Professional Documents
Culture Documents
P.W. MADSON
KATZEN International, Inc., Cincinnati, Ohio, USA
Reflux
Rectifying
Low boiling product
Feed mixture
Stripping
Steam (energy)
will be devoted to a description of the d. Vapor will rise up the tower and liquid will
modifications required of the simple distillation flow down the tower. The purpose of the
system in order to make it effective for the tower internals (trays) is to allow intimate
separation of a very pure ethanol product, contact between rising vapors and
essentially free of its water content. descending liquids correlated with separation
Figure 2 expands on Figure 1 by showing some of vapor and liquid.
additional features of a distillation tower. These
are:
Figure 3 shows a vapor-liquid equilibrium
diagram for the ethanol-water system at
a. The highest temperature in the tower will
atmospheric pressure. The diagram shows mole
occur at the base.
percent ethanol in the liquid (X axis) vs mole
b. The temperature in the tower will regularly percent ethanol in the vapor (Y axis). The plot
and progressively decrease from the bottom could also be made for volume percent in the
to the top of the tower. liquid vs volume percent in the vapor and the
equilibrium curve would only be slightly
c. The tower will have a number of similar,
displaced from that shown in Figure 3. Mole
individual, internal components referred to
percent is generally used by engineers to analyze
as ‘trays’ (these may also be described as
vapor/liquid separation systems because it
stages or contactors).
Vapor
Reflux liquid
Overhead product
Feed
Trays (contacting devices)
temperature
Higher
Vapor
Thermal energy
Boiling liquid
Bottoms product
relates directly to molecular interactions, which become quite complex and would not lend itself
more closely describe the process occurring in easily to graphic analysis.
a distillation system. Referring to Figure 3, a 45o line is drawn from
Analysis of the ethanol-water distillation the compositions of 0, 0 to 100% and 100%.
system is mathematically straightforward when This 45o line is useful for determining ranges of
using molar quantities rather than the more compositions that can be separated by
common measurements of volume or weight. distillation. Since the 45 o line represents the
This is because of an energy balance principle potential points at which the concentration in the
called ‘constant molal overflow’. Essentially, this vapor equals the concentration in the liquid, it
principle states that the heat (energy) required indicates those conditions under which
to vaporize or condense a mole of ethanol is distillation is impossible for performing the
approximately equal to the heat (energy) separation. If the equilibrium curve contacts the
required to vaporize or condense a mole of 45 o line, an infinitely large distillation tower
water; and is approximately equal to the heat would be required to distill to that composition
(energy) required to vaporize or condense any of vapor and liquid. Further, if the equilibrium
mixture of the two. This relationship allows the curve crosses the 45 o line, the mixture has
tower to be analyzed by graphic techniques formed an azeotrope. This means that even if
using straight lines. If constant molal overflow the tower were infinitely large with an infinite
did not occur, then the tower analysis would amount of energy, it would be impossible to
distill past that point by simple rectification.
Azeotrope
194° proof
100
90
Equilibrium Curve
80
70
Mole % ethanol in vapor
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100
Consider a very simple system consisting of a collection of small amounts of vapor, analysis
pot filled with a mixture of ethanol in water (a would reveal that each successive portion of
beer) containing 10% by volume ethanol (3.3 vapor would become richer in ethanol.
mole %). This composition is identified in the Thus we have created a series of steps by
lower left portion of Figure 3. A fire could be which we keep increasing the ethanol content
kindled under the pot, which would add thermal of the analyzed sample, both liquid and vapor.
energy to the system. The pot would begin to Unfortunately, this oversimplified process is
boil and generate some vapor. If we gathered a idealized; and practically speaking, is
small portion of the vapor initially generated and impossible. However if we had supplied our
measured its ethanol content; we would find original pot with a continuous supply of ethanol-
about 24 mole % ethanol (53 volume %). If we water feed and vapor generated in the first pot
condense this vapor (note: there will be only a was continuously condensed and supplied to the
small amount of this vapor), boil it in a second second pot, etc. then the process becomes similar
pot and again collect a small amount of the initial to the industrial distillation tower operation
vapor generated, this second vapor would shown in Figure 2.
contain about 55 mole % (83 volume %) of How far can this process be extended? Could
ethanol (see Figure 3). If we should continue we produce pure ethanol by continuously
this simplified process to a third and fourth extending our process of boiling and reboiling?
The answer is, no! We would finally reach a solutions of ethanol and water are also known
point in one of the downstream pots, where the as constant boiling mixures (CBM) since the
vapor boiling from the liquid was of the same azeotropic liquid will have the same temperature
composition as the liquid from which it was as the azeotropic equilibrium vapor being boiled
being generated. This unfortunate consequence from itself. Without some sort of drastic process
limits our ability to produce anydrous ethanol intervention, further ethanol purification
from a dilute ethanol-water feed. What we finally becomes impossible. The question then
encounter in our simplified process is the becomes: What can we do to make it possible to
formation of an azeotrope. This is a concentrated produce anhydrous ethanol? Methods of doing
solution of ethanol and water that when boiled so will be covered later in this chapter.
produces a vapor with a composition identical Figure 4 depicts the structure of the distillation
to the composition of the liquid solution from process by dividing the vapor/liquid equilibrium
which it originated. information into three distinct zones of process
In summary then, we are limited in ethanol- and equipment requirements: stripping, rectifying
water purification in any single multistage and dehydration. This division is the basis for
distillation tower to the production of azeotropic the design of equipment and systems to perform
ethanol-water mixtures. These azeotropic the distillation tasks.
Anhydrous
product
Stillage
Stripping system
Spirit
Dehydration
Rectifying system system
100
90
Equilibrium curve
80 Azeotrope 194° proof
70
Mole % ethanol in vapor
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100
Mole % ethanol in liquid
(10 volume %)
DISTILLATION CONTACTORS
Figure 6 depicts a perforated tray contactor with
certain accoutrements required to control the
Trays are the most common contactor in use. flow of liquid and vapor and to assure their
What are the functions expected of tray intimate contact. Another type of tray contacting
contactors in the tower? Figure 5 depicts a single device, the disc-and-donut or baffle tray is
tray contactor in a distillation tower and shows shown in Figure 7. The characteristics of this
the primary functions desired: type of contactor make it especially useful for
distilling materials such as dry-milled grain beer,
- mixing rising vapor with a falling fluid which would foul ordinary trays such as
perforated, valve, etc.
- allow for separation after mixing
- provide path for liquid to proceed down the ENERGY ANALYSIS
tower
In addition to the selection of the basic contacting
- provide path for vapor to proceed up the
device, the energy requirement must be
tower
Enriched Downcoming
Outlet weir vapor liquid
Inlet weir
V/L separation
V/L mixing
Downcomer
area
Perforated
area Vapor Stripped
liquid
Figure 6. Perforated trays.
established. This is accomplished by analyzing simplified procedure to calculate the
the vapor/liquid equilibrium data from Figure approximate energy requirement from the
4, for the liquid:vapor flow ratio to perform a liquid:vapor flow ratio that will be employed in
continuous series of steps within the limits of the tower design. Repetition of this type of
the equilibrium curve. Table 1 demonstrates a calculation for different conditions produces a
Descending Descending
liquid liquid
Enriched
Donuts vapor
Disc
Vapor
Stripped stillage
Example 2. Calculate the steam required to strip 100 gpm of a 5% volume beer (95 gpm water/5 gpm ethanol).
L/V = 6.33 (typical for a 5% volume beer) or L = 6.33 • V
L = 95 gpm • 500 lbs/hr = 47,500 lbs/hr = 6.33 • V
gpm
Therefore, V = 7,500 lbs/hr (steam)
And: 7,500 lbs/hr (steam) • hr = 25 lbs steam/gallon of product
5 gpm (product) 60 min
*L and V are liquid and vapor flow rates, respectively, expressed in lb-mole per hr.
Note: at base of column use simplifying assumption of water (L) and steam (V). Therefore: L (lb-mole/hr) = L (lbs/hr)
V(lb-mole/hr) V(lbs/hr)
design chart like that shown in Figure 8 for the are based on the energy input, as calculated and
ethanol-water system. Such a graph is useful represented in Figure 8. Because of the principle
when calculations are needed to ascertain of constant molal overflow, the operating lines
technical and economic feasibility and can be represented as straight lines. If constant
preliminary conditions for the design. molal overflow was not valid for the ethanol/
Figure 9 demonstrates how the liquid:vapor water distillation, then these lines would be
flow ratio, in connection with the number of curved to represent the changing ratio of liquid
stages (theoretically ideal trays) required for a flow to vapor flow (in molar quantities)
specified separation between ethanol and water, throughout the tower. The slope of the operating
is graphically determined. Note that the stages line (the ratio of liquid flow to vapor flow) is
are constructed by drawing straight lines also called the internal reflux ratio. If the energy
vertically and horizontally between the input to a tower is increased while the beer flow
equilibrium curve (previously determined remains constant, the operating lines will move
experimentally) and the operating lines. For an toward the 45o line, thus requiring fewer stages
ethanol stripper/rectifier, there are two operating to conduct the distillation. Likewise if the energy
lines: one for the rectification section and one input is reduced (lowering the internal reflux
for the stripping section. The operating lines ratio), the operating lines will move toward the
represent the locus of concentrations within the equilibrium curve, reducing the degree of
distillation tower of the passing liquid and vapor separation achievable in each stage and therefore
streams. The operating lines for a given tower
30
Constraints:
1. 190° proof product
2. 0.02% (wt) bottoms
25 3. Saturated feed
4. Direct steam
Lbs steam/gallon (anhydrous ethanol basis)
Practical minimum
20
15
10
Theoretical minimum
0
0 5 10 15
90 8 9 10 11 12 13 14
Equilibrium curve
80
7
6
5 190° proof
70 4
Mole % ethanol in vapor
60
2
50
40
Operating line
rectification
30
1
Operating line
stripping
20
Typical L / V=5.0
10
0
0 10 20 30 40 50 60 70 80 90 100
Stillage
(0.02 wt %)
Mole % ethanol in liquid
Beer feed
(10 volume %)
requiring more stages to conduct the distillation. diameter required for the given distillation tower.
The calculations underlying the preparation of Since all of the distillation ‘work’ is done by the
Figure 9 go beyond the scope and intent of this trays, the tower is actually the ‘container’ to
text, but have been included for continuity. The surround the vapor and liquid activity that is
dashed lines represent the graphical solution to ‘managed’ by the trays. Tower diameter design
the design calculations for the number of is, therefore, actually the design of the necessary
theoretical stages required to accomplish a tray diameter for proper vapor/liquid interaction
desired degree of separation of the feed and movement.
components. Figure 9 is referred to as a McCabe- The f factor (vapor loading) is an empirically
Thiele diagram. For further pursuit of this determined factor that depends primarily upon
subject, refer to the classical distillation textbook tray type and spacing, fluid physical properties,
by Robinson and Gilliland (1950). froth stability and surface tension at the
operating conditions of the system. The proper
values for f are determined by field observations.
TOWER SIZING In summary then, the f factor can be described
as an adjusted velocity term (units are ft/sec) that
The goal of the design effort is to establish the when multiplied by the square root of the density
size of the distillation tower required. Table 2 ratio of liquid to vapor, will give the allowable
shows the basic procedure to determine the vapor velocity in the empty tower shell, such
Table 2. Calculations for tower sizing (base of stripper).
Example: Calculate tower diameter required for a 10% volume beer at 100 gpm (15 lbs steam/gallon of product)
W Vapor flow rate = 9,000 lbs/hr (steam)
P Operating pressure at base = 1.34 ATM
MAVG Average MW of vapor = 18 lbs/lb-mole
ρL Liquid mixture density = 59.5 lbs/ft3 (227 °F)
T Absolute operating temperature = 687 °R
D Tower inside diameter in inches
f Vapor loading factor = 0.05-0.3
W 9000 16.45
D = 0.2085 • = 0.2085 • =
Sizing equation: P • M AVG • ρL f•
1.34 • 18 • 59.5 f
f•
T 687
Assuming f = 0.16 (specific to tray design and spacing), the tower diameter is:
16.45
D= = 41.125 inches
0.16
Tower diameter calculation utilizes the following equation. Values for the terms are indicated above.
W
D = 0.2085 •
P • MAVG • ρL
f•
T
The final design equation can be derived beginning with the fundamental equation:
u = f • ρL ρV
-
ρV
(Note: For most cases ρL is much greater than ρV, so that ρL – ρV ≅ ρL. For example, water (steam) at 212oF and atmospheric
pressure: ρL = 59.8 lbs/ft3 and ρV = 0.0373 lbs/ft3. Then ρL – ρV = 59.7627 lbs/ft3 ≅ 59.8 lbs/ft3, which results in a negligible
0.06% error.)
ρL
Consequently, u≅ f •
ρV
Imposing the equation of continuity: W = A•ρV•u or u = W/A•ρV
Where A = tower cross-section area (ft2)
ρV = vapor density (lbs/ft3)
u = average vapor velocity in empty tower shell (ft/sec)
and W = vapor mass flow (lbs/sec)
Substituting for u in the equation above:
W W
≅ f • ρL
W ≅ f • ρρLL • ρρvV or A ≅
A • ρρV then A f • ρρLL • ρρvV
V ρV
Use the Ideal Gas Law to express the vapor density.
W
P • MAVG A=
ρV =
AVG
P • MAVG ρ
AVG •• ρ LL
R•T
Then by substitution one obtains f • P •M
R•T
Using the Universal Gas Constant R = 0.73 (ft3)(atm)/(lb-mole)(oR) the equation becomes:
W
A= π • D2
P •• M
MAVG ρ
AVG • ρ L Now A= = 0.7854 • D22
1.17 • f • 4
T
2 W 1.0879 • W
D = =
and PP ••M
MAVG ρ
AVG •• ρ LL AVG • ρ L
P •• MAVG
0.9192 • f • f• L
T T
1.043 • 12 W W
Adjusting units: D = • Therefore, D (inches) = 0.2085 •
60 PP ••M
MAVG ρ
AVG •• ρ LL PP••M
MAVG ρ
AVG •• ρ LL
f• f•
T T
that liquid entrainment and/or vapor phase vapor/liquid mass transfer systems involves a
pressure drop in the tower will not be excessive. number of interrelated parameters. The positive/
Excessive vapor velocity will first manifest negative balance of a variety of contacting
itself by causing excessive liquid entrainment devices with different capacities and efficiencies
rising up the tower, causing loss of separation for promoting vapor/liquid mass transfer must
efficiency. Ultimately the excessive entrainment be taken into consideration. Along with the
and pressure drop will cause tower flooding. technical issues considered in such designs,
To achieve a well-balanced tower design, the economical operation is essential not only in the
foregoing analysis must be performed at each reduction of energy and other direct costs, but
stage of the tower, from bottom to top. also in relation to investment and return on
Composition changes, feed points, draws, etc., investment from the operation being considered.
each can cause a different requirement. The In this respect, distillation towers are not
tower must be examined to locate the limiting independent process-wise, as consideration must
point. also be given to other auxiliaries such as
Similar analyses, with empirically-observed reboilers, condensers, pumps, controls and
performance coefficients, are applied to vapor related equipment.
passing through the trays and through the liquid,
and to the movement and control of liquid
passing through downcomers and across the SIZING TOWERS
trays. These analytical procedures are beyond
the scope of this text. Reference should be made In determining optimum diameter and height of
to the aforementioned text by Robinson and towers for distillation, absorption, stripping and
Gilliland for further information. similar mass transfer operations, design factors
are affected by whether the installations will be
indoors or outdoors. With indoor installations,
Considerations in optimizing distillation building height limitations, as well as floor level
accessibility, are an important factor in the
system design design. Where there are height limitations, towers
Optimizing the technical and economic design must be increased in diameter to provide for
of distillation equipment and similar gas and reduced tray spacing, which in turn will require
lower vapor velocities. With outdoor Trays of various types are predominant in
installations, literally the ‘sky is the limit’, and vapor/liquid contacting operations, particularly
refinery and petrochemical towers of 200 feet on the very large scale encountered in the
in height are not uncommon. petroleum and petrochemical industries, in large
In either case, indoors or outdoors, the scale operations of the chemical process
interrelated tower diameter and tray spacing are industries and in the large scale plants of the
limited by allowable entrainment factors (f motor fuel grade ethanol industry.
factors) (Katzen, 1955). If outdoors, tower The venerable bubble cap tray, with a wide
heights and diameters must be related to variety of cap sizes, designs and arrangements
maximum wind loading factors in the specific to maximize contact efficiency, has fallen out
plant location and may be complicated by of favor during the past few decades because of
allowance for earthquake factors. the relatively high cost of manufacture and
assembly. Valve trays of several types have taken
over in operations requiring a relatively wide
TRAY AND PACKING SELECTION vapor handling capacity range (turndown). This
has been extended by use of different weights
Vapor/liquid contacting devices may be of two of valves on the same tray. Specialty trays such
distinct types, namely packed or tray (staged) as the Ripple, Turbogrid, tunnel cap and others
towers. In packed towers, the transfer of material designed to improve contact under certain
between phases occurs continuously and specific circumstances have been used to a
differentially between vapor and liquid through- limited extent.
out the packed section height. By contrast, in The long established perforated tray is a
tray towers, the vapor/liquid contact occurs on contacting tray into which a large number of
the individual trays by purposely interrupting regularly oriented and spaced small circular
down-flowing liquid using downcomers to openings have been drilled or punched. These
conduct vapor-disengaged liquid from tray to trays are commonly referred to as ‘sieve trays’
tray and causing the vapor/liquid contact to occur because of the original practice of putting the
between cross-flowing liquid on the tray with maximum number of holes in any given tray
vapor flowing up through the tray. In other area. This original design produced a fairly
words, the vapor/liquid contact is intermittent inefficient operation at normal loading, and a
from tray to tray, and is therefore referred to as very inefficient operation with decreased vapor
being stagewise. Thus, for any given separation loading. About 50 years ago, engineers began
system, the degree of vapor/liquid contact will to suspect that the design approach had been in
be greater with a greater height of the packed error, and that the hole area in the trays should
section, or in the case of tray towers, a greater be limited by the hole velocity loading factor to
number of trays used. obtain maximum contact by frothing, as
It is generally considered that packing-type indicated in Figure 10.
internals may be used with relatively clean vapor The hole vapor loading factor (or perforation
and liquid systems where fouling is not a factor) is defined as the vapor velocity through
problem. Economics indicate that packing is the perforations adjusted by the square root of
applicable in small and modest sized towers. As the vapor density at the specific tower location
the towers become larger, packing becomes of a given perforated tray. With the parallel
complicated by the need for multiple liquid development of separation processes in the
redistribution points to avoid potential vapor/ petroleum refining, chemical and ethanol
liquid bypassing and reduction in efficiency. industries, the modern approach has developed
Structured packings (Fair et al., 1990; Bravo et to what is now called ‘perforated tray’ design.
al., 1985) are designed to minimize these The Fractionation Research Institute of the
problems by reducing the height requirement and American Institute of Chemical Engineers
controlling, to some extent, the distribution of diverted its efforts from bubble cap studies to
liquid. However, high fabrication and perforated tray testing; and have established a
specialized installation costs would indicate that basis for the design of perforated trays with high
these are applicable only for relatively low- efficiency and wide capacity range (Raphael
volume, high-value product processing. Katzen Associates, 1978).
Enriched
vapor Downcoming
Outlet weir Froth zone liquid
Inlet weir
V/L separation
V/L mixing
Downcomer
area
Vapor Stripped
liquid
Rectifying
Reflux
Steam (energy)
Reboiler
Condensate
return to boiler
High boiling product
of cooling tower water with limited temperature distillation (similar to multiple effect
rise and minimal scale-forming tendencies. On evaporation) are also practiced. Pressure-to-
the other hand, where water is extremely scarce, atmospheric, atmospheric-to-vacuum, or
air-cooled condensers are used. pressure-to-vacuum tower stages are utilized,
with the thermal energy passing overhead from
one tower to provide the reboiler heat for the
Energy conservation next one. Two such stages are quite common
and three stage systems have also been utilized
The increasing cost of thermal energy, whether (Katzen, 1980; Lynn et al., 1986).
provided by natural gas, fuel oil, coal or biomass, Furthermore, the modern technique of vapor
is fostering an increased emphasis on heat recompression, commonly used in evaporation
recovery and a reduction in primary thermal systems, is also being applied to distillation
energy usage (Fair, 1977; Petterson et al., 1977; systems. Such a system can provide for
Mix et al., 1978). Conventional bottoms-to-feed compression of overhead vapors to a pressure
heat exchangers are now being supplemented and temperature suitable for use in reboiling a
with recovery of overhead vapor latent heat by lower pressure stripping tower. However, the
preheating feed streams and other intermediate compression ratios required for such heat
process streams. Techniques of multistage recovery may consume almost as much
electrical energy as would be saved in thermal The operation that has been most subject to
input. Alternative systems, using vapor critical comment is the distillation process. Many
recompression as an intermediate stage device relatively new ‘authorities’ in the field have
in the distillation system, have also been based their criticism on technologies that go
proposed. back 50-60 years, and have created an
unwarranted condemnation of distillation as a
viable process for low energy motor fuel grade
Control systems ethanol production. Systems developed over the
years will be described to show that much of
Control systems can vary from manual control, such criticism is unwarranted and unjustified.
through simple pneumatic control loops to fully
automated distributed control (Martin et al.,
1970). High level computer control has
facilitated the application of sophisticated PRODUCTION OF INDUSTRIAL ETHANOL
control algorithms, providing more flexibility,
Prior to the emphasis on motor fuel grade
reduced labor and higher efficiency with lower
ethanol, the major ethanol product utilized
capital investment. Such systems, when properly
worldwide was high purity, hydrous industrial
adapted to a good process design, have proven
ethanol, which is generally produced at a
more user-friendly than the control techniques
strength of 96 o GL (192 o US proof) ( oGL =
utilized in the past.
degress Gay Lussac = % by volume ethanol; US
proof = 2 x % by volume ethanol). Efficient
systems have been in commercial operation for
Economic design many years for the production of such high
In integrating the technology discussed, the final grade ethanol from ethylene, grain, molasses and
analysis must be economic. Alternative systems sulfite waste liquor. The basic distillation system
must be compared on the basis of investment is shown in Figure12.
requirements, recovery efficiency and relative In the case of synthetic ethanol (outside the
costs of operation. Thus, any heat exchangers scope of this publication), the beer stripping
installed for heat recovery must show a tower is not required and the refining system is
satisfactory return on the investment involved a simple three tower unit, which achieves 98%
in their purchase and installation. In comparing recovery of the ethanol in the crude feed as a
alternative separation systems, the overall first grade product. The final product may
equipment costs must be compared against contain less than 5 ppm total impurities and has
energy and other operating costs to determine a ‘permanganate time’ of more than 60 minutes.
which system offers the best return. Modern For the production of industrial or beverage
computer-assisted designs incorporate spirit products made by fermentation of grain,
economic evaluation factors so economic molasses or sulfite liquor, the system utilizes the
optimization can be determined rapidly. full complement of equipment shown in Figure
12. The beer feed is preheated from the normal
fermentation temperature in several stages,
recovering low level and intermediate level heat
Ethanol distillation/dehydration: specific from effluent streams and vapors in the process.
systems technology This preheated beer is degassed and fed to the
beer stripper, which has stripping trays below
Proven industrial technologies are available for
the beer feed point and several rectifying trays
distillation of various grades of ethanol from
above it. The condensed high wines from the
grain, sugarcane, molasses and other feedstocks.
top of this tower are then fed to the extractive
Improvements have been made over the years,
distillation tower, which may operate at a
particularly during development of the motor
pressure of 6-7 bars (87-101.5 psi). In this tower,
fuel grade ethanol industry. In such installations,
most of the impurities are removed and carried
a key requirement is the minimization of total
overhead to be condensed as a low grade ethanol
energy usage.
Preheater/
condenser Condenser
CW
Heads by-product
Beer feed
CW
Reflux
CW
Washwater
concentrating tower
Fusel oil
Condenser/ Condenser/ cooler Fusel oil
Reboiler Reboiler reboiler reboiler Reboiler by-product
Fusel oil
Steam Steam decanter
Steam
Stillage
Waste water
stream, from which a small purge of heads A small heads draw is taken from the overhead
(acetaldehyde and other low boiling impurities) condensate, which contains the acetaldehyde
may be taken while the primary condensate flow fraction along with a small amount of the ethanol
is fed to the concentrating tower. The purified, produced. This may be sold as a by-product or
diluted ethanol from the bottom of the extractive burned as fuel. A fusel oil side draw is taken at
distillation tower is fed to the rectifying tower, high fusel oil concentrations through a cooler
which has an integral stripping section. In this to a washer. In the washer, water is utilized to
tower, the high grade ethanol product, whether separate the ethanol from the fusel oil, with the
industrial or potable, is taken as a side draw from washings being recycled to the concentrating
one of the upper trays. A small heads cut is tower. The decanted fusel oil may be sold as a
removed from the overhead condensate. Fusel by-product. The ethanol recovered from the
oils (mixtures of higher alcohols such as propyl, crude streams is taken as a side draw from the
butyl, and amyl alcohols and their isomers, which concentrating tower and fed back to the
are fermentation by-products or ‘congeners’) are extractive distillation tower for re-purification
drawn off at two points above the feed tray but and recovery of its ethanol content.
below the product draw tray to avoid a buildup In an early version of this system, installed
of fusel oil impurities in the rectifying tower. The more than 60 years ago for the production of
overhead heads cut and the fusel oil draws are potable ethanol from grain and from molasses,
also sent to the concentrating tower. all towers were operated at atmospheric pressure.
It should be noted that the rectifying tower is However, installations made within the past 40
heated by vapors from both the pressurized years utilize the multistage pressure system to
extractive distillation tower and the pressurized reduce energy consumption to a level of about
concentrating tower. 50% of the all-atmospheric system.
In the concentrating tower, the various streams The commercial installations utilizing the
of congener-containing draws are concentrated. multistage pressure, or ‘pressure cascading’
technique operate with a steam consumption of and minimize investment, a common condensing
3.0-4.2 kg of steam/liter (25-35 lb/gallon) of 96o and decanting system is used for the two towers.
GL ethanol. This may be compared to about 6 The entrainer used to remove water as a ternary
kg of steam/liter for earlier conventional (three component) azeotrope may be benzene,
distillation systems. heptane (C 6-C 8 cut), cyclohexane, n-pentane,
diethyl ether or other suitable azeotropic agents.
Production of anhydrous ethanol The entrainer serves to create a three component
azeotrope that boils at a temperature lower than
Systems have been designed and installed for any of the three individual components and
production of extremely dry and very pure lower than the ethanol/water binary (two
anhydrous ethanol for food and pharmaceutical component) azeotrope. Therefore the ternary
use, primarily in aerosol preparations. These mixture will pass overhead from the tower,
systems, as shown in Figure 13, yield ethanol carrying the water upward. Upon condensing,
containing less than 200 ppm water (99.98o GL), the mixture separates in a decanter into an
less than 5 ppm total impurities and more than entrainer-rich layer and a water-rich layer.
60 minutes permanganate time. The hydrous ethanol feed enters the
The two tower dehydrating system has been dehydrating tower near the top. The feed
operated in two super-anhydrous plants in contacts the entrainer in the upper section of the
Canada, and was used to produce motor fuel tower. The three component mixture in this
grade ethanol (99.5o GL) in four installations in section of the tower seeks to form its azeotrope,
Cuba (prior to the advent of the Castro regime). but is deficient in water and contains more
The dehydrating tower and the entrainer- ethanol than the azeotrope composition.
recovery tower are operated at atmospheric Therefore, the ethanol is rejected downward in
pressure. Thus, they may utilize either low the liquid and is withdrawn as an anhydrous
pressure steam, hot condensate or hot waste product from the bottom of the tower. The water
streams from other parts of the ethanol process joins the entrainer, passing upward as vapor to
to minimize steam usage. To simplify equipment form a mixture that is near the azeotrope
CW
Cooler
Anhydrous ethanol
to storage
Dehydration
190° proof ethanol feed tower
from distillation Entrainer
recovery tower
CW
Condenser
CW
Reboiler Cooler Reboiler
Low pressure steam
or hot condensate Decanter
Condensate return
Waste
water