Wwproj 226 12.08am

CHAPTER I
Development of Wastewater Treatment Design for Distillery Industry: 1

Destileria Limtuaco & Co., Inc.
AMANO | DIONISIO | MENDOZA | REDUBLO | SIM
INTRODUCTION
Molasses-based production of ethanol is among the main industries in
the Philippines (Rollon, Dionisio, 2015). Ethanol distillery plants generate
large volumes of wastewater in the range of 13-15 m 3 per m3 of product
ethanol. It has a dark brown color which may not be easily removed by
common biological treatment processes. The brown color of distillery
wastewater has been attributed to recalcitrant polymeric pigments called
melanoidin (Alfafara et al., 2000). They are products of the Maillard reaction
of amino acids with carbohydrates, which is specifically the interaction of
amino acids with reducing sugars, sugar dehydration, and fragmentation of
the reducing sugar.
In perspective, the alcohol distilleries are growing extensively

worldwide due to widespread industrial applications of alcohol in chemicals,
pharmaceuticals, cosmetics, beverages, food, and perfumery industry. The
industrial production of alcohol products by fermentation results in the
discharge of large quantities of high-strength liquid wastes. Distillery
wastewater is one of the most polluted waste products to dispose because of
the low pH, high temperature, dark brown color, high ash content, and high
percentage of dissolved organic and inorganic matter with high biochemical
oxygen demand (BOD) and chemical oxygen demand (COD) values
(Kharayat, 2012). Its characteristics are depending on the feed stock and
various aspects of the production process.
In this study, a preliminary comprehensive review of the methods for

handling distillery wastewater is presented. Although a number of treatment

schemes are being used or have been proposed, there is no widespread
agreement on the most suitable methods. These discrepancies reflect in part
the wide variations in the characteristics of distillery wastewater—in turn
these are the result of different raw materials, agricultural practices, and
distillery operating techniques (Pant, 2007; Sheehan, Greenfield, 1980).
STATEMENT OF THE PROBLEM
Distillery wastewater (DWW) should be adequately treated for the

degradation and detoxification of organic and inorganic pollutants prior to its
final discharge into the environment. Physical and chemical treatment
options alone such as coagulation, flocculation, and adsorption have not
been very successful until now and are not feasible to meet the discharge
standards set by various environmental protection agencies (Chowdhary,
Raj, Bharagava, 2017; Patyal, 2015). However, biological methods like
aerobic and anaerobic treatment processes were found somewhat capable to
reduce BOD/COD load of DWW, but the substantial concentration of organic
and inorganic pollutants and dark color left behind require further treatment
(Safari et al., 2013).
Anaerobic digestion is still the most appropriate approach for the

mitigation of high organic carbon content for DWW (Chowdhary, Raj,
Bharagava, 2017). High strength brewery effluents are traditionally treated
on-site in anaerobic sludge blanket (ASB) reactors, fixed film reactors, and/or
completely stirred tank reactors (CSTR) (Weber, Stadlbauer, 2015). The
limitations of anaerobic treatment processes are the requirement of high
dilution due to the presence of many antimicrobial compounds such as 2,3-
dimethylpyrazone, 2,2-bifuran-5-carboxylic acid, 2-nitroacetophenone,

among others (Jimenez et al., 2004; Bharagava, Chandra, 2010). Despite
high COD removal from diluted DWW, these chemical inhibitors remain in the
DWW even after the digestion process. Meanwhile, CSTRs, which are
anaerobic reactors equipped with a gas collection system, require long
hydraulic retention times (HTR) to achieve high DWW degradation as HTR is
determined by the growth rate of the microorganism growing in the medium.
Therefore, a further pre- or post-treatment is required to remove the

remaining dark color, COD, and BOD, but it is preferable to treat the DWW
anaerobically first and then with other treatment methods. It is thus the
responsibility of this study entitled “Development of Wastewater
Treatment Design for Distillery Industry: Destileria Limtuaco & Co.,
Inc.” to design a DWW treatment plant that will aim to address the problems
arising in conventional anaerobic digestion processes.
Objectives of the Study
General
To design a wastewater treatment plant of Destileria Limtuaco & Co.,

Inc. with wastewater effluents complying the standards set by DENR
Administrative Order 2016-08.
Specific
This study also aims:
To assess the wastewater treatment procedure of Destileria Limtuaco &

Co., Inc;
To determine the standard operating procedures of the said company
in compliance with DAO 2016-08

To conduct a comprehensive review of related literature and studies
that will aid in the design proper of the wastewater treatment plant in
terms of equipment efficiencies, etc.
To recommend improvements to wastewater treatment procedures of
the said company
To provide corrective actions if necessary
Scope and Limitations
Scope of the Study
This study will aim to design an improved wastewater treatment design

for Destileria Limtuaco & Co., Inc, and in general, for other distillery
companies that will find the researchers’ design applicable for a particular
company’s use. It is the duty also of this study to determine, if possible, the
effectiveness of the existing practices of Destileria’s wastewater treatment
procedures in terms of (1) promoting water quality standards with respect to
DAO 2016-08 and (2) comparing the improved wastewater treatment design
against the former practices.

Limitation of the Study
The study may face a constraint in gathering pertinent influent and

effluent data due to concerns of confidentiality on the part of the company.
The researchers’ may be restricted from visiting the actual wastewater
treatment site because of protocols. In terms of inorganic compound
contents of the wastewater, the researchers’ may not be able to quantify this
parameter.

CHAPTER II

LITERATURE & STUDIES
II.1 Wastewater in the Distillery Industry
II.1.1 Global
II.1.2 Local
II.2 Pilot Plant: Destileria Limtuaco & Co., Inc.
II.2.1 Company Profile
II.2.2 Raw Wastewater Characteristics
II.2.3 Receiving Water Bodies Nearby
II.3 Beneficial Uses of Class C Water Body as per Dao 2016-08
II.4 Effluent Standards of Class C Water as per DAO no. 35
II.5 Proposed Treatment Technologies
II.5.1 Anaerobic Lagoon
II.5.1.1 Anaerobic Treatment
II.5.1.2 Efficiency
II.5.1.3 Anaerobic Lagoon Mechanism
II.5.2 Upflow Anaerobic Sludge Blanket Reactor
II.5.2.1 UASB Reactor Mechanism
II.5.2.2 Efficiency
II.5.3 Aerobic Treatment (Trickling Filter)

II.5.3.1 Trickling Filter Mechanism
II.5.3.2 Efficiency
II.5.4 Aerobic Lagoon
II.5.4.1 Aerobic Lagoon Mechanism
II.6 Alternative Treatment Methods for Distillery Wastewater
II.6.1 Physical Treatment
II.6.2 Chemical Treatment
II.6.3 Anaerobic Treatment
II.6.4 Aerobic Treatment

II.1 WASTEWATER IN THE DISTILLERY INDUSTRY
II.1.1 GLOBAL
Distilleries generate wastewater at various stages in the manufacturing

process as distillation, condenser cooling, fermenter cooling, fermentation
and washing stages. 88% of its raw materials are converted into waste and
discharged into the water bodies, causing water pollution hence, Jain, et. al.
(2012) categorized distilleries to be among the most polluting industries
generating large volume of wastewater known as spent wash.
In the distillery, for every litre of alcohol produced, about 15% of spent
wash is released (Ravikumar et al. 2007). In India, there are about 315
distilleries with a total capacity of 3250 million litres of alcohol per annum
with 40.4 billion litres of effluent, annually (Mohan,a et al. 2009). In China, it
is estimated that 11–15 L of distillery wastewater can be generated from 1 L
of Chinese liquor production (Zhu, et al. 2015).
II.1.2 LOCAL

Molasses based production of ethanol is among the main industries in
the Philippines. Because the sugar industry is a major agricultural sector in
the Philippines, its byproduct, molasses, is the main feedstock for the alcohol
distilleries in the country. These distilleries produce ethyl alcohol or ethanol,
an ingredient used in the manufacture of alcoholic drinks like gin and rum
(International Institute for Energy Conservation, 2007).
Ethanol distillery plants generate large volume of high strength

wastewater which contains high levels of organic matter that is of serious
environmental concern (Rollon, A.P. & Dionisio, M.G., 2015). One liter of
alcohol produced generates 10 to 15 liters of wastewater (International
Institute for Energy Conservation, 2007). Effluents from molasses-based
distilleries mainly contain dark colored molasses spent wash (MSW). MSW is
a polluting waste product because of its low pH, high temperature, dark
color, high ash content and high percentage of dissolved organic and
inorganic matter (Tansengco M.L. et.al., 2016). The primary sources of
pollutants in a distillery plant are the stillage, cooling water from fermenter
and condenser, and wastewater from fermenter (Pant, D. & Adholeya, A.,
2007).
II.2 DESTILERIA LIMTUACO & CO., INC.
II.2.1 COMPANY PROFILE
Destileria Limtuaco & Co. Inc., located at E.

Delos Santos Avenue, Quezon City, Metro Manila, is
the oldest distillery in the Philippines which was
established in 1852 by a Chinese immigrant named
Lim Tua Co. It is known as premium distillers of
whisky, brandy, london, dry gin, rum, vodka,
cocktails, liquor, and herbal wine.
As Destileria Limtuaco continues to embrace

the challenges of the modern times, it strives to

maintain the quality of which its products were known. As part of this
commitment, the company was accredited by Technischer
Überwachungsverein (TUV) organization as an ISO certified production plant.
This enables the company to maintain consistent quality checks and

production schedules. Furthermore, the ISO seal attests that Destileria
Limtuaco is a company that complies with international standards. As part of
its continuing commitment to quality, the company’s quality management
system underwent another certification audit by TÜV SÜD Asia Pacific Ltd.
last March, 2009.
Destileria Limtuaco & Co., Inc. is proud to be among the first companies
worldwide to be certified under the latest ISO 9001:2008 standards for its
ability to consistently provide products that meet both customer and
applicable regulatory requirements.
In a study ‘Treatment of Molasses-Based Distillery Wastewater in a

Pilot- Scale Anaerobic Sequencing Batch Reactor (ASBR)’ by Tansengco M.L..,
et.al. (2016), the researchers used the data collected from Destileria
Limtuaco & Co., Inc. Distillery wastewater had a pH of 4.58, total solids of
15.25% and COD of 171,000 mg/L. The characteristics of raw distillery
wastewater is presented in Table 1.
II.2.2 RAW WASTEWATER CHARACTERISTICS
Table 1. Characteristics of Raw Wastewater of Destileria Limtuaco &

Co., Inc.
PARAMETERS UNIT DISTILLERY WASTEWATER
Color TCU Dark brown

Odor - Burnt sugar
pH - 4.58
COD mg/L 171,000 ± 1.53
BOD mg/L 42, 000 ± 5.66
Total Suspended mg/L 7,200 ± 0.58

Solids
Total Volatile Solids mg/L 81.68 ± 0.61
II.2.3RECEIVING WATER BODIES NEARBY

There are three water of bodies near Destileria Limtuaco & Co., Inc.
plant which are Tullahan River, Marikina River and Pasig River. Among the
three, Tullahan river is the nearest to the distillery plant.
The Tullahan River is located to the north of Manila and has an

approximate length of 7.6 miles or 15 kilometers. It starts at the La Mesa
Reservoir in Quezon City and flows through Malabon and Valenzuela and
empties into the Manila.
According to Environmental Management Bureau (EMB), Tullahan River

is classified as Class C water body.
II.3 BENEFICIAL USES OF CLASS C WATER BODY AS PER DAO 2016-08
According to DENR Administrative Order (DAO) 2016-08 Standards, the

beneficial uses of Class C water body are as follows: (1) fishery water for the
propagation and growth of fish and other aquatic resources, (2) recreational
water class II – for boating, fishing or similar activities, and (3) for agriculture,
irrigation, and livestock watering.
II.4 WASTEWATER CHARACTERISTICS AND EFFLUENT STANDARDS

The characteristics of Destileria Limtuaco & Co., Inc. raw wastewater is
shown in Table 2 together with corresponding effluent standards as per DAO
no. 35.
Table 2. Limtuaco Wastewater Characteristics and Effluent

Standards
Distillery Wastewater, Effluent

Standards
Paramete Unit Destileria Limtuaco & Co.,
rs Inc. of Class C
Water
BOD mg/L 42,000 50
COD mg/L 171,000 100
Color TCU Dark brown 150
pH - 4.58 6.0-9.5
TSS mg/L 7,200 100
II.5 PROPOSED TREATMENT TECHNOLOGIES
Our proposed treatment processes for the raw wastewater of the

distillery Disteleria Limtuaco & Co. Inc., to meet the effluent standards of
class C water listed on DAO 35 are as follows:
1. Anaerobic Lagoon
2. Upflow Anaerobic Sludge Blanket Reactor
3. Trickling Filter
4. Aerobic Lagoon (2)

II.5.1 ANAEROBIC LAGOON
II.5.1.1 Anaerobic Treatment
Anaerobic wastewater treatment is an effective biological method for

treating many organic wastes. The microbiology involved in the process
includes facultative and anaerobic microorganisms, which, in the absence of
oxygen, convert organic materials into gaseous end products such as carbon
dioxide and methane. Methane gas produced in anaerobic processes
provides an economically valuable end product (Adams, C.E., et.al., 1999).
Furthermore, higher influent organic loading is possible for anaerobic

systems than for aerobic systems because the anaerobic process is not
limited by the oxygen transfer capability at high-oxygen utilization rates in
aerobic processes (Adams, C.E., et.al., 1999).
The high organic content of molasses spent wash makes anaerobic

treatment attractive in comparison to direct aerobic treatment. Therefore,
biomethanation is the primary treatment step and is often followed by two-
stage aerobic treatment before discharge into a water body or on land for
irrigation (Nandy et al., 2002).
Anaerobic treatment can be successfully operated at high organic

loading rates (Nandy et al., 2002). Furthermore, as compared to aerobic
treatment which converts 50% of the COD to sludge after treatment,
anaerobic treatment converts over half of the effluent COD into biogas which
can be utilized for steam generation in the boilers thereby meeting the
energy demands of the unit (Sennitt, 2005; Wilkie et al., 2000).
II.5.1.2 Efficiency
The performance and treatment efficiency of anaerobic process can be

influenced by thermal treatment of wastewater. According to Satyawali, Y. &
Balakrishnan, M. (2007), wastewater treated at lower temperature (170 °C)
showed 66% COD reduction which was nearly twice the removal obtained
with treatment at 230 °C.

Anaerobic lagoons are the simplest option for the anaerobic treatment
of distillery spent wash. It was reported that employing two anaerobic
lagoons in series resulted in final BOD levels up to 600 mg/l.
According to Turker, U., et.al. (2009), experimental results showed that

the installation of innovative anaerobic lagoons was able to reduce the BOD
and TSS concentrations to desirable values that fell within the discharge
limits of national and international effluent standards. The significant
improvement in BOD removal percentages increased the BOD removal
performance up to 93%, whereas the TSS removal performance increased to
84%.
II.5.1.3 Anaerobic Lagoon Mechanism
Anaerobic lagoons are the simplest option for the anaerobic treatment
of distillery spent wash (Satyawali, Y. & Balakrishnan, M., 2007). The
anaerobic lagoon is applicable to high-strength wastes (usually greater than
500 mg/l of BOD) and applications in which a highly purified effluent is not
required. In anaerobic lagoons, either the sulfate concentration must be low
(less than 100 mg/l), or the lagoon must be in a remote location.
An anaerobic lagoon is similar in construction to an aerobic lagoon in

levee dimensions and construction materials. The anaerobic lagoon,
however, usually requires less surface area than the aerobic facility. Since
oxygen transfer from the atmosphere is not important, the anaerobic lagoon
can be as deep as is practical. According to Shieh, W.K. & Nguyen, V.T., a
depth of at least 15 ft is recommended whenever groundwater
considerations and area geology permit. The relative depth of an anaerobic
lagoon provides improved heat retention. Furthermore, the lagoon should be
as long as practical (an efficient length to width ratio is 2:1).
The BOD loading rate in anaerobic lagoon design is 500 to 1000 lb BOD
per acre per day with an expected BOD removal efficiency of 50 to 80%. The
required detention time is between 30 and 50 days. The ideal Ph range for
the anaerobic process is 6.6 to 7.6, but lagoon efficiency is not significantly

hampered if pH is gradually increases to 9.0. Above pH 9.0, the efficiency
drops off rapidly. Sudden bursts of high and low pH also hinder lagoon
performance (Shieh, W.K. & Nguyen, V.T., 1999).
The anaerobic process functions optimally over two temperature

ranges: the mesophylic range of 85° to 100°F and the thermophilic range of
120° to 135°F. Only the mesophylic range, however, applies to an unheated
lagoon. The lagoon is optimally effective when the temperature range for
mesophylic operation is not violated. However, as temperatures decrease
below 85°F, the lagoon efficiency decreases only slightly until a temperature
of about 60°F is reached, at which point the efficiency drops off rapidly. This
temperature requirement is why the lagoon should be as deep as possible,
i.e., to maximize heat retention.
Anaerobic microorganisms do not require dissolved oxygen in the

water to function. They obtain their oxygen requirement from the oxygen
chemically contained in organic materials. Anaerobic decomposition involves
two separate but interrelated steps. First, the acid-producing bacteria
decompose the dissolved organic waste to organic acids, such as acetic,
propionic, and butyric acid. The organic acids are then further decomposed
by methane-producing bacteria to the end products of methane, carbon
dioxide, and water. Effective operation requires a balance between acid
production and breakdown because methane producers are sensitive to the
concentration of volatile acids.

II.5.2 UPFLOW ANAEROBIC SLUDGE BLANKET (UASB) REACTOR
II.5.2.1 UASB Reactor Mechanism
Anaerobic treatment systems such as UASB do not require an energy

consuming aeration system and can be constructed much simpler than
aerobic treatments. They convert the organic matter into biogas, which can
be recovered. The nutrient-rich effluent can be used for agricultural irrigation
(Rose, 1997). Sludge is even partly stabilised (mineralised) and can be used
as an organic soil fertiliser after composting or drying.
UASB Reactors are constructed out of concrete or another watertight

material and can be designed in a circular or rectangular way. Wastewater is
pumped from the bottom into the reactor where influent suspended solids
and bacterial activity and growth lead to the formation of sludge. The sludge
blanket is comprised of microbial granules (1 to 3 mm in diameter), i.e.,
small agglomerations of microorganisms that, because of their weight, resist
being washed out in the upflow. The microorganisms in the sludge layer

degrade organic compounds. As a result, gases (methane and carbon dioxide
i.e. biogas) are released. The rising bubbles mix the sludge without the
assistance of any mechanical parts. Upstream velocity and settling speed of
the sludge is in equilibrium and forms a locally rather stable, but suspended
sludge blanket (Sasse, 1998). Sloped walls deflect material that reaches the
top of the tank downwards. The clarified effluent is extracted from the top of
the tank in an area above the sloped walls. A gas-liquid-solids separator
(GLSS) separates the gas from the treated wastewater and the sludge
(Sanimas, 2005).
After several weeks of use, larger granules of sludge form which, in

turn, act as filters for smaller particles as the effluent rises through the
cushion of sludge. Because of the upflow regime, granule-forming organisms
are preferentially accumulated as the others are washed out. Fortunately,
these bacteria are also more efficient for biogas production than flocculated
biomass (Wendland, 2008).
Anaerobic digestion is widely accepted as the first treatment step in

distilleries. Wilkie et al. (2000) have reviewed the role of anaerobic digestion
in stillage (spent wash) treatment. Anaerobic digestion can convert a
significant portion of the COD to biogas, which may be used as an inplant
fuel, and also saves the energy that would be required for aeration using
aerobic treatment. At present, the anaerobic biological treatment of distillery
effluents is widely applied as an effective step in removing >50% of the COD
in the effluent stream (Wolmarans and de Villiers, 2002).
Upflow anaerobic sludge blanket (UASB) reactors can be found among

the list of common types of anaerobic reactors used for distillery effluent
treatment by Akunna and Clark (2000) and it has been widely adopted for
treatment of alcohol distillery wastewaters (Akarsubasi et. Al., 2006).
Advantages for the UASB process are the high loadings and relatively
low detention times possible for anaerobic treatment and the elimination of
the cost of packing material. Another major advantage is that the UASB
process is a proven process with more than 500 full-scale facilities in

operation. Limitations of the process are related to those wastewaters that
are high in solids content or where their nature prevents the development of
the dense granulated sludge (Tchobanoglous, 2003).

II.5.2.2 Efficiency
Table 3 Efficiency of UASB in Reduction of Wastewater

Characteristics
Parameter Reduction Efficiency Reference
COD 90-95% Tchobanoglous, 2003
II.5.3 AEROBIC TREATMENT (TRICKLING FILTER)
Following the primary treatment of molasses-based distillery

wastewater, it is recommended that a two-stage aerobic treatment follow
suite (Nandy et, al. 2006). This is mainly due to the high organic nature of
the molasses spentwash.
Aerobic treatment processes come in many forms, primarily the

suspended and attached growth systems. Although both serves their
purpose in their own manner, attached growth systems were found more
useful in industrial settings such as in the distillery wastewater treatment
processes prominently the trickling filters, with hybrid forms of aerobic
lagoons being employed (Shivajirao, 2012).
II.5.3.1 Trickling Filter Mechanism
Trickling filter is an attached-growth type of process in which

microorganisms attached to a medium are used for removing organic matter
from wastewater. Trickling filter uses packing medium over which the
wastewater is distributed. A rotary distribution mechanism distributes
wastewater from the top of the filter percolating it through the interstices of
the film-covered medium. The oxygen required for organic degradation is
supplied by air circulating through the filter.

The trickling filter treatment process occurs through the biological
degradation of organic material by bacteria and micro-organisms contained
in the zoogleal film on the filter media. As the wastewater moves through the
filter, the organic matter is adsorbed onto the film and degraded by a mixed
population of aerobic microorganisms. The microorganisms used are mainly
facultative bacteria that decompose the organic material in the wastewater
along with aerobic and anaerobic bacteria. It includes Achromobacter,
Flavobacterium, Psudomonas, and alcaligenes.
II.5.3.2 Efficiency
Anaerobically treated spentwash from molasses based distilleries has a

high organic content and requires further aerobic treatment (Shivajirao
2012). Aerobic treatment through trickling filter following the anaerobic
treatment reduces the BOD content of the molasses-based spentwash. The
trickling filter does this job through the use of wide array of media such as
rock, slag, plastics or the combination. Through a rock media, BOD removal
efficiency of 90 percent is feasible. This is achievable through low rate
operations involving a hydraulic loading of 0.02 to 0.06 gal/ft2-min and
organic loading of 0.005 to 0.025 lb/ft3-day. Trickling filter depth of 6 to 8 ft
was also employed for this purpose (Liu and Liptak, 1999). Veltz equation
and NRC Equation for single-stage system employing rock media could be
used for calculating dimensions of the trickling filter.
II.5.4 AEROBIC LAGOON
II.5.4.1 Aerobic Lagoon Mechanism

The post-anaerobic treatment stage effluent still has high organic
loading and is dark brown in color, hence it is generally followed by a
secondary, aerobic treatment. (Satyawali and Balakrishnan, 2006). For the
biological treatment of wine distillery wastewater, aerobic systems such as
aerated lagoons or activated sludge plants are commonly used to remove
the COD (Benitez et al., 1999)
Aerated lagoons are an extended aeration, activated sludge process

without sludge recycling. These systems usually require deeper stabilization
ponds than the other types of lagoons with depths varying from 3 m to 5 m.
This process is usually used for treating wastewater from both agricultural
and industrial sources. It is also used for removal of nitrogen from chemically
contaminated wastewaters. (United Nations Environment Programme)
II.6 ALTERNATIVE TREATMENT METHODS FOR DISTILLERY

WASTEWATER
Current treatment options used to treat distillery spent wash includes

physical, chemical, physicochemical and biological methods before its
disposal. The selection of treatment methods depends on various factors viz.

treatment efficiency, treatment cost, local geography, climate, landuse,
regulatory constraints, and public acceptance of the treatment.
II.6.1 Physical treatment
Physical treatment methods are used at the initial stage of effluent

treatment. Various physical treatment methods currently being used in
distillery wastewater treatment are screening, flow equalization mixing,
flotation, and sedimentation (Thakur 2006) Adsorption is also a one of the
most widely used physical method. Adsorption on activated carbon is widely
employed for removal of colour and specific organic pollutants. Physical
treatment is used to decrease suspended/settable solids from wastewater
which may be removed inexpensively via sedimentation by using the force of
gravity to separate suspended material, oil, and grease from the wastewater
(Jayanti and Narayanan 2004). Hamoda et al. (2004) reported removal of
total suspended solids (TSS) by passing wastewater through a fine granular
media such as sand, the particles are captured in the fine pores and sorbed
on the surface of the granular media. Nataraj et al. (2006) also reported that
membrane based nano-filtration and reverse osmosis processes can be used
to reduce the total dissolved solids (TDS), COD, and potassium (K +) content
of distillery wastewater by 99.80, 99.90, and 99.99%, respectively.
II.6.2 Chemical treatment
During chemical wastewater treatment, compound like chlorine (Cl 2),

oxygen (O2), ozone (O3), and permanganate (MnO4) are added to the
wastewater to oxidize the wastewater components into carbon dioxide (CO 2),
water, inorganic matter, and other harmless products (Benitez et al., 2003).
Coagulation and flocculation processes are used for rapid and economical

removal of suspended, inert, or undesirable colloidal materials in industrial
wastewater (Tatsi et al. 2003). Mohana et al. (2009) have reported that
melanoidins can be decolourized by various physiochemical methods.
Majority of these methods remove colour by either concentrating the colour
into sludge or by partial or complete breakdown of the colour molecules.
Adsorption is a physical process so discuss it in physical process paragraph.
Adsorption on activated carbon is widely employed for removal of colour and
specific organic pollutants.
Pikaev et al. (2001) reported that treatment of distillery wastewater

using iron sulfate (Fe2 (SO4)3) as a coagulant results, 40% removal of
wastewater pollutants. Beltrain de Heredia et al. (2005) also achieved 55%
reduction in COD by using integrated Fenton-coagulant/flocculation process
in distillery wastewater treatment. In another report, addition of ferrous
sulfate, aluminum chloride, calcium oxide, ferric chloride along with
coagulants reduced the colour to 95%, 74.4%, 80.2%, and 83%, respectively,
while COD was reduced as 78%, 61.3%, 39.8%, and 55%, respectively
(Chaudhari et al. 2007)

II.6.3 Anaerobic treatment
Anaerobic digestion is a natural process in which various microbial

species work together, in the absence of O 2, to transform organic wastes
through a verity of intermediates into biogas (Mata-Alvarez, 2003). During
anaerobic digestion, biomass and biogas are produced, while pathogenic
microorganisms and offensive organic matter are reduced. Therefore,
anaerobic digestion can be used both as a depollution tool and to produce
energy (Moletta, 2005). Anaerobic digestion of high strength wastewater
usually occurs in successive steps and is accomplished by four trophic
groups of bacteria (Ranade et al. 1999). These bacteria groups function in a
synergistic relationship and form a food chain, in which the final products are
CH4 and CO2 (Figure 3). There are a number of microorganisms that are
involved in the process of anaerobic digestion including acetic acid-forming
bacteria (acetogens) and methane-forming archaea (methanogens). There
are four key biological and chemical stages of anaerobic digestion:
hydrolysis, acidogenesis, acetogenesis, and methanogenesis.

Figure 1. Schematic diagram of anaerobic digestion indicating the process steps and the four
bacteria groups involved in the process (Garcia-Heras 2003).
Various anaerobic treatment devices have been used, viz. anaerobic

lagoons, anaerobic digester, anaerobic contact reactor, anaerobic filter, up
flow UASB, anaerobic fluidized, and expended bed reactor.
Anaerobic digestion is the most suitable option for the treatment of

high strength organic effluent. Anaerobic treatment is an accepted practice
and various high rate anaerobic reactor designs have been tried at pilot and
full-scale operation (Lata et al. 2002). The major advantages of anaerobic
treatment using up flow UASB is that besides treatment of the wastewater,
methane gas is also generated in this process which can be used as a fuel

specially in boilers, thus anaerobic treatment processes not only helps in
wastewater treatment but also lowers fuel consumption cost. Some of the
anaerobic systems being applied for treatment of distillery wastewater are
summarized in Table 6.

The performance and treatment efficiency of anaerobic process can be
influenced both by inoculum source and feed pre-treatment. Anaerobic

lagoons are the simplest option for the anaerobic treatment of distillery
spent wash. Rao (1972) reported that employing two anaerobic lagoons in
series resulted in final BOD levels up to 600 mg/l. Rao (1972) carried out the
pioneering research work in the field of distillery waste management by
studying the application of anaerobic lagoon treatment in two pilot-scale
lagoons in series, with overall BOD removal ranging from 82 to 92%.
Treatment of winery wastewater was investigated using an anaerobic
sequencing batch reactor (ASBR). The reactor was operated at an organic
loading rate (OLR) of 8.6 kg COD m−3 d−1 with soluble COD removal efficiency
greater than 98%, hydraulic retention time (HRT) of 2.2 days (Ruiz et
al. 2002)
Garcia-Calderon et al. (1998) reported the application of the down-flow

fluidization technology for the anaerobic digestion of red wine distillery
wastewater. The system achieved 85% total organic carbon (TOC) removal,
at an organic loading rate of 4.5 kg TOC m3 day−1. Up flow UASB reactor is
the most popular high rate digester that has been utilized for anaerobic
treatment of various types of industrial wastewaters (Akunna and
Clark 2000). Treatment by a UASB reactor resulted in 75% COD removal in
sugarcane molasses spent wash (MSW). Wolmarans and De Villiers (2002)
have also reported COD removal efficiency of greater than 90% over three
seasons in a UASB plant treating distillery wastewater. In another anaerobic
treatment method, fluidized bed reactors contain an appropriate media such
as sand, gravel, or plastics for bacterial attachment and growth. A two stage
process with an anaerobic filter followed by a UASB reactor was investigated
by Blonskaja et al. (2003). The acidogenic and methanogenic phases were
clearly separated ensuring better conditions for the methanogens. COD

reduction was 54% and 93% in the first and second stage, respectively. The
highest BOD removal is possible in open lagoon, whereas highest
biomethane produced is in up flow UASB bioreactor. Compared to aerobic
system, it has slow growth rate, mainly associated with methanogenic
bacteria. Therefore, it requires a long retention time, and also only a small
portion of the degradable organic waste is being synthesized to new cells
(Pant and Adholeya, 2007)
II.6.4 Aerobic treatment
Aerobic processes are biological treatment processes that occur in the

presence of oxygen. The aerobic environment in the reactor is achieved by
the use of diffused or mechanical aeration, which maintain the mixed liquor
in a completely mixed regime. Aerobic digestion is an alternative method of
treating the organic sludge's produced from various treatment operations. In
the conventional aerobic digestion (Coverti et al. 1993), the wastewater is
aerated for an extended period of time in an open, unheated tank using
conventional air diffusers, or surface aeration equipment (Hsu and
Shich 1993. According to Metcalf and Eddy Inc. (1995), there are two
variations in the aerobic digestion process, namely, conventional and pure
oxygen. Aerobic treatment systems are used mainly to remove the BOD of
these wastes. Partial reduction of BOD and COD is achieved in many
distilleries using biological treatment (Jawed and Tare 1999); Laubscher et
al. 2001); Wolmarans and De Villiers 2002); Coetzee et al. 2004)
Jackson et al. (2007) used a bioreactor system to treat distillery wastewater

with a two-week HRT. COD of the distillery wastewater was decreased from

2255 mg/l to a final value of < 150 mg/l. Some of the aerobic systems being
applied for treatment of distillery wastewater are summarized in Table 7.

Table 5 Some of the aerobic systems being applied for treatment of
distillery wastewater
The aerobic treatment of industrial wastewaters usually depends on the

oxidative activities of microorganisms. Although, a large number of
microorganisms, such as bacteria, cynobacteria, yeast, fungi, etc. have been
used for treatment of spent wash. Filamentous fungi can be of important
sources of phenolic-degrading organisms, as they frequently grow on wood,
utilizing lignin as a carbon source (Benitez et al. 1999); Coulibaly et
al. 2003); Mendonca et al. 2004)

CHAPTER III
Conceptual Framework
and Methodology

CONCEPTUAL FRAMEWORK
PHILIP
PINES country, the
As an agricultural
major crops produced
SUGARC COCONare:
CORN Important RICE
ANE UT
byproducts
MOLA : BAGA
UsesSSES
/ Feed SSE
BIOET stock
DISTI
for: ANIM
HANO LLER AL
FERM Lwastewater Y are generated
FEED
ENTE inCOND
these different stages:
BOTT
R ENSE FLOO
TYPICAL
SPENWASTE LING
COOL R R
CHARACTERISTICS
T PLAN
ING & COOLI WASH
COD: WASH
104,000-134,000 T
CLEA NG
BOD: 46,100-96,000
NING
TDS: 79,000-87,990
Total N: 1660-4200
Total P: 255-3038
pH: 3.9-4.3
All units are in mg/L

PHILIPPINES AS AN AGRICULTURAL COUNTRY
The Philippines is an agricultural country with a land area of 30 million

hectares, 47% of which is agricultural land. The total area devoted to
agricultural crops is 13 million hectares distributed among food grains, food
crops and non-food crops. Among the food crops, coconut, rice, corn and
sugarcane are the top four food crops cultivated.
According to Philippine Statistics Authority (PSA), sugarcane has the
highest volume production in 2016 amounting to 22,370,546.22 metric tons
(MT), followed by rice production of 17,627,244.82 MT. Coconut and corn
productions are 13,825,080.08 MT and 7,218,816.55 MT, respectively. Even
though rice is the most important staple food crop in the country, sugarcane
still has the highest volume production since the Biofuels Act of 2006 was
implemented. This was aimed at the sugar industry in the Philippines, which
is the major source of ethanol and domestic sugar, where government
requires the use of biofuels for transport to reduce the country's dependence
on imported fossil fuels and to mitigate greenhouse gas emissions..
(Department of Agriculture – Sugar Regulatory Administration, 2016).
OVERVIEW OF SUGARCANE INDUSTRY

The sugarcane industry in the Philippines has grown into a multi-
product industry with sugar, bioethanol and power as its major products. In
2015-2016, there are 27 operational sugar mills and 14 sugar refineries.
Presented below are the top sugar millers and sugar refineries in the
Philippines.

Table 1. Top sugar millers and sugar refineries (Capacity),
2014-2015
Sugarcane industry generates important by-products such as

molasses, bagasse, and sugarcane tops. Sugarcane bagasse and tops are
usually used as biomass energy sources. It is estimated that 1.17m tons of
sugarcane waste is recoverable as a biomass resource in the Philippines. In
addition, 6.4m tons of surplus bagasse is available from local sugar mills.
According to Food and Agriculture Organization, annual molasses
production output has averaged about 916 000 metric tons. Of this, about 67
percent is exported, 17 percent is used by the distilleries, and 16 percent is
for animal feed, etc. However, the implementation of Biofuels Law of 2006
increases the utilization of molasses for the production of bioethanol and for
distillery industry.
OVERVIEW OF DISTILLERY INDUSTRY

Molasses based production of ethanol is among the main industries in
the Philippines. Because the sugar industry is a major agricultural sector in
the Philippines, its byproduct, molasses, is the main feedstock for the alcohol
distilleries in the country. These distilleries produce ethyl alcohol or ethanol,
an ingredient used in the manufacture of alcoholic drinks like gin and rum
(International Institute for Energy Conservation, 2007)
Effluents from molasses-based distilleries mainly contain dark colored
molasses spent wash (MSW). MSW is a polluting waste product because of its
low pH, high temperature, dark color, high ash content and high percentage
of dissolved organic and inorganic matter (Tansengco M.L. et.al., 2016)
DISTILLERY INDUSTRY WASTE CHARACTERIZATION AND SOURCES
Ethanol distillery plants generate large volume of high strength
wastewater which contains high levels of organic matter that is of serious
environmental concern (Rollon, A.P. & Dionisio, M.G., 2015). One liter of
alcohol produced generates 10 to 15 liters of wastewater (International
Institute for Energy Conservation, 2007) The effluent is characterized by
extremely high chemical oxygen demand (COD) (80,000–100,000 mg/l) and
biochemical oxygen demand (BOD) (40,000–50,000 mg/l), apart from low pH,
strong odor and dark brown color (Central Pollution Control Board (CPCB),
2003).
The primary sources of pollutants in a distillery plant are the stillage,
distillation, cooling water from fermenter and condenser, and wastewater
from fermenter (Pant, D. & Adholeya, A., 2007)
In distillation is a two-stage process and is typically carried out in a
series of bubble cap fractionating columns. The first stage consists of the
analyzer column and is followed by rectification columns. The cell free

fermentation broth(wash) is preheated to about 90◦C by heat exchange with
the effluent (‘‘spent wash’’) and then sent to the degasifying section of the
analyzer column. Here, the liquor is heated by live steam and fractionated to
give about 40–45%alcohol. The bottom discharge from the analyzer column
is the spent wash. The figure above shows how distillery process works and
where the spent wash, and other wastes, are generated.
Table 2. Sample quantities and characteristics of wastewater

streams generated in a distillery

Table 2 lists the major wastewater streams generated at different stages in
the alcohol manufacturing process. Table 3 summarizes the typical
characteristics of spentwash
generated in Indian distilleries using sugarcane molasses. The main source of
wastewater generation is the distillation step wherein large volumes of dark
brown effluent (termed as spentwash, stillage, slop or vinasse) is generated
in the temperature range of 71–81 °C (Yeoh, 1997; Nandy et al., 2002; Patil
et al., 2003). The characteristics of the spentwash depend on the raw
material used (Mall and Kumar, 1997); also, it is estimated that 88% of the
molasses constituents end up as waste (Jain et al., 2002). Molasses
spentwash has very high levels of BOD, COD, COD/BOD ratio as well as high
potassium, phosphorus and sulfate content (Table 3).

Table 3. Characteristics of spentwash generated from cane molasses

METHODOLOGY
The method used in the study is descriptive and a pilot-scale is
designed. Data gathering was done to establish the viability of the study. The
information such as distillery wastewater effluent characteristics and
receiving body effluent standards were collected. Moreover, an analysis of
the exiting distillery wastewater treatment methods was conducted and a
novel method is proposed.
A. Data Gathering
i. Wastewater Effluent Data were collected from Destileria Limtuaco &
Co., Inc
ii. The receiving body is identified including the effluent standard
requirement
B. Comparative Analysis of Alternative Treatment Methods for Distillery
Wastewater
Exisitng and alternative distillery wastewater treatment methods were
analyzed.
C. Distillery Wastewater Treatment Method Proposal

A treatment method is proposed based on the analysis of literature and
studies as well as the existing distillery wastewater treatment methods and
aiming to solve the setbacks mentioned in the statement of the problem.
D. Designing and Computations

The equipment involved in the proposed treatment process were designed.
E. Data Analyses
The proposed treatment process was analyzed based on the specifications
obtained from the design and calculations, as well as the BOD, COD, and TSS
reductions in each stage.

RESEARCH DESIGN

Current status of Distillery Industry in
the Philippines
Related Literatures
Data Gathering
Designing & Computations
Analysis
PROPOSED WASTEWATER FACILITY FOR

DISTILLERY INDUSTRY

PROPOSED WASTEWATER TREATMENT FLOWCHART


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CHAPTER I

Development of Wastewater Treatment Design for Distillery Industry: 1

In perspective, the alcohol distilleries are growing extensively

In this study, a preliminary comprehensive review of the methods for

Development of Wastewater Treatment Design for Distillery Industry: 2

STATEMENT OF THE PROBLEM

Distillery wastewater (DWW) should be adequately treated for the

Anaerobic digestion is still the most appropriate approach for the

Development of Wastewater Treatment Design for Distillery Industry: 3

Therefore, a further pre- or post-treatment is required to remove the

Objectives of the Study

To design a wastewater treatment plant of Destileria Limtuaco & Co.,

This study also aims:

To assess the wastewater treatment procedure of Destileria Limtuaco &

Development of Wastewater Treatment Design for Distillery Industry: 4

Scope and Limitations

Scope of the Study

This study will aim to design an improved wastewater treatment design

Development of Wastewater Treatment Design for Distillery Industry: 5

The study may face a constraint in gathering pertinent influent and

Development of Wastewater Treatment Design for Distillery Industry: 6

Development of Wastewater Treatment Design for Distillery Industry: 7

II.1 Wastewater in the Distillery Industry

II.2 Pilot Plant: Destileria Limtuaco & Co., Inc.

II.2.1 Company Profile

II.2.2 Raw Wastewater Characteristics

II.2.3 Receiving Water Bodies Nearby

II.3 Beneficial Uses of Class C Water Body as per Dao 2016-08

II.4 Effluent Standards of Class C Water as per DAO no. 35

II.5 Proposed Treatment Technologies

II.5.1 Anaerobic Lagoon

II.5.1.1 Anaerobic Treatment

II.5.1.3 Anaerobic Lagoon Mechanism

II.5.2 Upflow Anaerobic Sludge Blanket Reactor

II.5.2.1 UASB Reactor Mechanism

II.5.3 Aerobic Treatment (Trickling Filter)

Development of Wastewater Treatment Design for Distillery Industry: 8

II.5.4 Aerobic Lagoon

II.5.4.1 Aerobic Lagoon Mechanism

II.6 Alternative Treatment Methods for Distillery Wastewater

II.6.1 Physical Treatment

II.6.2 Chemical Treatment

II.6.3 Anaerobic Treatment

II.6.4 Aerobic Treatment

Development of Wastewater Treatment Design for Distillery Industry: 9

Distilleries generate wastewater at various stages in the manufacturing

Development of Wastewater Treatment Design for Distillery Industry: 10

Ethanol distillery plants generate large volume of high strength

II.2 DESTILERIA LIMTUACO & CO., INC.

II.2.1 COMPANY PROFILE

Destileria Limtuaco & Co. Inc., located at E.

As Destileria Limtuaco continues to embrace

Development of Wastewater Treatment Design for Distillery Industry: 11

This enables the company to maintain consistent quality checks and

In a study ‘Treatment of Molasses-Based Distillery Wastewater in a

II.2.2 RAW WASTEWATER CHARACTERISTICS

Table 1. Characteristics of Raw Wastewater of Destileria Limtuaco &

PARAMETERS UNIT DISTILLERY WASTEWATER

Color TCU Dark brown

Development of Wastewater Treatment Design for Distillery Industry: 12

COD mg/L 171,000 ± 1.53

BOD mg/L 42, 000 ± 5.66

Total Suspended mg/L 7,200 ± 0.58