Contents

1. Introduction...........................................................................................................1
1.1 Distillery Yields................................................................................................................1
1.2 Definition and formula of yields..................................................................................2
1.2.1 Fermentation yield............................................................................................2
1.2.2 Fermentation efficiency....................................................................................2
1.2.3 Alcohol recovery..............................................................................................2
1.2.4 Overall Conversion Efficiency.........................................................................4
1.3 Values of Yield..................................................................................................................4
2. Raw Material.........................................................................................................4
2.1 Molasses Quality..............................................................................................................4
2.2 Molasses treatment..........................................................................................................4
3. Fermentation process.............................................................................................5
3.1 Pre - fermentation and batch fermentation................................................................5
3.2 Continuous Fermentation...............................................................................................7
4. Distillation.............................................................................................................9
5. Spent wash (stillage) treatment /or disposal........................................................13
6. References...........................................................................................................14

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1. Introduction

More than half of the mass of the molasses content is total sugar. This rich source of sugar
remains unutilized for the last 50 years by Ethiopian sugar industries except that of recently
Metahara sugar factory. The utilization of this by product primarily for ethanol production
will reduce dependency on foreign oil. In the face of the nation's fast-growing rate of energy
consumption, alternative bio-fuel projects especially ethanol can limit the growing demands
for oil and save hard-earned foreign currency in Ethiopia. With world reserves of petroleum
depleting in factory recent years, ethanol has emerged as most important alternative resource
for liquid fuel. In line with this, Minister of Mines and Energy of Ethiopia announced a
policy to begin blending of 5% ethanol into the country’s transport petrol pipeline, in Sept,
2008.

Brazil's sugar cane-based ethanol industry is far more efficient than the U.S. corn-based
industry. The efficiency difference between Brazil and US is not due to technological
difference; but it is due to the raw material difference utilized for ethyl alcohol production.
The cane molasses, the raw material being used in Brazil for ethanol production has also been
used in Ethiopia and several other countries. If Brazil has been efficient in producing ethanol
from molasses, there is no reason for Ethiopia to be inefficient as long as standard process
parameters have been maintained.

Just as in a sugar factory, there are a number of measures of operational efficiency in a

distillery.

1.1 Distillery Yields

There are four commonly used measures of yield

 Fermentation yield
 Fermentation efficiency
 Alcohol recovery
 Overall Conversion Efficiency

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1.2 Definition and formula of yields

1.2.1 Fermentation yield

Fermentation yield is measured in liters of absolute alcohol in beer per ton of sugars in
molasses, and is calculated by the formula below

Yf = Vb  ab / (Mm · fsm)

Where
Yf = fermentation yield
Vb = volume of beer (liter)
ab = alcohol content of beer (v/v)
Mm = mass of molasses (tone)
fsm = fermentable sugars content of molasses (m/m)

1.2.2 Fermentation efficiency

Fermentation efficiency is an expression of how much alcohol was actually produced in beer
relative to the amount that could be theoretically produced, and is given by

Ef = Yf  0.794 / 0.5111 × (100/1000)

The factor 0.794 corresponds to the specific gravity of absolute alcohol and the factor 0.5111
is best explained as follows: If one kilogram of sugar was completely fermented (using
theoretical 100% efficient yeast); 511.1 grams of alcohol and 1000 - 511.1 = 488.9 grams of
carbon dioxide would result.

1.2.3 Alcohol recovery

Alcohol recovery is a measure of how much alcohol was finally produced relative to the
amount that was in the beer. It shows the amount of losses in the evaporation and distillation
sections combined. Alcohol recovery is calculated as follows

E de = (aaVp + ssVf) / aaVb  100

Where
Ede = Alcohol recovery (or distillation and evaporation efficiency)
aaVp = volume of potable alcohol as liters of absolute alcohol

ssVf = volume of feints (alcohol left in distillation columns) as liters of absolute alcohol

aaVb = volume of beer as liters of absolute alcohol

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 1.2.4 Overall Conversion Efficiency

Overall conversion efficiency is a measure of how much alcohol is finally produced relative
to the amount that could be theoretically produced, and is given by
E o = E f  E de  100

1.3 Values of Yield

In a well run distillery, the standard values of yield that would be expected is shown in Table
1.

Table 1: Standard values of distillery yield

Parameter Value

Alcohol Recovery 98.5%

Fermentation Yield (L/ton of mol) 573

Fermentation Efficiency 89%

Overall Conversion Efficiency 87%

2. Raw Material

2.1 Molasses Quality

Total sugar is the most quality criterion in the sale of molasses since it is the factor that
determines its value in the most common uses of molasses. However, from the point of view
of ethanol production, the first step is to know how much molasses will be supplied to the
distillery plant. The next step is to calculate the amount of fermentable sugars (FS) in the
molasses. The fermentable sugars in molasses are sucrose, glucose and fructose. There are a
number of ways of measuring fermentable sugars in molasses; the most accurate method is to
use High Performance Liquid Chromatography (HPLC). The following factors leads to the
standardization of molasses.
 Ash content above 10 % can retard the rate of fermentation by 5 - 10 %.
 Extent of Caramelization: (Measured as color in Optical Density (OD) units at 375 nm of
0.1 % molasses dilution) > 0.40 OD retards fermentation rate by 20-25%; reaction ceases
beyond 0.65.
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 Volatile acids in mash > 2500 ppm reduces the rate of fermentation and yeast growth.
 Volatile acids in mash > 5000 ppm reduces fermentation rate by 30 - 40 %.
 Volatile acids in mash > 7000 ppm can kill the yeast reducing viability up to 40-50 %.

Table 2: Important parameters of molasses for Ethanol production

Parameters Standard value

Total sugar as invert, % 50-52
2.2
RDS, % 85
Gravity Purity,% 37.0
Fructose, % 7.0-8.0
Glucose% 5.0-6.0
% Fermentable Sugar % brix in molasses 45-50
Ash content, % < 10
Caramel content @ 0.1 % mol solution 0.3 Absorbance @ 375 nm, Max
Titrable volatile acidity in terms of 3000 – 5000
acetic acid and acetate salts (PPM)
Bacteria content in Colony forming unit (cfu)/g 10
Ratio of Fermentable to Total sugar (F:T) ≥ 0.9
Molasses treatment

Molasses has to be treated before feeding to pre-fermenters and/or fermenters. There are
various possible pretreatments of molasses prior to fermentation, all mostly aimed at reducing
the suspended and dissolved compounds that might cause scaling and blocking of distillation
columns. The main problem is the presence of calcium compounds, which are mostly derived
from the lime added to the hot cane juice in the clarification process. Thus, one of the usual
important specifications for molasses as an alcohol feedstock is that it should not contain
more than 10 % ash which can lead to serious scaling problems.
Scaling problem has come to be a major challenge in the ethanol plant of Metahara sugar
factory. To minimize this problem, installation of molasses treatment plant based on prior
study may be required. Molasses is first diluted to about 45 o Brix with hot water and held
above 70o C for a few hours in a decanter, then much of the suspended solids will settle out.
This method is advantageous for using centrifugal pumps. If sulphuric acid is used, the
temperature has to be minimized as shown in Table 3.
Table 3: Standard parameters of molasses treatment for batch fermentation

Parameters Standard values

RDS of molasses, % 50 -52
Ratio of condensate to molasses 0.67 - 0.7
Working temp of pre-diluter - heaters, oC 60 - 65

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pH of molasses in the pre-diluter - heaters 4.7- 4.9
H2SO4 kg/ton of mol @ 85 oBx 2.6 - 3.0
Exhaust steam 120 -130 oC (1.1-1.5 kg/cm2)
Temp at the diluted mol heater, oC 95 - 100
Time of decantation after filling, hr 2.0 - 2.5

3. Fermentation process

The fermentation efficiency depends upon the characteristics of fermentation material such as
pH, sugar content, CO2 content and the alcohol tolerance of the yeast. The design of the
fermentation system and the operational parameters such as temperature, oxygen content,
compositional uniformity etc. also affects the performance of the fermenter. Recalculation of
the fermentation material by passing through heat exchangers to control the temperature is
the common practice used in the industry. Mechanical stirrers are also provided for uniform
mixing of the fermentation material (Dongare and Oke, 2011).

3.1Continuous Fermentation

The decanted molasses has to be diluted further in such a way that it could not cause any
osmotic stress to the yeasts. In the pre fermentation and fermentation section, the following
operational phases needs a special precaution

 Yeast propagation
 Wash preparation for yeast propagation and fermentation
 Fermentation control
 Beer centrifuging or yeast recovery

Before starting any fermentation operation, cleaning of all the culture vessels, continuous
mixed bioreactors or fermenters, holding tanks, plate heat exchangers, pipes are extremely
important. Cleaning of the wash and fermentation apparatus is usually done with steam in
commercial operations. And hence, all bioreactors and interconnecting pipelines should be
sterilized with steam at 1.5 kg/cm2 (G). If wash and fermentation residues are allowed to
accumulate, bacterial contamination will be out of control and will greatly reduce alcohol
yield and even leads to rejection or replacement of the wash in a new batch. Having
sterilized with steam, any disinfecting cleaner can be used, but, from economic point of view,
it is best to use formaldehyde solution by wearing gas mask.

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To start yeast multiplication process, the molasses has to be diluted to about 18 oBx or s.g of
1.07 and for that of continuous fermentation, fermentable wash of 18 o - 20o brix is used.
Nutrient application, temperature, and pH control is the other important issue and will be
detailed in Table 5. The most preferred nitrogen source is urea. In cane molasses
fermentation, ammonium sulfate, which is used quite often as a nitrogen source in industrial
fermentations, should be avoided, since it may add to the scaling problem by forming calcium
sulfate. Another common nitrogen source in industrial fermentation is liquid ammonia but is
not encouraged to be used since it will raise the pH which subsequently favors bacterial
contamination.

Table 4: Standard Parameters for Continuous Biofermentation process

Parameters Standard values Remark

Initial volume of fermentable wash in the 40 % of the fermenter
bio-reactor before putting culture
Bx of mash feed for yeast culture 18
Temperature of fermented wash to be 30 - 32
maintained in bioreactors, oC
Yeast to be added 6 - 8 g/L of wash
Bx of mash to bio-reactor 18 - 20
Nutrients for yeast culture 2 g/L Urea and 1 g/L DAP
Nutrients for bio-reactor 0.1 kg Urea / m3 of mash
0.1 kg DAP/ m3 of mash
Antifoam 0.575 kg/ton of molasses
wash acidity, pH 4.2 - 4.4
Water to Yeast milk ratio 2.0 - 2.5:1
Biocide (Sodium metabisulfite) % wash in 75 ppm
case of bacterial contamination

4. Distillation

Separation operation achieve their objective by the creation of two or more coexisting zones
which differ in temperature, pressure, composition, and/or phase state. Distillation utilizes
vapor and liquid phases at the same temperature and pressure for the coexisting zones. The
feed material, which is to be separated into fractions, is introduced at one or more points
along the column shell. Because of the difference in gravity between vapor and liquid phases,
liquid runs down the column, cascading from tray to tray, while vapor flows up the column,
contacting liquid at each tray.

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Liquid reaching the bottom of the column is partially vaporized in a heated reboiler/or direct
injected steam to provide boil-up which is sent back up the column. The remainder of the
bottom liquid is withdrawn as bottoms, or bottom product. Vapor reaching the top of the
column is cooled and condensed to liquid in the overhead condenser. Part of this liquid is
returned to the column as reflux to provide liquid overflow. The remainder of the overhead
stream is withdrawn as distillate, or overhead product.

The overall flow pattern in a distillation column provides countercurrent contacting of vapor
and liquid streams on all the trays through the column. Vapor the liquid phases on a given
tray approach thermal, pressure, and composition equilibriums to an extent dependent upon
the efficiency of the contacting tray.

The alcohol (the lower-boiling component) tends to concentrate in the vapor phase, while the
water (the higher-boiling component) tends toward the liquid phase. The result is a vapor
phase that becomes richer in ethanol as it passes up the column and a liquid phase that
becomes richer in water as it cascades downward.

The feed is introduced at a point along the column shell at which the column is divided into
an upper section, which is often called the rectifying section, and a lower section, which is
often referred to as the stripping section.

The performance of the distillation process is measured by the distillation efficiency, which
depends up on the equipment set up, utilities, level of automation and other operational
factors.

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Table 5: Standard parameters for Multipressure distillation process (MSF)

Parameters Standard values

Alcohol content of fermented wash/beer, % 8- 9
Temp. of the preheated fermented wash/beer, °C 85 - 90
Wash level to be maintained in primary column reboiler, % 60
Operating Conditions of Degasser Column
 Top vacuum  0.37 - 0.45 bar(a)
 Top temperature  68 - 72 oC
 Bottom vacuum  0.55 - 0.65 bar (a)
 Bottom temperature  72 - 75 oC

Operating Conditions of Degasser Column

 Top vacuum  0.55 - 0.65 bar(a)
 Top temperature  72 - 74 oC
 Bottom vacuum  0.4 - 0.55 bar (a)
 Bottom temperature  80 - 84 oC

Operating Conditions of Dealdehyde Column

 Top vacuum  0.2 - 0.4 bar(a)
 Top temperature  78 - 80 oC
 Bottom pressure  0.6 – 1.0 bar (a)
 Bottom temperature  92 - 98 oC
 Alcohol Conc. at top tray  95- 96 % (v/v)
 Alcohol Conc. to be maintained at bottom column  12 - 20 % (v/v)

Hydrous alcohol, oGL ≥ 96 oGL

Grade of Power alcohol, oGL ≥ 99.9 oGL
Stillage alcohol content, % < 0.03 %
Fermentation efficiency, % 87- 90%
Distillation efficiency, % ≥98 %
Alcohol yield (Alcohol /tons of molasses) 250 - 265

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 Table 6: Anhydrous Ethyl Alcohol Standards (Ashok Organic, India)

S.N Parameters Standard values

1 Appearance A clear, colorless, volatile liquid free from foreign
particles
2 Oder Characteristic and burning
3 Miscibility Miscible with water, ether, chloroform
4 Rxn with NaOH and iodine A yellow precipitate is formed
5 Specifications
(a) Acidity as acetic acid, w/v < 20 ppm
(b) Density at 20 oC < 0.7900
(c) Aldehydes as acetaldehyde, w/v < 5 ppm
(d) Esters as ethyl acetate, w/v < 30 ppm
(e) Methanol, w/v < 5 ppm
(f) Higher alcohols as isobutanol < 5 ppm
(g) Non volatile residue < 50 ppm
(h) Water Content, %, w/v < 0.08
(i) Ethyl Alcohol assay, %, v/v > 99.9

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5. Spent wash (stillage) treatment /or disposal

The Biological Oxygen Demand (BOD) and Chemical Oxygen Demand (COD) of waste
from alcohol (spent wash) are very high and of the following order.

BOD ------------ 35000-45000mg/L

COD ------------ 65000-95000mg/L

Based on the type of treatment followed the amount of the BOD and COD removal is
presented as follows:

Table 7: Typical operating parameters for different biological process (Reign, 2007)
Biological process BOD removal in % Residence time in h/d Area of Application
Activated sludge
- Conventional 80-90 4-8h
- Extended aeration 90-99 3-7h
Pond/lagoon
- Aerobic (low rate) 80-95 10-40 days

The spent wash is colored and highly acidic with a very offensive odor, which poses serious
environmental problems. To overcome the ill effects of spent wash and reduce the cost of the
effluent treatment, manufacturing bio-compost using the press mud and spent wash has
helped industry to achieve zero pollution status (Signh, 2008). Bio-compositing of the
concentrated vinasse and filter cake to use as fertilizer is in use at Metahara Sugar Factory
and has to be managed well especially safety of workers in connection with hygiene and the
malodorous gasses.

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6. References

Briggs, D.E, 2004. Brewing Science and practice. CRC press, USA
Dongare, M.K and Oke, D. 2011. Efficient fermentation/distillation and effluent treatment
process to achieve maximum ethanol production and minimum effluent. Proc. of 10 th Joint
Conv. of STAI and DSTA: 43 -46. Bhosari, pune-411 026, India

Drapcho, C.M., 2008. Biofuels Engineering Process Technology. McGraw-Hill Companies,

Inc.
KBK Chem. Engg. Pvt Ltd. Operating Manual for Fermentation, Distillation Molecular Sieve
Dehydration (MSDH), and Evaporation Section for Metahara Sugar Factory. Pune, India

McNeil B. and . Harvey L. M, 2008. Practical Fermentation Technology. John Wiley & Sons,
Ltd. ISBN: 978-0-470-01434-9

Perry, R.H. and Green, D.W. 1999. Perry’s Chemical Engineers’ Handbook. 7th ed.

Peter Rein, 2007. Cane Sugar Engineering. Luckhoffstr. 16, D-14129 Berlin, Germany

Singh, N. 2008. Giocompost from sugar distillery effluent: effect on metribuzin degradation,
sorption and mobility. Pest Manag Sci 64:1057-1062.

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