ARTICLE IN PRESS

WAT E R R E S E A R C H 40 (2006) 2349 – 2356

Available at www.sciencedirect.com

journal homepage: www.elsevier.com/locate/watres

Distillery wastewater treatment by the membrane-based

nanofiltration and reverse osmosis processes$

Sanna Kotrappanavar Nataraj, Kallappa M. Hosamani, Tejraj M. Aminabhavi

Membrane Separations Division, Center of Excellence in Polymer Science, Karnatak University, Dharwad 580003, India

art i cle info A B S T R A C T

Article history: A hybrid nanofiltration (NF) and reverse osmosis (RO) pilot plant was used to remove the
Received 30 September 2005 color and contaminants of the distillery spent wash. The feasibility of the membranes for
Received in revised form treating wastewater from the distillery industry by varying the feed pressure (0–70 bar) and
24 February 2006 feed concentration was tested on the separation performance of thin-film composite NF
Accepted 12 April 2006 and RO membranes. Color removal by NF and a high rejection of 99.80% total dissolved
Available online 6 June 2006 solids (TDS), 99.90% of chemical oxygen demand (COD) and 99.99% of potassium was
Keywords: achieved from the RO runs, by retaining a significant flux as compared to pure water flux,
Membrane which shows that membranes were not affected by fouling during wastewater run. The
Reverse osmosis pollutant level in permeates were below the maximum contaminant level as per the
Nanofiltration guidelines of the World Health Organization and the Central Pollution Control Board
Distillery specifications for effluent discharge (less than 1000 ppm of TDS and 500 ppm of COD).
Wastewater & 2006 Elsevier Ltd. All rights reserved.
Effluents

1. Introduction generation, etc., is in the range of 14.5–21.4 L/L of alcohol

Distilleries are one of the 17 most polluting industries listed
by the Central Pollution Control Board (CPCB, 2002–03). For
every liter of alcohol produced, the molasses-based distil-
leries would usually generate about 8–15 L of wastewater,
characterized by high chemical oxygen demand (COD) and
dark brownish color. Indian spent wash also contains a large
percentage of potassium compared to spent wash from other
countries (Sekar and Murthy, 1998). Even though wastewater
is generated at various stages of alcohol production, waste-
water from the fermenter sludge, spent wash and spent lees
are the main contributors to pollution. Distilleries (Uppal,
2004) are one of the highest consumers of raw water, with a
consumption in the range of 25–175 L/L of alcohol. The raw
water requirement includes both process and non-process
applications. Water consumption in process applications,
such as yeast propagation, molasses preparation, steam
production. On the other hand, water consumption in non-
process applications, like cooling water, steam generation,
making potable liquor etc., is much higher, i.e., between
102.65 and 240 L/L of alcohol production. Most distilleries in
India have been generating huge quantities of high toxic
effluents. However, hitherto, the best efforts made for a
comprehensive treatment have not been successful. Most of
the treated effluent with the best available process technol-
ogy also yields very high levels of COD and total dissolved
solids (TDS), with black-colored effluent with odors to the
streams, rivers and natural water. The problem of colored
effluent is particularly identified with the use of reactive dye
stuffs, as nearly 50% of the total dyes applied can be
discharged into the effluent.
Membrane-based separation processes like nanofiltration
(NF), ultrafiltration (UF) and reverse osmosis (RO) have been
applied for treating a wide variety of industrial effluents

$
This article is Center of Excellence in Polymer Science Communication number 92.
Corresponding author. Fax: +91 836 2771275.
E-mail addresses: dr_kmhosamani@yahoo.com (K.M. Hosamani), aminabhavi@yahoo.com (T.M. Aminabhavi).
0043-1354/$ - see front matter & 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.watres.2006.04.022
 ARTICLE IN PRESS
2350 WAT E R R E S E A R C H
(Sostar-Turka et al., 2005; Amjad, 1993; Lee and Leuptow, 2001;
Rautenbach et al., 2000; Townstand et al., 1992; Hoffman et al.,
1997). Most of the effluents from different industrial source
were used to be discharged directly in the soil or in ground
water. But due to the stringent environmental restrictions,
CPCB has become more strict and has imposed very stringent
norms. Worldwide scarcity of water is also another incentive
for recovering pure water from such industrial effluents.
However, for the treatment of an effluent by conventional
methods like aerobic and non-aerobic digestion, the ratio of
biological oxygen demand (BOD) to COD should be 40.6
(Chain and Dewalle, 1977). An effluent from the distillery
industry has high BOD/COD, which would cause the destruc-
tion of microorganisms that are useful in biodegradation. In
their effort to conform to discharge norms, Indian distilleries
employ various forms of primary, secondary and tertiary
treatment. The typical treatment sequence is screening or
equalization, followed by biomethanation. The biometha-
nated effluent is occasionally subjected to a single- or two-
stage aerobic treatment through the activated sludge (Malina
and Pohaland, 1992), trickling filters or even a second stage of
anaerobic treatment in anaerobic lagoons. Ferti-irrigation and
biocomposting with sugarcane press mud are the most widely
used options for effluent disposal. However, these methods
are highly energy intensive and hence quite expensive. These
disadvantages emphasized the need for further research
using novel separation methods. In this situation, mem-
brane-based separation techniques such as RO and NF would
yield excellent results when applied (Noble and Stern, 1995;
Rautenbach and Albrecht, 1989). The effectiveness of NF
membrane processes in water and wastewater treatment is
generally acknowledged and has now become the most
reliable standard technique. Hybrid techniques are also quite
popular. The main objective of this study was to purify the
distillery wastewater by removing the color and the con-
taminants by the combined use of NF and RO hybrid process.
The effect of process variables such as feed pressure and feed
Distilled Yeasts
Molassese
CO2
Free
Fermenter Fermenter
Fig. 1 – Schematic of production of distillery spent wash.
40 (2006) 2349– 2356
concentrations on membrane modules was investigated. The
results are presented for the waste effluent samples collected
from the local distillery industries.
2. Materials and methods
2.1. Wastewater generation pattern in a distillery
Surface water is the source of raw water supply for distillery
industries. Each liter of alcohol produced in India generates
about 15 L of spent wash. Even though wastewater is
generated at various stages of alcohol production, wastewater
from the fermenter sludge, spent wash and spent lees are the
main contributors to pollution and the generation involves
three main steps, viz., feed preparation, fermentation and
distillation, as shown in Fig. 1. In feed preparation, molasses
is diluted with water to obtain a feed containing 15–16%
sugar. The pH is adjusted, if required, by the addition of
sulfuric acid. Then, the diluted molasses solution is trans-
ferred to a fermentation tank where it is inoculated with
yeast, typically 10% by volume. The mixture is then allowed to
ferment anaerobically under controlled conditions of tem-
perature and pH. The process involves:
(a) Conversion of sucrose to glucose and fructose:
Invertase
C12 H22 O11 þ H2 O
! C6 H12 O6 þ C6 H12 O6 . (1)
(b) Fermentation of glucose to alcohol, releasing carbon
dioxide and heat:
Zymase
C12 H12 O6 þ H2 O
! 2C2 H5 OH þ 2CO2 þ 23:5 kcal: (2)
Once the fermentation is complete, yeast is separated by
settling and the cell-free broth is taken for distillation.
Distillation proceeds with heating the cell-free fermented
Rectifying
Column Alcohol
55%
Analyser Column
Spent Wash
Spent less
 ARTICLE IN PRESS
WAT E R R E S E A R C H
broth to about 90 1C, and is sent to the de-gasifying section of
the analyzer column. The bubble cap fractionating column
removes any trapped gases (CO2, etc.) from the liquor, which
is then steam heated and fractionated to give 40% alcohol.
The bottom discharge from the analyzer column is the main
effluent, spent wash. Water consumption in process applica-
tions like yeast propagation, molasses preparation, steaming,
etc., is in the range of 14.5–21.4 L/L of alcohol production.
Water consumption in non-process applications such as
cooling water, steam generation, making potable liquor etc.,
is much higher, i.e., ranging between 102.65 and 240 L/L of
alcohol production.
2.2. Materials
The commercial NF and thin-film composite (TFC) polyamide
RO membrane in spiral wound configuration was purchased
from Permionics, Vadodara, India. The membrane was
specified for seawater desalination with catalogue designa-
tion Perma PPT-9908, effective area 2.5 m2, module length
40 inches and diameter 2.4 inches. The pure water flux was
specified to be 90 L/(h m2) at 55.2 bar feed pressure and 25 1C.
The standard NaCl salt rejection under these conditions was
99.4% for 32,000 ppm feed concentration for the pH range of
2–11 for the operation.
The effluent sample was collected from the S.L.N Dis-
tilleries, Garag, Dharwad, India. Tetrasodium EDTA, hydro-
chloric acid and sodium bisulfate for membrane cleaning and
storage were purchased from S.D. Fine Chemicals, Mumbai,
India. KCl and NaCl for the atomic absorption spectrometer
(AAS) standard preparation were obtained from Himedia,
Mumbai, India, and all were of analytical grade. Deionized
water for cleaning and analytical standards preparation was
generated from the same RO system.
2.3. Pre-treatment
The effluent collected from the distillery industry is highly
acidic with a pH range of around 3. Hence, it was neutralized
2 3
Retentate
6
2 3
Pump
1 2
1. Feed
2. Control valve
3. Pressure guage
Fig. 2 – Schematic of NF and RO pilot plant.
4 0 (200 6) 234 9 – 235 6 2351
using sodium hydroxide. The neutralized solution has a lot of
suspended solids, so the filtration was carried out to remove
the suspended particles with a fine-pore thin cloth. This pre-
filtrate was used as feed.
2.4. Pilot plant description
A pilot-scale skid-mounted system as shown schematically in
Fig. 2 was built by incorporating a commercial TFC polyamide
RO membrane with an inlet operating pressure of 400 psi and
TFC NF with an inlet pressure of 300 psi inside an FRP
cylindrical pressure vessel; 2.5 inches diameter  21 inches
length was the size of each module. A feed tank of 30 L
capacity made of stainless steel-316 was provided for storage
and supply of effluent to the system as well as collection of
the recycled concentrate. A cooling coil was installed inside
the feed tank for circulating cold water to maintain constant
feed temperature within the range of 27–29 1C. A high-
pressure pump capable of maintaining a pressure of 100 bar
was installed for transporting the feed liquid throughout the
system. A 2 HP single-phase motor ran the pump. A restrict-
ing needle valve was provided on the concentrate outlet of the
membrane pressure vessel to pressurize the feed liquid to a
desired value, as indicated by a pressure gauge installed at the
upstream of the valve.
Permeate and concentrate flow rates were measured by two
glass rotameters containing metal floats. An adjustable safety
valve was fixed on the pump discharge line to prevent the
system pressure from exceeding the maximum desired value
(70 bar). All the accessories were connected by the 0.5 inches
outer-diameter stainless steel-316 piping in the high-pressure
region, whereas the low-pressure outlets from concentrate
and permeate sections were made of PVC braided tubing.
2.5. Experimental procedure and sampling
Thirty liters of the pretreated feed was poured in the feed
tank after thoroughly cleaning the membrane systems and
wetting with deionized water. The high-pressure pump was
3
Pump
NF Permeate
4
3 RO Permeate
4. NF module
5. RO module
6. Thermocouple
 ARTICLE IN PRESS
2352 WAT E R R E S E A R C H
employed to transport the feed to the spiral wound mem-
brane module and the system pressure was adjusted at a
value greater than the osmotic pressure, by means of a
restricting needle valve. With a control valve, the retentate
flow rate was maintained constant (10 L/min) throughout the
experiments, to ensure the steady hydrodynamic conditions
inside the membrane module. The feed pressure was varied
from 0 to 70 bar and keeping the feed TDS concentration (for
NF 206,000 ppm and for RO 10,000 ppm) constant, permeate
samples were collected after 10 min with every 6.9 bar
increase in the feed pressure. Flux was noted by collecting
the permeate in a measuring jar for a period of 2–3 min.
Around 300–400 mL of permeate was collected in each
pressure increase for a thorough analysis. The experiment
was repeated twice with every feed sample for reproducibility
of the permeate characteristics.
2.6. Analytical methods
The feed and retentate of the experimental samples were
analyzed for COD, TDS, conductivity, pH and other contami-
nants by the different methods. Conductivity and pH values
were measured by the conductivity/pH meter (JENWAY 4330,
UK), TDS was measured by TDScan 1 meter (Singapore),
cations were detected by AAS (GBC Avanta, model 932,
Victoria, Australia), COD was determined by open-reflux
method and chloride was estimated by the titration method.
2.7. Flux and percent rejection
Nanofiltration, in concept and in operation, is much the same
as reverse osmosis. However, the key difference is the degree
of removal of monovalent ions. NF is not as fine a filtration
process as RO, but it also does not require the same energy to
perform the separation. In RO membrane process, separation
performance of the membrane is judged by the percent
rejection (%R) of TDS, COD and other feed components, which
is calculated as (Noble and Stern, 1995; Rautenbach and
Albrecht, 1989)
 
Cp
%R ¼ 1
 100, (3)
Cf
where Cp represents the concentration of a particular
component in the permeate and Cf is its feed concentration.
The flux (J) is the volume of the permeate (V) collected per
unit membrane area (A) per unit time (t):
V
J¼ . (4)
At
2.8. Membrane fouling and its prevention
Fouling of the membrane surface is the bane of membrane
operations. The concentration of calcium in the form of
carbonate and sulfate and hardness in the distillery effluent
was reasonably high, which would cause scale formation on
the membrane surface, thereby causing subsequent fouling.
There are two types, colloidal flocculation or inorganic scaling
above the membrane surface, and adsorption of organics to
40 (2006) 2349– 2356
the membrane. Fouling layers are removed by using appro-
priate cleaning procedures. The most common procedures
are by using caustic detergent for the removal of dirt, oils and
colloidal material, acids for metal hydroxides, and oxidizing
agents for adsorbed organics. A dosage of 10 ppm of sodium
hexametaphosphate antiscalant to the RO feed helped in
preventing CaSO4 scaling.
The CaCO3 scaling was controlled by treating the mem-
brane at the end of the day’s study with an acid solution (HCl,
pH ¼ 2), which converts the carbonate to CO2 and also
removes other metal precipitates and mineral scales. Wash-
ing with a 1% aqueous solution of tetrasodium EDTA, a
chelating agent useful in removing organics and silt, was
done on alternate days. To prevent biological fouling, the
membrane was washed thoroughly with deionized water and
stored in a 0.5% solution of sodium bisulfate (NaHSO3) at the
end of the experimental runs. The above methods were
efficient in restoring the water flux.
3. Results and discussion
Specifications of the distillery spent wash used for this study
are given in Table 1. Flow rates of the permeates at different
pressures were determined with their respective electrical
conductivity, pH and for all other contaminants. Earlier
laboratory studies have shown that the presence of fulvic
acid lowers the optimum pH for turbidity removal and
increases the amount of coagulant required to treat the dilute
clay suspensions (Hall and Packham, 1965; Narkis and
Rebhun, 1975). However, the coagulant dose and optimum
pH for color removal are independent of the presence of clay.
As humic acid and certain metal complexes of humic
substances are poorly soluble at the pH of potable water,
they will be responsible for a portion of the turbidity in a
water sample. Another constituent of the suspended solids
fraction of water is a complex of clay particles with humic
substances. Furthermore, as dissolved humic substances in
water exist predominantly as colloidal dispersions, optical
measurements of turbidity are influenced by particles in the
colloidal size range.
3.1. NF experiments
In this study, NF experiments were carried out mainly to
remove the color. NF module effectively removed the particles
Table 1 – Characteristic contaminants of distillery spent
wash
Parameter
pH 3.0
Color Dark brown
Conductivity (mS/cm) 346
TDS (mg/L) 51,500
COD (mg/L) 100,000
Potassium (mg/L) 2050
Chloride (mg/L) 4900
 ARTICLE IN PRESS
WAT E R R E S E A R C H 4 0 (200 6) 234 9 – 235 6 2353

Fig. 3 – Untreated and NF-treated distillery spent wash.

Fig. 6 – Concentration of chloride as a function of pressure

for NF process.

Table 2 – Characteristics of NF permeate

Parameter

pH 6.5–7.5
Color Colorless
Conductivity (mS/cm) 15.06
TDS (mg/L) 9050
COD (mg/L) 2900
Potassium (mg/L) 1750
Chloride (mg/L) 2650

Fig. 4 – TDS as a function of pressure for NF process.

from 1 to 6, for the original effluent and the NF-treated

samples. The left with number 1 is the wastewater sample
and samples numbered 2–6 are permeates after NF at
20–70 bar pressures. Feed with a TDS concentration of
51,500 ppm was run mainly to remove the color. At the
optimal pressure range of 30–50 bar, permeate was transpar-
ent. Thus, our analysis showed that the permeate concentra-
tion was reduced to 9050 ppm of TDS, conductivity from 346
to 15.06 mS/cm, and chloride concentration 4900 to 2650 ppm
(Figs. 4–6). This indicates high efficiency of the NF membrane
module in rejecting the possible bivalent and trivalent ions
that include calcium, magnesium, and iron-like trace metals.
As shown in Fig. 3, sample number 6 has retained some color
due to the penetration of suspensions as a result of high
applied pressures (70 bar). Table 2 shows characteristics of NF
permeate.
Fig. 5 – Conductivity as a function of pressure for NF process.

in the colloidal size range. As the distillery wastewater has a 3.2. RO experiments
very dark brown color, the pre-treated effluent samples free
from suspended particles were used as feed for the NF RO is suitable for the remaining ions and larger species from
experiment with the characteristics as shown in Table 1. Fig. 3 dye bath effluents. Several parameters have been studied
displays the screening of six samples with numbers starting here.
 ARTICLE IN PRESS
2354 WAT E R R E S E A R C H 40 (2006) 2349– 2356

Table 3 – Effect of pressure on RO permeate characteristics

Feed pressure (bar) Conductivity (mS/cm) Concentration (ppm)

TDS COD Potassium Chloride

Atmospheric 15.06 9050 2900 1750 2650

20 2.56 1535 125 11.6 120
30 0.432 259 96 4.7 180
40 0.359 236 66 3.5 200
50 0.198 119 30 1.7 210
60 0.143 86.3 26 1.8 230
70 0.233 138.8 32 2.1 450

Fig. 7 – Comparison of pure water flux (J) to that of

wastewater (W) as a function of pressure for RO process. Fig. 9 – Variation in COD concentration as a function of
pressure for RO process.

Fig. 8 – Variation in TDS concentration as a function of Fig. 10 – Variation in potassium concentration as a function
pressure for RO process. of pressure for RO process.

3.2.1. Effect of feed pressure on permeate characteristics
Effect of pressure on the removal efficiency of different ions
through RO module is shown in Table 3. A comparison of pure
water flux with feed flux shown in Fig. 7 clearly demonstrates
the effect of osmotic pressure in RO transport. The flux for
distillery spent wash feed increased almost linearly from 20
to 70 bar. Even though small decline in flux rate of pure water
was obtained, the comparison shows that the performance of
the membrane was not affected by the fouling phenomenon.
Figs. 8 and 9, respectively, show that the amount of TDS in the
permeate reduced drastically, while COD decreased about 20-
fold. The percent rejection of TDS increased from 83 to 99.06,
 ARTICLE IN PRESS
WAT E R R E S E A R C H
Fig. 11 – Variation in chloride concentration as a function of
pressure for RO process.
Fig. 12 – Variations in TDS concentration of RO permeate
with feed concentration (at a constant pressure of 50 bar and
a temperature of 25 1C).
whereas COD increased more significantly from 95.6 to 98.96
for a pressure of 50 bar. The change in concentration of
potassium with a high rejection (99.9%) in permeates as a
function of applied pressure is shown in Fig. 10. The
concentration of potassium in the permeate decreased
exponentially with pressure up to 60 bar and a slight increase
is observed at the end. An almost similar trend was observed
for potassium (99.9%) and chloride ion rejection (96.8%), as
evident from Figs. 10 and 11. Even though the rejection of
contaminants at 60 and 70 bar pressure is desirable under the
minimum contaminant levels, the figures show an increase in
concentration of each contaminant, which indicates the
possible penetration of ions through the membrane pores at
high pressure.
3.2.2. Effect of feed concentration on permeate characteristics
To ensure the feasibility of membranes process, effluents
from different distillery industries with different raw materi-
4 0 (200 6) 234 9 – 235 6 2355
als were used. However, TDS along with other contaminates
may vary, as NF permeate collected at varying applied
pressures was having a long range of contaminant character-
istics. The effect of feed concentration on permeate char-
acteristics was studied by keeping a constant feed pressure of
50 bar and maintaining the temperature at 25 1C. The RO
permeate for different sets of feed concentrations had good
analytical characteristics. The membrane performance was
reasonably good, i.e., TDS concentration was up to around
30,000 ppm. Fig. 12 shows that TDS rejection increased
exponentially to 99.5% for a TDS concentration of
28,300 ppm, while the rejection rate was decreased to
99.26% for a TDS concentration of 32,000 ppm and to 99.17%
for that above 36,300 ppm. Along with the decreased solute
rejection, a decrease in flux was also observed, indicating the
possible concentration polarization of the solute, which
increases osmotic pressure at the membrane surface and
causes a loss in effective trasmembrane pressure (Amjad,
1993).
4. Conclusions
As the cost of wastewater disposal increases, more emphasis
is being placed upon the recovery and recycling of the
valuable chemicals contained within these streams. The
present membrane-based separation study demonstrated
that the hybrid NF and RO processes can be successfully
employed for the removal of color and contaminants in the
distillery spent wash and for a good water recovery rate. Due
to high fluxes obtained, significant rejection rates of TDS,
COD, potassium etc., were achieved. The absence of heat
application and a high rate of mass transfer generated by RO
shows that a large amount of water can be permeated
economically instead of being vaporized by the energy-
intensive evaporation processes or steam distillation using
the tall towers. The reclaimed water by NF and RO processes
could be reused for either municipal or industrial purposes.
The system is very simple to operate, with a minimum of
pumps and controls in addition to low requirements for
operator attention. Typical daily maintenance includes mon-
itoring of the performance parameters. This hybrid process
has proven its potential technological applicability for treat-
ing domestic and other wastewaters, by producing excellent
effluent quality for safe and environmentally benign dis-
charge, even under variable feed conditions. Moreover, the
ability to recover valuable materials, recycle water reducing
fresh water consumption and wastewater treatment costs,
using a point-source approach for minimum capital costs,
small disposal volumes that will minimize the waste disposal
costs, reduction in regulatory pressures and fines improved
the heat recovery systems.
Acknowledgements
The authors thank the university grants commission (UGC),
New Delhi, India, for a major funding (Grant no. F1-41/2001/
CPP-II) to establish the Center of Excellence in Polymer
Science (CEPS) at Karnatak University, Dharwad. Dr. K.M.
 ARTICLE IN PRESS
2356 WAT E R R E S E A R C H
Hosamani thanks the Department of Science and Technology,
New Delhi, India (Grant no. SR/S1/OC-08/2005), for financial
support.
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