-
taining potassium sulfate gave scaling. I n this case the scale
was light and occurred in patches. A sample was prepared by
saturation with potassium sulfate at 70' C. Evaporation of
this sample resulted in a heavy coating of scale evenly dis-
tributed over the entire length of the heater tube. -4second
lot of stillage which was nonscaling was treated with sulfuric
acid. Here again, scaling was heavy as compared with the con-
trol. It appears from these experiments t h a t sulfate added
either as potassium sulfate or sulfuric acid aggravates the scaling
tendency.
B 4CK S LOPPING
A sample of stillage resulting from the fermentation o f a
molasses high in ash which had given heavy scale in plant equip-
ment was evaporated in the apparatus, This stillage could be
evaporated in the laboratory evaporator without scale formation
over a 4 h o u r run. However, when sulfuric acid was added, espe-
cially heavy scaling took place, either with or without backslopping.
Backslopping alone gave moderate scale formation. I n general,
the scaling was heavier with this sample than with stillage which
gave no plant difficulties, although additions as noted above
were necessary t o bring out the scaling tendency in the 4-hOur
laboratory runs. It was evident from t h e appearance and
quantity of scale formed after the treatments noted that a high
ash molasses is more likely t o scale than one low in ash, and under
such conditions, the use of stillage as a mash ingredient (back-
slopping) may aggravate the conditions sufficiently t o bring
about serious scaling. With a molasses low in ash, the same rate
of backslopping would not cause difficulty.
Typical results are shown in Figure 3 (right), where rates are
plotted as percentages of the initial rate on water. Curve 1
shows ethyl stillage from a fermentation mash make-up using
high ash molasses. Examination of t h e tube after this run
showed it to'be nearly free of scale (Figure 6). Compare this
with curve 2 where sulfuric acid was added t o the mash make-up.
This gave a heavy coating of scale (Figure 7) and repeated
experiments showed this heavy scale t o be formed when acid
was added either with or without backslopping. A comparison
should also be made between curves 1 and 3, which shows the
effect of backslopping which, by adding t o the salt content of the
mash, aggravates the scale-forming tendency. The use of tetra-
phosphoglucosate retards scale formation as shown by a com-
parison of curves 3 and 4. Figure 8 further illustrates the effect
of backslopping, and Figure 9 shows a lighter scale formation
when tetraphosphoglucosate is used.
RUNS MADE WITH FORCED CIRCULATION
Many commercial evaporators operate with forced circulation,
a high capacity centrifugal pump being used in each effect t o
bring the rate of flow of the solution into the heater up t o 5 t u
758 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 41, No. 4

lage produced no scale if the foam was absent, as is t,he case

when natural circulation was used. Thus, it was shown tha,t
where the solution t,o be cvaporated has scaling potentialit icx,
Foaming produces a n initial rise in evaporation rate follon-cti h\-
heavy scaling.
The most significant differences between natural and t'orccd
circulation were the creation of more foam in the case of the latter
and an increase in the rate of evaporation a t the start of the run.
Arrangements of the apparatus shown in Figures 10 and 11 wew
used t o c o n h u e the investjigation of t,he effect of foam on seal<:
formation. The arrangement shown in Figure 10 gave very little
foam entering the evaporator proper from the pump xhile
the added free space and swirliiig motion of the tangential inlet
in t h e arrangement in Figure 11 gave a foamy discharge from the
pump.
Typical results from the above arrangements of the equipment
are shown in Figures 12 (left) arid 13. Curve 1 of Figure 12 (left,)
was plotted from data from a nonfoamy run and shows only a
slight rate of decrease with time. Curve 2 is plotted from data
Figure 9. Comparison of Clean Tube with from a foamy run. Conditions were identical for each run except
Tube Scaled Lightly after $-Hour Run with for the physical changes in catchall arrangement necessary to
High Ash Stillage Treated w-ith 100 P.P.M. increase or decrease foam. Thc steeper gradient of curve 2,
Tetraphosphoglucosate the foaniy run, as compared to that of curve, 1, a norifoamy I'un,
Fermentation mash make-up included backslop but is due t o scale formation. Iternoval and visual Comparison of
n o acid used
the tubes confirmed the results obtained from condensate meas-
urements. The nonfoamy run gave a tube free of scale arid
15 feet per second. Under such conditions, molasses *olutioria the foarny run gave a coatirig of corisiderable t,hickness. The
which would cause bad scaling in a natural circulation cvaporator same basic data are shown iri Figure 13 where the total amourit,s
can be handled successfully k t h o u t un- of a-ater evaporated from the foamy
due difficulty, owing t,o the scouring effect runs are shown in curve 2 and from
of the rapidly moving liquid. Therefore, the nonfoamy run in curve 1. Under
a pump was inserted in t'he laboratory foamy conditions which gave a high
apparatus as shown by Figures 10 and
11 and a series of experiments made to
test' the effect of forced circulation in the
small equipment. The punip has a tend-
ency to cause foaming and experimenk
were first conducted t o see what effect this
factor had on the evaporation rate.
A test was made first with wat'er in t'he
evaporator. This gave an evaporation rate
of 16.4 ml. per minute. At the end of
0 . 5 hour several drops of Triton K-60 (a
quaternary ammonium salt, manufactured
by Rohm & Haas Company) were added
t o the water, which gave a very foamy so-
lution. When equilibrium conditions had
been obtained measurements mere made
.on the distillate and it was found to have
increased to a maximum of 22 ml. per
minute. After running for 0.5 hour a t
this rate, a small amount of defoamer was
sdded and the rate of evaporat'ion dropped
t o 17.1 ml. per minute when the foam
.had subsided. Thus, with pure water hav-
:ing no scale-forming potentiality, foaming
.increases the evaporation rate.
The first run with st,illa,gefoamed very
badly and an appreciable amount of liquid
came over from the catchall, which re-
quired lowering of the level in the evapo-
rator. It was obvious t'hat high evapo-
ration rates were prevailing a t the start
cof the run. Examination of t'he tube
after 90 minutes of running time, how-
ever, showed an unusually heavy coating Figure 10. Laboratorj Evaporator Figure 11. Forced Circulation
Arranged for Forced Circulation Laboratory Evaporator with Catch-
of scale, which differed from that formed with Downward Discharge from all and Downleg Arranged to Give
in previous runs in that a marked quantity Evaporator into Catchall to Mini- Foamy conditions on Discharge
of stillage solids was occluded. This etil- m i z e C a r q -Over of Foam Side of Pump
April 1949 INDUSTRIAL AND ENGINEERING CHEMISTRY 7594
1750
1 I I I 1

I
30
I
60 90
I
120
I , I I
Jo 60 90 IZO
RUNNING T I M E (MINJ RUNNING TIME (MIN)
Figure 12. Left. High Ash Molasses R u n s with Forced Figure 13. High Ash Molasses Runs with
Circulation with and without Foamy Conditions in Forced Circulation with and without
Evaporator Foamy Condition i n Evaporator
1, nonfoamy run, m a s h make-up with backslopping; 2, duplicate
o f 1 under foamy conditions; 3, r u n with rosin a n d tallow as de- 1, nonfoamy run, mash make-up w i t h baokslop-
foamers, m a s h make-up with hackslopping; 4, duplicate of 2 ping; 2, duplicate of 1 under foamy conditions; 3,
with 100 p.p.m. tetraphosphoglucosate added to stillage run with rosin a n d tallow as defoamers, m a s h
make-up with backslopping; 4, duplicate of 2 with
Right. Runs on Low Ash Molasses Stillage with Forced 100 p.p.m. tetraphosphoglucosate added to stil-
Circulation lage
1, without baclcslopping under foamy Conditions; 2, with back-
slopping under foamy conditions
defoamer addition improved the evaporator performance sob
that a t the end of a 2-hour period the per cent of the initial
initial evaporation rate, more water was evaporated in a 2- evaporation rate had decreased to about 55 with defoamer, while
hour period than under nonfoamy conditions with its naturally under foamy conditions the rate was only slightly over 10.
occurring lower initial evaporation rate. However, it is seen At the same time more water had evaporated from the solution
that the slope of the curves from the foamy run decreases, containing defoamer. Examination of the tube confirmed the
so that a t the end of 2 hours there is a definite falling off in indications from condensate amounts and showed a n extremely
the condensate owing t o scale formation. On the other hand, light coating of scale with defoamer, and a heavy coating where
the nonfoamy run, where the tube is not scaled, maintained no defoamer was used.
its rate well. Additional runs with forced circulation were made with low
I n evaluating evaporator performance on scaling solutions, ash stillage with and without backslopping but under foamy
both the scaling potentialities and the foaming characteristics conditions. Curves 1 and 2, Figure 12 (right), show that under
must be considered when determining cycles for shutdown and foamy conditions backslopping even with a low ash stillage i s
cleaning. It is indicated that less scaling might be expected if a detrimental t o evaporator performance.
defoamer were used and if the tubes were kept submerged when
solutions with high scaling potentiality were being evaporated. MICROMETER MEASUREMENTS OF SCALE THICKNESS
Curve 4 on Figures 12 (left) and 13 shows t h a t the addition of
tetraphosphoglucosate gives no marked benefit under foamy Table I offers further evidence of the results described above.
conditions over untreated solutions such as curve 1. Tubes were removed from the evaporator and measurements
In order t o investigate further the effect of foam on scale forma- were taken over the scale with a machinist’s micrometer t o t h e
tion and evaporation rates, the evaporator was run under condi- nearest 0.001 inch at four places on the tube length. At adjacent
tions which produced a heavy foam and observations were made points the scale was removed and the tube diameter measured.
o n the rate of condensate delivery and condition of tube. With- The difference between the two measurements is averaged.
out changing the conditions except to add a defoamer, the experi-
ment was repeated. Exaniination of curves 2 and 3 shows that SUMMARY
The experimental evaporator described makes possible a dem-
onstration of the manner of formation of calcium sulfate scale on
the heater tube. The scale forms rapidly during t h e early stages
TABLEI. MICROMETERMEASUREMENTS OF SCALE THICK- of evaporation of calcium sulfate solutions and less rapidly as t h e
NESSES AFTER R u m WITH FORCED
CIRCULATION scale thickness increases.
Scale The physical characteristics of the scale such as crystal size,
Conditions Thicknesses in Duration area between the crystals, and degree of adherence to the tube
in Thousandths of of Run, wall, are altered by addition of certain compounds to the evaporat-
1R.laterial Used for Run Evaporator Inch, Averaged Minutes ing solution. The manner in which commercial scale preventives
High ash molasses slop, 43% Mostly 12.2 90 work could be readily shown by the effect of these substances on
baokslon foam
High ash- molasses slop, 43% Little 0.0 120 the calcium sulfate scale. Wax coatings in combination with
backslop foam commercial scale preventives gave especially good results.
High ash molasses slop, 43 % Foamy 5.5 90 Spontaneous descaling during the run occurred where the tube
baokslop was resin coated. Addition of starch to the boiling solution also
High ash molasses slop, 43 % Fonniy 5.6 120
backslop caused spontaneous descaling.
High ash molasses slop, 43 % Foamy 6.0 120 When the apparatus was used to study stillage from molasses
backslop and 100 p.p.m. tetra-
p hosp hogluoosat e ethyl fermentation, i t was found that the addition of sulfate ion
High ash molasses slop, 43% Slightly 1 5 120 aggravated the scale-forming tendency; molasses high in ash
backslop and rosin and tallow foamy had more tendency to scale than molasses low in ash; and the
Lour ash molasses slop, no back- Foamy 1.0 120
Slop practice of backslopping aggravated the tendency to form scale.
Low ash molasses slop, 4370 back- Foamy 3.3 120 The runs gave a n interesting insight into the relation between
slop foaming, evaporation rate, and scaling otentialities. With
water, the evaporation rate was increase% by adding a foarn-
760 INDUSTRIAL AND ENGINEERING CHEMISTRY
producing substance, but fell back to the original rate when a
defoamer was added. When molasses was caused t o foam in the
evaporator, there was a n initial increase in rate followed by a rapid
and complete scaling of the heater tube. Superheating of the
films due t o the foaming apparently aggravated the tendency to
scale. Thus, where a solution has scale-forming potentiality,
foaming in the evaporator should be combated by the use of
defoamers or by suitable changes in evaporator design.
The data are presented on a laboratory scale and up t o the
present time very few experimental data have been obtained on
plant equipment. However, the authors have some evidence
that the conclusions drawn will be comparative t o some extent
with industrial oractice.
LITERATCJRE CITED
Ames, W.M., Chemistry & Indzistrg, 1946, 194-5.
Badger, W. L., and Caldwell, H. B., Chem. & M e t . Eng., 32,
616-17 (1925).
Bott. E. C. B.. J . SOC.Chem. Ind.. 56, 453-6 (1937).
Hall, R. E . , IND.EXG.CHEM..17. 283-90 (1925).
WRINKLE RESISTANCE OF FABRICS
I. J. GRUNTFEST AVD D. D. GAGLIARDI
Rohrn & Haas Compun.y, Philadelphia 57, Pa.
T h e results of experiments described in this paper show
that the wrinkle resistance of a fabric is determined by the
extent of its multifilament character and by the ability of
the separate fibers of which it is composed to recover from
tensile deformations. The extent of multifilament
character depends on the ratio of fiber diameter to fabric
thickness. This ratio determines the minimum strain
with which a fold may be made. The extent to which the
minimum strain is realized depends on the ease with
which the separate fibers can move relative to one an-
T H E properties of a fabric must be determined by the riature
of the fibers of which it is composed, its structural features,
end the type and distribution of finishing materials which rnay be
present. The details of the relations among these variables and
the properties of the finished fabric are very complicated, how-
ever, and it is not likely that a complete and exact analysis will be
given for some time. The experiments to be discussed here pro-
vide a limited and qualitative analysis of these relations, which
is a step ton-ard understanding the factors determining the wrinkle
resistance of fabrics. This study was initiated because, although
chemical treatments have been used for some time to improve the
wrinkle resistance of fabrics, the mechanism by whirh these
effects are produced has not been altogether clear.
Before the experiments are described, the general considera-
tions which led t o their design will be discussed. When anv
sheet material is folded, a permanent nrinkle or crease will br
produced if the deformations accompanying the fold are so great
that the material cannot recover its original form.
Fabrics differ from other sheet materials, such as
cellophane, by being knitted or woven from yarns
made of many small fibers 01 filaments. As a re-
sult of this rnultifilamcnt character, fabrics are
much more easily folded and more winkle resist-
ant, because the deformations which accompany
folding can be relieved by adjustment of the rela-
tive positions of the separate fibers or filaments. FIGURE IA
HOMOGENEOUS B E A M
Figure 1 illustrates the mechanism by which
bending strains ran he rclicvcd in a multifila- Figure 1. Mechanism of Strain Reduction in RIuZtidilament Yarns
Vol. 41, No. 4
(5) Hewlett. A. M.,Mulfekuhler, A . F., and Lui, E., 8ugur. 42
30-1 (1947).
(6) Hildebrandt, F. M., FoodPnd., 13, No. 12, G2-4 (1941).
(7) Kerr, E. W., Louisiana Expt. Sta., Bull. 149 (1914).
(8) Lamb, C. J., Chem. Inds., 60, 411 (1947).
(9) McAdams, W. H., “Heat Transmission,” 1st ed., pp. 301-5,
New York, McGraw-Hill Book Co., 1933.
(10) McCabe, W. L., and Robinson, C;., IND.ENG.CHEM.,16, 47H
(1924).
(11) Mitchell, D. T., Shildneck, P., and. Dustin, J . , IND.
I 3 . s ~CHEM.,
.
A N ~ LED.,
. 16, 754-5 (1944).
(12) Olin, H. L., Dowell, W. H., and Toynbee, C. M . , Chem. & M e t
Em.. 31. 116-19 (19241.
(13) Othmer. D. F.. Ixu. ENG.CHEII.. 21. 876-7 (1929)
(14; Pridgeon, L. A., and Badger, W. L., Ibid., 16, 474-9 (1924).
(15) Reavell, B. N., Chemistry & Industry, 1946, 254-5.
(16) Van Marle, D. J., IND. ENG,CHEM.,16, 458 (1924).
(17) Webre, A. L., and Robinson, C. S., “Evaporation,” pp, 189-92,
Kew York. Chemical Catalog Co., 1926.
KECPSVED
\Inrcli 3, 1948.
other. This is, in turn, regulated by the structure of thp
fabric, the presence of sizing or lubricating agents, the
smoothness of the fiber surface, and the stiffness of the
fibers. Selected urea-formaldehyde resins, formalde-
hyde alone, and glyoxal, which have access to the inside of
the fiber, improve the ability of cellulose fibers to recover
from deformations and increase their stiffness. Resin
deposited on the outside of the fibers impairs the niulti-
filament character, stiffens the fabric, and reduces i t a
ability to recover from folding.
ment material. A represents a single-filament yarn (homo-
geneous beam) being bent through a 90” angle. The path,
which an imaginary element on thc outside of the bend must
traverse, is greater than the original length of this element
Consequently, when the bend is made, the element must be
stretched. Similarly, the element on the inside must be com-
pressed, since the path length in this position is smaller than
the original length of the element. Somewhere in the middle of
the beam there are elements which are neither stretched nor com-
pressed when a bend is made. These me said to be in the neutral
plane of the deformation. For any imaginary elements in this
beam, the amount of deformation suffered depends on the dig-
tance from the neutral plane of the deformation. Figure 1, B,
shows one way in which both tensile and compressiv~strain? mhv
he relieved when a multifilament yarn is bent; the separate.
fibers slip by one another rather than stretch out. C illustratei
another mechanism by which bending deformations ran be rr-
FIGURE I5 FIGURE I C
M ULTI FILAMENT YARN MULTlFlLAMENT YARN