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drain a flake bed saturated with miscetla which, as the ethanol are also soluble in petroleum ether. At 5 C
discussed earlier, corresponds to the residence time in the solubility of oil in the lighter phase in 3%. T h e
a n extraction stage. T h e e x t r a c t o r was charged with heavier phase contains 85% oil. Decreasing the tem-
flakes to a height of 10 cm, and ethanol was circulated perature below 5 C does not appreciably affect the
t h r o u g h it for 30 min. It was then allowed to drain for solubility.
1 min. The flakes were removed and the weight of E q u i l i b r i u m curves. The results of the equilibrium
miscella r e m a i n i n g on the flakes per unit weight of experiments are shown in Figures 4 and 5. Data points
solids was determined. T h e r e a c t o r was t h e n re- clustered together are results of the repetition of one-
c h a r g e d a n d the above e x p e r i m e n t was r e p e a t e d charge, two-charge and three-charge experiments. In
except t h a t the drain time was increased to 2 min. the ethanol extractions four- a n d five-charge experi-
This experiment was performed repeatedly for drain ments also were performed. For each solvent at least
times up to 7 min. In order to determine the drain five repetitive experiments were performed for each
time as a function of bed height, two more sets of n u m b e r of charges. Some of the d a t a points overlap
experiments were t h e n performed in a m a n n e r sim- on the plots because several of the repetitions pro-
ilar to the above except t h a t the extractor was charged duced very close results. In Figure 4, as the oil con-
with 18- and 25-cm-high flake beds. c e n t r a t i o n s increase, the slope of the line on the
drained miscella versus bound miscella curve for
ethanol is greater t h a n t h a t for the isopropanol curve
RESULTSAND DISCUSSION
which in turn is greater t h a n t h a t for the h e x a n e
Solubilities. At its boiling point, 78 C, 95% ethanol curve which has a c o n s t a n t slope of 1. This behavior
has a 12% oil solubility. At 75 C, a realistic operating can be explained by considering t h a t on a molecular
temperature, the solubility is 10%. The 12% solubility level there is a driving force, or potential, which
of cottonseed oil in 95% aqueous ethanol, measured in causes the oil to dissolve in the solvent. If the oil is
this work, is greater t h a n previously reported values only partially miscible in the solvent, t h e n this force
(13,14). T h e s e o t h e r studies, however, h a v e used decreases as the concentation of oil in the solvent
expeller-produced crude oil or commercially refined increases a n d goes to zero at the s a t u r a t i o n concen-
oil in their d e t e r m i n a t i o n s whereas in this study tration. Since isopropanol h a s a greater saturation
ethanol-extracted crude oil was used. Apparently,
some of the nontriglyceride components extracted by
70
25.0
65
~ 0 - ~ o ISOPROPANOL
-
ETHANOL
"~. 20.0
50
U
rr
f...l 55
Z
15.0 nr
0 I
Z
/
d 0
UJ < 50
U
CD
10.0 -3
llJ / "
rj / "
O3
Z
~E .~>,/././"/ HEXANE
45
tlJ
Q
i'1
d
5.00
/" 40
.000 I I I I
.000 5.00 10.0 15.0 20.0 35 ................. I I I I I
• 00 5.0 10. 15. 20. 25.
c o n c e n t r a t i o n t h a n ethanol, its driving force de- the more oil there is in a hexane miscella the more
creases more slowly t h a n ethanol over the same con- viscous the liquid becomes and the less it drains. The
centration range. Because hexane is completely mis- alcohols, on the other hand, are more polar t h a n hex-
cible with oil, its driving force is not a function of ane a n d have a greater affinity for the flakes. The
concentration. In an alcohol extraction, due to a addition of oil to the alcohol reduces the polarity of
reduction in the driving force, the miscella bound to the liquid and facilitates draining.
the flakes after draining consists of two parts, the Drain curve. The results of the ethanol draining
alcohol with dissolved oil and the unextracted oil. It experiments are shown in Figure 6. The points shown
is not necessary to consider the unextracted oil and represent the time it took flakes to drain free miscella
actual bound miscella as two distinct species, but at each bed height. Draining for longer periods t h a n
rather to treat them as a bound miscella h a v i n g an oil shown did not decrease the ratio of bound miscella to
concentration greater t h a n saturation (7). For exam- solids. As discussed earlier, these times represent the
ple, at a concentration of 12% in the drained ethanol optimum residence time in each stage. For example, if
miscella, the saturation point at the temperature of the bed depth is 25 cm then it takes about 6.5 min to
the experiment, the bound miscella contains 24% oil. drain the bed. Consequently, if the solvent spraying
Further, when the concentration of oil in the drained heads are, say, 130 cm apart, then the bed speed
ethanol miscella is 8%, the bound miscella concentra- through the extractor should be 20 cm/min. It is
tion is 14%. This shows t h a t even though the drained important to note t h a t the bed should not be allowed
miscella is not saturated there is still unextracted oil to become dry and should be operated at near flood-
in the flakes because the concentration of 14% is ing conditions.
greater t h a n the saturation concentration of 12%. It is E x a m p l e s of modeling calculations. U s i n g the
not until the drained miscella contains less t h a n above laboratory data as input to the computer model,
about 5% oil t h a t the bound and drained concentra- various parameters of a pilot or commercial scale
tions are approximately equal. Figure 5 shows the extraction operation can be computed. Figure 7 shows
amount of miscella left on the flakes as a function of the calculated minimum solvent-to-feed ratio for the
the a m o u n t of oil in t h a t miscella. The percentages three solvents considered in this study. It ranges
are calculated on a weight basis. It is interesting to from a value of 1 in hexane to almost 4 in ethanol, the
note t h a t as the percentage of oil in the miscella on least miscible of the three. These results are for a chill
the marc increases, the amount of miscella bound to separation of the alcohol solvents and an evaporative
the marc increases when hexane is the solvent but separation of hexane. For the alcohol solvents, this
decreases when alcohol is the solvent. This pattern factor is a function of both the concentration of oil in
remains when the percentages are calculated on a the fresh miscella and the solubility ofoil in the alco-
volume basis. A possible explanation for this is t h a t hol at the extraction temperature. T h a t is, at this
30.0
4.0
ETHANOL
25.0
3,0
Q
LU
20.0 UJ ISOPROPANOL
I LL
0_
uJ 1--
o z
IM
o >
w
m .J
Q
@.0
15.0 Ul
HEXANE
20.0
5.00
.000
l
2.00
DRAIN
I
A.O0
TIME
I
6.00
{MINUTES)
I
8.00
I
i0.0
i.O
! EXTRACTION SOLVENT
FIG. 6. E x p e r i m e n t a l l y d e t e r m i n e d t i m e n e e d e d to d r a i n
t h e f r e e m i s c e l l a f r o m a bed o f f l a k e s for t h r e e d i f f e r e n t FIG. 7. Model c a l c u l a t i o n o f t h e s o l v e n t to f e e d r a t i o s
bed h e i g h t s . for t h e t h r e e s o l v e n t s c o n s i d e r e d in t h i s study.
7.0
6.0
4.o T
5.0
ISOPROPANOL
3~ a.o T /
u) 4.0 ISOPROPANOL
D
H /
D_ /
J
3.0
2,0
121 ETHANOL
I--I -J
U~
W
II £D //~ET~ANOL
2.0
£r
l.O
1.0 HEXANE
.......... I I -~, I
3 4 5 6 7 8 9 t.0 2.0 3.0 4.0 5.0