Accepted Manuscript

Title: Wastewater sludge stabilization using pre-treatment

methods

Author: Muzammil Anjum Naief H. Al-Makishah M.A.

Barakat

PII: S0957-5820(16)30081-7
DOI: http://dx.doi.org/doi:10.1016/j.psep.2016.05.022
Reference: PSEP 784

To appear in: Process Safety and Environment Protection

Received date: 15-12-2015

Revised date: 2-5-2016
Accepted date: 23-5-2016

Please cite this article as: Anjum, M., Al-Makishah, N.H., Barakat, M.A.,Wastewater
sludge stabilization using pre-treatment methods, Process Safety and Environment
Protection (2016), http://dx.doi.org/10.1016/j.psep.2016.05.022

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1 Highlights

2  Modification of conventional processes of sludge treatment.

3  Limitations of aerobic and anaerobic digestion of wastewater sludge.

4  Pretreatment approaches for sludge disintegration and solubilization.

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5  The combined pretreatment increases the efficiency of the process

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 Wastewater sludge stabilization using pre-treatment methods

Muzammil Anjum1, Naief H. Al-Makishah1, M.A. Barakat1,2

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Department of Environmental Sciences, Faculty of Meteorology, Environment and Arid Land

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Agriculture, King Abdulaziz University, Jeddah, Saudi Arabia

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2
Central Metallurgical R & D Institute, Helwan 11421, Cairo, Egypt

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ABSTRACT

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The production and management of sludge in wastewater treatment plants is a significant
environmental issue. Sludge is a complex material, treated primarily by biological stabilization
methods, i.e., anaerobic and aerobic digestion. However, the presence of complex organics,

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microbial flocs, extracellular polymeric substances, and various inhibitory compounds,
considerably hinders the efficiency of these processes. In order to overcome the effect of these
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rate-limiting factors, the literature proposes a number of pretreatment technologies, which can
be used either as single pretreatment methods, or in combination. The present review describes
both the anaerobic and aerobic digestion of sludge, and highlights the issues that limit the
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efficiency of the process. Emphasis is placed on the potential use of pretreatment methods,
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including: thermal; ultrasonic; microwave; Fenton; wet oxidation; photocatalysis and some
others. These pretreatment approaches demonstrate varying potential for sludge disintegration
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and solubilization under different circumstances (e.g., operating conditions and sludge
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composition). However, the ultimate goal is to improve the subsequent biological treatment of
sludge. In short durations, thermal, ultrasonic and microwave processes can efficiently
solubilize the components of sludge and disrupt the cell walls of microbial flocs. However,
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issues related to high levels of energy requirements render these processes uneconomical for
field application. The Fenton process can be used in combination with either bioleaching or
ultrasound. Visible-Photocatalysis pretreatment for sludge can improve the anaerobic treatment
of sludge and biogas production, with low energy demand.

Keywords: Sludge, stabilization, anaerobic digestion, aerobic digestion, pretreatment, combine

pretreatment, energy


Corresponding author: mabarakat@gmail.com

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 CONTENTS

1 ABSTRACT .............................................................................................................................................................2

2 1. INTRODUCTION.................................................................................................................................................4

3 2. SLUDGE PRODUCTION PROCESS AND COMPONENTS........................................................................................7

4 3. SLUDGE STABILIZATION PROCESSES..................................................................................................................8

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5 3.1. AEROBIC DIGESTION OF SLUDGE AND LIMITATIONS .......................................................................................... 9

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6 3.2. COMPOSTING ....................................................................................................................................................... 9
7 3.3. ANAEROBIC DIGESTION OF SLUDGE AND LIMITATIONS .................................................................................... 10

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8 4. FACTORS AFFECTING SLUDGE STABILIZATION.................................................................................................11

9 5. APPROACHES TO SLUDGE PRETREATMENT .....................................................................................................13

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10 5.1. SINGLE PRE-TREATMENT APPROACH ............................................................................................................. 13
11 5.1.1. Thermal Hydrolysis.................................................................................................................................. 14
12 5.1.2. Ultrasound Irradiation ............................................................................................................................ 14
13 5.1.3. Microwave Irradiation ............................................................................................................................ 15

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14 5.1.4. Fenton Oxidation..................................................................................................................................... 16
15 5.1.5. Catalytic Wet Oxidation .......................................................................................................................... 17
16 5.1.6. Photocatalytic pre-treatment ................................................................................................................. 18
17 5.1.7. Other Pretreatment Methods ................................................................................................................. 19
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18 5.2. COMBINED PRETREATMENT APPROACH.......................................................................................................... 21
19 5.2.1. Thermal combined pretreatment............................................................................................................ 21
20 5.2.2. Microwave Combined pretreatment....................................................................................................... 22
21 5.2.3. Ultrasonic combined pretreatment......................................................................................................... 23
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22 5.2.4. Fenton Combined pretreatment.............................................................................................................. 24

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23 6. EVALUATION OF PRETREATMENTS AND ENERGY BALANCE ............................................................................25

24 7. CONCLUSIONS.................................................................................................................................................27
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25 REFERENCES........................................................................................................................................................28
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1. Introduction

Sludge production currently results in serious environmental issues in many developed, and

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developing, nations. Rapid industrialization, in conjunction with the extensive growth of urban

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zones, has also raised concerns in relation to sludge disposal (Chang et al., 2011). A wastewater
treatment plant is a facility in which a combination of various processes (e.g., physical, chemical

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and biological)are used to treat industrial wastewater and remove pollutants (Hreiz et al., 2015).
The waste residue generated during these treatment processes is known as sludge (Svanstrom et

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al., 2004; Abelleira et al., 2012). Sludge is potentially hazardous, because it contains adsorbed
residual organic pollutants from treated wastewater (Bolobajev et al., 2014). The treatment of

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the sludge is thus considered one of the most significant issues in wastewater treatment, due to
higher energy demands and treatment costs (Huang et al., 2014; Yan et al., 2015). The sludge
disposal processes comprise 60% of the total operating (Yan et al., 2015) and40% of total
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greenhouse gas emissions from wastewater treatment plants (Brown et al., 2010; Pilli et al.,
2015). Furthermore, sewage sludge is rich in pathogenic microorganisms and toxic pollutants,
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with the potential to cause serious risks to health. In order to acquire ‘class A’ solids, and fulfill
the demands of the Environmental Protection Agency, sludge must be stabilized and detoxified
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prior to its final disposal, or use for land application (Chang et al., 2011).
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A number of techniques have been developed for sludge treatment and minimization. These
consist of physical, chemical and biological technologies, or a combination of the three (Xu et
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al., 2014). Previously, the disposal of excessive sludge has been undertaken through traditional
methods, including incineration, land filling or ocean-dumping. However, an increase in related
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environmental concerns, and stringent environmental laws, has led to these disposal options
being replaced by biological methods, i.e., composting, aerobic and anaerobic digestion. These
biological processes are now widely accepted and are employed for the following: the removal
of toxic compounds and pathogenic organisms; to reduce the total volume of sludge; and to
transform sludge into stable biosolids (Semblante et al., 2015; Chang et al., 2011).

Anaerobic and aerobic digestion systems for sludge are now commonly integrated into
wastewater treatment plants, specifically to stabilize the waste activated sludge (Chang et al.,
2011a). However, this leads to the efficiency of biological treatments being highly

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compromised, due to a number of factors, including: complex structural components in sludge;
rate-limiting cell lysis (Chang et al., 2011); the presence of extracellular polymeric substances
(Xu et al., 2014) and various inhibitory compounds (i.e., ammonical nitrogen) (Bolzonella et al.,
2005; Serrano et al., 2015). Furthermore, Ruffino et al. (2015) and Cho et al. (2014) have
reported that that bacterial cells and cell walls/membrane form strong barriers to the penetration

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of hydrolytic enzymes to degrade the intracellular organic components in waste-activated

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sludge. The component cell walls are either very hard, or dissolve because they are composed of
recalcitrant complex compounds, e.g., lignin, cellulose and hemicellulose (Abelleira-Pereira et

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al., 2015). In the case of anaerobic digestion, the efficiency of sludge degradation is generally
affected by hydrolysis. This is the first stage in anaerobic digestion, which is known as the rate-

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limiting step, due to the complex structural components present in the sludge (Chang et al.,
2011).

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In order to overcome the above-noted issues associated inhibiting the biological treatment of
sludge, a number of interventions are required. The efficient stabilization of sludge can be
improved through the application of pre-treatment to the sludge prior to biological digestion.
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Various methods of pretreatment are reported in the literature, e.g., photocatayisi; ozonation;
thermal hydrolysis; ultrasound; enzymatic lysis; acidification; alkaline hydrolysis; freezing and
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thawing; and mechanical disintegration (Zhang et al., 2010: Chang et al., 2011; Liu et al.,
2013a). Moreover, more advanced research has been undertaken over recent years to apply these
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pre-treatments in a number of combinations, aimed at enhancing the process efficiency at a high

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level, e.g., alkaline-thermal (Na et al., 2011); thermal-H2O2 (Abelleira et al., 2012); microwave-
alkaline (Chang et al., 2011a); and Fenton-ultrasonic (Ning et al., 2014). The primary aim of
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sludge disintegration using the pretreatment option is to rupture the microbial cell wall, leading
to the release of both extracellular and intracellular organic compounds. This can accelerate the
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subsequent biological treatment (aerobic/anaerobic digestion) of the sludge, and reduce the solid
retention time required during digestion (Zhang et al., 2010; Chang et al., 2011).

The present review describes the details of the sludge treatment process through the aerobic and
aerobic digestion processes, along with key factors impacting the efficiency of the digestion
process. Furthermore, in order to enhance the efficiency of the biological treatment of sludge,
there will be a discussion of the use of various advance methods of pre-treatments, i.e., physical
and chemical methods. Figure 1 provides an overview of a sludge management flow chart, using

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 the pretreatment approach either as a single process or in combination.

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1 Figure 1: Sludge management flow chart: application of pretreatment approach either as single
2 or in combination (information acquired from: Abelleira et al., 2012; Semblante et al. 2015;
3 Na et al., 2011; Ning et al., 2014).

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2. Sludge production process and components

Sludge is produced from either industrial, domestic, or wastewater treatment plants during the
process of wastewater treatment, and is the solid residue that remains following the wastewater
treatment (Abelleira et al., 2012). A treatment plant is a facility in which wastewater is treated to
achieve the removal of pollutants using a combination of various physical, mechanical, chemical

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and biological processes (Hreiz et al., 2015). The most common treatment technology is the
‘activated sludge system’ (invented early in the previous century), with current systems

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retaining similarities to this conventional system (Keller et al., 2002; Perez-Elvira et al., 2006).
In the activated sludge system, the wastewater treatment plant generally combines two levels of

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treatment, i.e., primary and secondary. The primary treatment ensures the removal of particulate
pollutants, e.g., sand, debris, grease, oils, and other particulate wastes. These materials are
separated from the wastewater through a gravitational separation method in a large tank, termed

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the primary settler. The solid residues produced in the primary settler is referred to as primary
sludge. During the secondary treatment stage, the dissolved and colloidal components are
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removed in a secondary clarifier, or settling tank, resulting in the production of secondary
sludge (Hreiz et al., 2015).

The sludge is primarily composed of biomass and microbial cells, produced during the activated
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sludge process. Overall, the biomass contains approximately 30% protein, 40% carbohydrate
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and the remaining 30% is lipids in particulate forms (Lin et al., 1999; Sahinkaya et al., 2015).
See Table 1 for the chemical characteristics of various types of sludge (e.g., COD; volatile
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solids; total solids; pH; and nitrogen). Municipal wastewater sludge contains high
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concentrations of organic matter, e.g., COD and BOD, phosphorous, nitrogen, and heavy metals
such as Zn, Cu, Ni, Pb, Hg and Cr (TAO et al., 2012). Industrial sludge contains a variety of
specific toxic pollutants, which can vary according to the type of industry and product process,
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e.g., pharmaceutical industrial sludge contains a high concentration of endocrine disrupters and
toxic antibiotics, such as sulfonamides (Galan et al., 2012). A considerable amount of oil sludge
is generated in oil refineries, containing hundreds of organic compounds that are highly toxic,
carcinogenic and mutagenic. These pollutants are classified as priority pollutants by the
Environmental Protection Agency, leading to strict controls being required for their release into
the environment (Cui et al., 2009; Zhou et al., 2009; Jing et al., 2012).

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3. Sludge Stabilization Processes

The sludge stabilization process has been applied for over 20 years globally, especially in
United states, Europe, Canada, Japan and other developed countries or regions (GTZ/Holcim,
2006; Liu et al., 2015a). Sludge minimization is performed by three main process at wastewater
treatment plant: (1) minimization in the water line, (2) minimization at sludge line and (3)

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minimization through final disposal (Perez-Elvira et al., (2006). However, in most of the large
wastewater treatment plants, the sludge is stabilized through process at sludge line or in general

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terms through biological process. The typical method of sludge stabilization is composed of
two stages: firstly, sludge thickening or dewatering and secondly, stabilization. The thickening

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process is performed to increase sludge concentration to 3% total solids (TS), or higher, using
the following: centrifugation; gravity settling; rotatory drum filtration; and air flotation. In the
second step (i.e., stabilization), sludge degrades the volatile solids, and reduces the pathogenic

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organisms and other unwanted qualities of the sludge (Tchobanoglus et al., 2003; Semblante et
al., 2015). There are a number of available biological treatment options widely adopted for
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sludge stabilization, including anaerobic digestion, composting and aerobic digestion (Zhang,
2010; Pilli et al., 2015). These processes not only produce stable bio-solids, but also a number of
value-added products, e.g., compose and bioenergy in the form of methane (Khanal et al., 2007;
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Chang et al., 2011). In China, about 20-50% of total investment of sewage treatment is spent on
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sludge management (Hu et al., 2009). The stabilization process has given priority to anaerobic
digestion which accounts about 38%, while aerobic digestion and composting is applied only in
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6% of the total treatment plants (Liu et al., 2015a)Whether the process is anaerobic, or aerobic,
the digestion of the organic content of the sludge is the fundamental process influencing the
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efficiency of digestion.

In the biological treatment of waste activated sludge, the digestion of macro-molecules is the
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primarily degradation. The macromolecules of the sludge are primarily composed of

carbohydrates, proteins and humic substances, of which proteins are the most abundant
component, accounting for 50% of total organic matter volume (Jimenez et al., 2013; Shao et
al., 2013). Due to waste activated sludge being generated as result of the biological treatment of
wastewater, it is rich in microbial cells containing intracellular organic matter. Thus, the key
point of the disintegration of sludge is to facilitate intracellular organic matter by rupturing the
cell wall. Accessing the organic matter can help accelerate the subsequent anaerobic or aerobic

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 digestion of sludge, with the benefit of only a low retention time being needed for the digestion
process (Tiehm et al., 2001; Zhang et al., 2010; Chang et al., 2011).

3.1. Aerobic Digestion of sludge and limitations

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The aerobic digestion process is widely used for sludge stabilization (Fall et al., 2014);

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involving the treatment of dewatered, or thickened, sludge in a completely aerated reactor. The
biodegradation in aerobic digestion is highly dependent on retention time, and the temperature

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of the system (Semblante et al., 2015). It is reported that aerobic stabilization of sludge has
industrial application for food industrial effluent (Elia Ruda et al., 2013; Arun and Sivashanmugam

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2015). In United States, there are about 4,880 sludge treatment facilities in 2005, out of which 2,200
are using aerobic digestion processes (UN-HSP, 2008). An aerobic process may be employed at

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mesophilic or thermophilic temperatures, of which, thermophilic digestion has gained more
importance during previous years. Jin et al. (2015a) report that, in the thermophilic aerobic
process, the sludge is agitated with oxygen at a residence time of ten days, and a temperature
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above 50oC can achieve volatile solids removal of up to 38%.

Among the classification of thermophilic processes, autothermal thermophilic aerobic digestion

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(ATAD) has been reported as an efficient technology, due to its capacity for insulation, and
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considerable levels of self-heat production through microbial degradation. The process can
provide a rapid degradation of biomass, along with low sludge retention time (SRT) in the
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reactor and efficient inactivation of pathogenic microorganism at high temperature (Layden et

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al., 2007; Liu et al., 2012a). However, one of the main disadvantages of the process consists of
the high levels of ammonium nitrogen produced as a result of the degradation of the protein
content. At temperatures above 35oC, the nitrification and denitrification processes are hindered,
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resulting in an accumulation of ammonium nitrogen in the system (Layden et al., 2007; Yuan et
al., 2014). Meanwhile, the increased concentration of ammonium nitrogen impedes bacterial
activity, because its ability to penetrate the cell wall increases with rising temperature, while a
bacterial cell is unsustainable if the level of ammonium nitrogen is higher than the appropriate
requirement (Yuan et al., 2014).

1 3.2. Composting
Compositing process is applied for sludge treatment and conversion of complex bio waste in to
stabilized product that can be utilized as organic fertilizer and value added product (Malinska et

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al., 2014). Compositing is operated in aerobic conditions where the micro-aeration can be
effective to hydrolyse complex substances in to simple materials due to production of hydrolytic
enzyme and increase the specific growth rate of microorganism (Ariunbaatar et al. 2014).
Compositing process is completed in three stages which are based on evolution in temperature.
The first stage is attributed to growth of mesophilic microbiota which increases the temperature

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of the system. The continuous increase in temperature initiate second stage that associated with

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the activation of thermophilic microbiota. In this stage most of the pathogens are killed under
high temperature regime. Finally, the third stage is maturation phase which involves a

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diminution in temperature and reactivation of mesophilic population (Gonzalez et al., 2016)

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Composting has been used successfully as a sludge treatment method both at lab scale and full
scale studies (Elia Ruda et al., 2013; Hu et al., 2015: Gonzalez et al., 2016). The stabilization of
sludge by composting requires an addition of bulking agent to stabilize material and microbial

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degradation process. Elia Ruda et al., (2013), used sawdust as bulking agent and aeration to
stabilize the sludge during composition process. Similarly, in another study the mixture of
sewage sludge and bulking agent was composted in a semi-closed system at the El-Salao
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biosolids composting plant (Spain) (Gonzalez et al., 2016). It was found that the system
achieved high temperature in short time and maintained during the stage, decreasing the
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pathogens significantly carbon content up to 41%. Compositing is widely accepted technology

for sludge stabilization, however, the process may be some times limited due presences of
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complex compounds, temperature loss, unavailability of microorganisms, presence of

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unstabililzed materials and pathogens.

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3.3. Anaerobic digestion of sludge and limitations

Anaerobic digestion of sludge is claimed to be a highly cost-effective technology, as it provides

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energy recovery in the form of methane, with limited environmental impact (Khalid et al., 2011;
Mata-Alvarez et al., 2011; Anjum et al., 2012; Pilli et al., 2015). The technology is widely
applied at full scale sewage treatment works, for instance, in California 82% of total sewage
treatment plants are operating anaerobic digestion for sludge stabilization (NBRA, 2007). In
modern wastewater treatment plants, an anaerobic digestion system for sludge is integrated as
essential, thus assisting in the transformation of excessive organic matter into biogas containing
over 60% methane. Anaerobic digestion has the ability to considerably reduce final solids, as
well as destroying the majority of the pathogenic microorganisms in the sludge. However, 50%
of the costs at a wastewater treatment plant are associated with the processing of sludge (Appels

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et al., 2008: Abelleira et al., 2012). In the field of the anaerobic digestion of sludge, current
research is highly focused on two major concerns: (1) improvement in the degradation
efficiency of dry organic matter; and (2) the potential for the production of biogas (Schievano et
al., 2012; Ruiz-Hernando et al., 2014; Abelleira-Pereira, 2015).

Beside the beneficial aspects, anaerobic digestion is a comparatively slow process, due to the

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complex compounds being in need of a longer retention time at the hydrolysis stage, and

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requiring a larger volume of bioreactor (Pilli et al., 2015). Chen et al. (2008) report that the

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persistence of trace organic contaminants of sludge pose a number of issues for anaerobic
digestion, as methanogens are highly susceptible to trace organics (i.e., halogenated aliphatic,

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chlrophenols, and N-subsituted aromatic compounds). Moreover, some anaerobic co-metabolic
pathways produce even more toxic pollutants (e.g., estradiol, nonylphenol, etc.), with serious
implications for the anaerobic digestion of sludge (Semblante et al., 2015). In the case of

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secondary sewage sludge, anaerobic digestion is becoming increasingly challenging, due to the
implementation of strict regulations on nitrogen limits, the elimination of primary sedimentation
units, and longer sludge ages, etc. (Dwyer et al., 2008; Abelleira et al., 2012).
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4. Factors Affecting Sludge Stabilization
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Previous studies have reported potential for the use of single microbial species in the biological
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processing of sludge for particular contaminants. However, this restricts its field application due
to the presence of a variety of other contaminants, which cannot be degraded by existing
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microbial species (Ramteke and Gogate, 2015). For example, in a conventional biological
process, aromatic compounds (e.g., p-nitrophenol and ethylbenzene) cannot be degraded by
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existing microbial diversity obtained from municipal sludge (Jahan et al., 2014). An additional
step is therefore required as a pre-treatment, because of the limited ability of microorganisms to
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degrade a considerable variety of contaminants (Ramteke and Gogate, 2015).

A further factor influencing the biological treatment of sludge is the presence of heavy metal
ions (i.e., Cr, Pb, Cu, Zn, Ni and Cd). If present at concentrations above critical values, these
metals can cause toxicity to microorganisms, and specifically to hydrogenogenic and
methanogenic organisms (Jaesang et al., 2011; Liu et al., 2013a).

In the anaerobic digestion process, the low efficiency of the microorganisms involved in the
hydrolysis stage is due to the presence of the following: microflocs; flocks; aggregates of
extracellular polymeric compounds; recalcitrant compounds of lipids and proteins; and hard cell

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 walls (e.g., lignin, cellulose and hemicellulose) (Carballa et al., 2011; Carlsson et al., 2012;
Abelleira-Pereira et al., 2015). These factors are also responsible for the increased retention time
of the anaerobic digestion process. Thus, researchers are currently focusing on methods of
increasing the digestion efficiency by promoting hydrolysis, which is generally regarded as a
rate-limiting stage (Jang et al., 2013). Khanal et al. (2007) and Pilli et al. (2015) have suggested

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the use of sludge pretreatment in order to achieve lower retention times in the anaerobic

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digestion of sludge. Without such a pretreatment step, the efficiency of organic matter removal
is limited to 30-50% even at solid retention times of up to forty days (Toreci et al., 2009; Jang et

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al., 2014)

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A number of different methods of pretreatment have been developed to improve sludge
solubilization for subsequent biological treatment. These include physical and chemical
methods, or a combination of both. There has been a specific focus in the literature on a number

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of pre-treatments, e.g., ultrasonic; thermal; Fenton; ozonation; alkaline; wet oxidation; and
photocatalysis (Carrere et al., 2010; Jang et al., 2014; Chang et al., 2011; Liu et al., 2013a). In
the case of combined pretreatments, a number of different methods have been reported,
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including: alkaline-thermal (Na et al., 2011); thermal-H2O2 (Abelleira et al., 2012); microwave-
alkaline (Chang et al., 2011a); and Fenton/ultrasonic (Ning et al., 2014).
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The key factors resulting in limitations to the biological treatment of sludge in relation to the
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above discussion are listed in Box 1. The application of appropriate pretreatment can have a
positive effect over these factors and improve the degradability of the sludge during the
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biological process.
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Box 1: Key factors that inhibit the aerobic or anaerobic digestion of sludge

 Limited ability of microbial diversity to degrade variety of contaminants

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 Presence of macro-flocks and macromolecules inside the sludge

 Intercellular organic matter in bacterial cells in waste activated sludge

 Aggregation of biological flocks

 Presence of extracellular polymeric substances (EPS) in sludge

 Inhibitory compounds

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 5. Approaches to sludge pretreatment

In a vast majority of wastewater treatment plants, the sludge stabilization performed by

anaerobic digestion (Perez-Elvira et al., 2006), thus most of the studies are conducted to enhance

anaerobic stabilization of sludge using pre-treatment. Number of pretreatment approaches have

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been devised for the efficient stabilization of sludge using a biological treatment process,

including thermal hydrolysis; ozonation; microwave; ultrasound; Fenton; alkali, photocatalysis,

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electrochemical, free nitrous acid and many others.These can be used either as a single

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pretreatment or in combination. However, in selection of an appropriate pretreatment method

the factors such as energy and chemical demand are highly crucial. The energy consumption is

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depended on the amount of total solids in the sludge. To evaluate various pretreatment methods,

a simple equation described by Cano et al. (2015) can be used to assess, weather the energy
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balances are contended for self sufficiency of the process.

EC ≤ 0.20 c (kWh/m3)
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1 Where EC is energy consumption per unit volume of sludge and c is kilograms of total solids in the

2 sludge. Although, the energy balance plays an important role in selection of pretreatment method, but
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3 the primary aim is to disintegrate the sludge components, EPS and disrupt the cell wall of
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4 microbial flocks, in order to render the sludge components more accessible to the subsequent

5 biological treatment (Chang et al., 2011a; Carlsson et al., 2012). In this context, this section
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6 provides a comprehensive description of efficiency of various treatment methods with respect to

7 improvement in sludge stabilization process.

5.1. Single Pre-Treatment Approach

The efficiency of biological sludge stabilization can be enhanced using various types of
pretreatment techniques. A comprehensive view of the effectiveness of various pretreatments is
summarized in Table 2. The details of these methods are described as follows:

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5.1.1. Thermal Hydrolysis

Thermal pretreatment of the sludge at high temperatures has been found to be highly effective in
terms of the reduction of organic matter, leading to positive effects on biological processing,
including biogas potential, lower hydraulic retention time, and removal of pathogens (Tyagi et
al., 2012; Souza et al., 2013). Thermal hydrolysis as pretreatment has been applied successfully

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at full scale in 30 wastewater treatment facilities for sludge stabilization (Cano et al., 2015).

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There are a number of methods available for thermal pretreatment, however thermal hydrolysis

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has attained a high level of acceptance among scientist and fields of industry (Morgan-
Sagastume et al., 2011; Abelleira-Pereira et al., 2015). The appropriate temperature for thermal
hydrolysis generally lies between 160-180 oC, while pressure tends to be in the range of 600–

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2500 kPa for a duration of up to sixty minutes (Carrere et al., 2010: Souza et al., 2013). These
conditions can assist in disrupting the cell walls of the bacterial flocs, and increasing the rate

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limiting hydrolytic process in biological processing. It is also reported that a wide range of
temperatures (i.e., 100-175 oC) at low pressure conditions (1300 kPa) can partially disrupt the
cell walls, however the cell contents could be available enough for biological treatment
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(Abelleira et al., 2012). It has also been observed that these pretreatment conditions decrease the
viscosity, and increase the dewaterability, of sludge. Beside these, the non-biodegradable
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organic matter (such endogenous substances) remain unchanged during the thermal hydrolysis.
However, it has been established that the heterotrophic biomass converts into two fractions;
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slowly biodegradable organic content (64%) and readily biodegradable organic content (36%)
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(Burger and Parker, 2013).

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Thermal hydrolysis has the capacity to increase the biogas potential of anaerobic reactors to
considerably high levels. Perez-Elvira et al. (2010) found an increase of up to a 40% in biogas
yield from an anaerobic system assisted by thermo hydrolysis of mixed sludge. This biogas
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forms an efficient source of electricity production, with Kepp et al. (2000) estimating that the
overproduction of electricity from the biogas of anaerobic digestion of mixed sludge was 20%
higher with thermal hydrolytic pretreatment, in comparison to anaerobic digestion without
pretreatment (Abelleira-Pereira et al., 2015).

5.1.2. Ultrasound Irradiation

Ultrasound irradiation is regarded as a rapid pretreatment method, one that is comparatively

simple to operate in comparison to other technologies used to dissociate the biomass of the
sludge. There are number of ultrasound pre-treatment systems have been installed in treatement

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plants around the world. For instance, in Europe, Doosan Enpure's system has developed full
scale Sonix system for ultrasound pretreated of sludge and subsequent improvement in
anaerobic digestion (Pilli et al., 2011). Cano et al., (2015) also mentioned the successful
application of ultrasound pretreatment in six industrial scale treatment plants (Cano et al.,
2015).The organics released as result of ultrasound can easily be hydrolyzed, thus enhancing the
rate of biological treatment with a lower retention time (Jinfeng et al., 2007). The mechanism of

t
ip
the ultrasound-assisted destruction of sludge is completed in three stages: (1) The first stage is
referred to as ‘floc losing.’ Here, the size of the microbial flocs begins to decrease and the

cr
extracellular material detaches from the surface of microbial flocs. (2) The second stage is
known as the ‘cell breakage step’. Here, intracellular organic material forms a microbial cell

us
release from the cell, due to a disruption of the cell wall. The majority of the organic materials
are macromolecule. (3) Finally, in the third stage, macromolecules are degraded into short chain
organic compounds (Khanal et al., 2007). The high power ultrasound pretreatment induces a rise

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in the temperature of the system, which further increases the efficiency of sludge disintegration
(Jinfeng et al., 2007).
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The use of ultrasound irradiation for sludge can increase the soluble COD content up to a
remarkable level, which can be further increased with irradiation time and ultrasound intensity.
d

The duration and intensity are highly linked to each other, and require balancing during
ultrasound irradiation. Jinfeng et al. (2007) report that the duration of irradiation is the key
te

factor to consider, should the irradiation be higher than 1040 W/m2. A short length of exposure
can only break the microbial flocs, without destroying the cell wall, whereas a longer duration
p

can completely destroy the bacterial cells (Wang et al., 2005). There is a change in the specific
ce

energy input in response to a change in the intensity of the ultrasound, in which the
disintegration of the sludge components is dependent on a specific energy input. Should the
Ac

specific energy input from ultrasound irradiation achieve up to l0 kJ/g dry solids, the sludge
disintegration can be as high as 40%. However, Chang et al. (2011) have achieved high cell
disruption at a high ultrasonic energy input of 397 kJ/g, although the pretreatment increased the
dissolution of COD up to 44.4%.

5.1.3. Microwave Irradiation

Microwave pretreatment of sludge is based on the microwave heating disintegration of the

sludge. Compared to conventional heating methods, the application of microwave irradiation
has a number of potential advantages, including: rapid and selective heating; instant control of

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Page 15 of 53
processes; compactness; and cost effectiveness (Tian et al., 2011; Tyagi et al., 2012). The use of
microwave irradiation allows the desired temperature to be achieved to provide the subsequent
benefit of a lower use of energy and a low level of environmental emissions (Yu et al., 2009;
Tang et al., 2010; Chang et al., 2011a).

In the case of sludge pretreatment, microwave pretreatment is generally studied at two

t
temperatures: (1) high temperature (<100oC), under normal pressure input; and (2) low

ip
temperature (100oC), under high-pressure. However, if both temperature and pressure are at a

cr
high level, sludge solubilization can also be increased. This renders the process energy-
intensive, and increases the overall capital, and operational, costs of the process. This forms the

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major drawback of microwave heating (Tyagi et al., 2012).

Appels et al. (2013) have established that the use of microwave pretreatment alters the

an
composition of the sludge. This change in composition results in increasing biogas production
by 50% in semi continuous anaerobic digestion, in comparison to untreated sludge. Similarly, in
a further study, the microwave pretreatment of mixed sludge at 100oC demonstrates a
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remarkable increase in biogas production of up to 84%, in comparison to untreated sludge
(Elagroudy and El-Gohary, 2013). These studies have revealed that microwave heating increases
biogas production to a considerable level, making it possible to balance the issue of energy
d

demand in terms of the operational cost of the process.

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5.1.4. Fenton Oxidation

p

Fenton oxidation is considered an attractive technology for the oxidation of a variety of organic
ce

pollutants. The process requires a Fenton's reagent, which is composed of a solution of ferrous
iron and hydrogen peroxide. Fenton oxidation is highly accepted, due to iron being a nontoxic
element and (due to its abundance) a cheap metal, while the use of hydrogen peroxide rapidly
Ac

degrades, generating the yield oxidants (Frontistis et al., 2011; Li et al., 2014).

The Fenton oxidation process is primarily completed in four steps: (1) the adjustment of pH to
low acidic condition; (2) oxidation; (3) neutralization; and (4) byproducts separated by
coagulation. The pH factor generally hinders the Fenton process due to low acidic conditions
being important for optimum operation (Ramteke and Gogate, 2015). However, the efficacy of
the Fenton process is more closely linked to the oxidation step, with its mechanism being highly
dependant on the generation of a hydroxyl radical (OH•) under low pH values by the catalytic
dissociation of hydrogen peroxide (H2O2) in the presence of ferrous iron (Fe2+) (Sahinkaya et

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Page 16 of 53
al., 2015). The oxidizing radicals produced by this process contain redox potential (+2.33 V), in
comparison to that produced by hydrogen peroxide alone (+1.36 V) (Erden and Filibeli, 2010;
Pham et al., 2010). Thus, due to the high redox potential, the solids have been reduced up to
60% and have transformed the sludge into class A biosolids (Pilli et al., 2015).

The application of Fenton oxidation as a sludge pretreatment has a high capability to degrade

t
extracellular polymeric substances, and break the microbial cell walls, thus releasing the

ip
intracellular organic content. The sludge may contain refractory organic compounds, which can

cr
be transformed into two available forms (e.g., readily and soluble organics) for subsequent
biological treatment (Tyagi and Lo, 2011; Li et al., 2014). Dewil et al. (2007) have observed a

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75% increase in biogas production from the anaerobic digestion of Fenton pretreated sludge.
Similarly, a further study has found a solubilization and biodegradation efficiency up to 70%,
after applying Fenton pretreatment at the optimal conditions of (1) temperature (i.e., 25 oC) and

an
(2) duration (i.e., 60 minutes) (Pham et al., 2010). The optimum conditions for the Fenton
pretreatment of sludge may vary according to the type of sludge and the biological treatment
process. For activated sludge pretreatment, the optimum Fenton reagent dose has been found to
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be iron = 4 g/kg and H2O2 = 40 g/kg on a total solid basis at pH 3. The methane content of
biogas has been achieved up to a maximum 38% in a pretreated reactor, in comparison to
d

untreated raw sludge (Sahinkaya et al., 2015)

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5.1.5. Catalytic Wet Oxidation

The catalytic wet oxidation (CWO) forms a process in which organic substances are completely
p

oxidized into carbon dioxide and water in the presence of air. It is a liquid phase process,
ce

completed in the presence of a specified catalyst. The catalyst improves the operating conditions
at a high reaction rate, with a short reaction time (Levec and Pintar, 2007; Jing et al., 2012). Wet
Ac

oxidation without the use of a catalyst has been applied as a pre-treatment step for sludge
stabilization, in which the complex organic content is partially solubilized, thus yielding
biodegradable COD (Urrea et al., 2014). However, a number of authors have also studied the
use of a catalyst in a wet oxidation process to improve the efficiency of solublization (Hii et al.,
2014; Urrea et al., 2014; Jing et al., 2012). Urrea et al. (2014) report that the use of a catalyst
can cause the refractory compounds of sludge to be more susceptible to solublization and can
ensure mild operation conditions requirements.

Bhargava et al. (2006) found that the use of hydrogen peroxide in the wet oxidation of oily
sludge can remove the greater organic content, when up to 80% of chemical oxygen demand has

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Page 17 of 53
been removed from the sludge. The use of a carbon supplement can increase the wet oxidation
efficiency, as these are able to increase the rate of biological denitrification. Strong et al. (2011)
found that acetate and ethanol supplementation in the wet oxidation of waste activated sludge
has a positive effect on the rate of denitrification. Little development has yet been made in the
case of the pretreatment of already digested sludge, however, using raw sludge for CWO

t
pretreatment has significantly enhanced the biodegradability, i.e., up to 75 % (TOC basis) (Genc

ip
et al., 2002).

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5.1.6. Photocatalytic pre-treatment

Photocatalysis has been widely used for the treatment of wastewater. However, over recent

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years, there has been a focus on its properties as a pretreatment method for sludge
solubalization. Photocatalysis has a number of advantages over conventional processes,

an
particularly in respect to energy requirements, low cost treatments and environmental protection
(Liu et al., 2014). In photocatalysis, the catalyst (such as TiO2 on the absorption of light as an
energy source) generates reducing electrons in conduction bands, and holes in valance bands
M
having an oxidizing property . These holes naturalize the OH- from water and generate strong
oxidizing oOH radicals. The chemical oxidation during photocayalysis breaks down the organic
pollutants from complex into simpler molecules, which thus become available for further
d

biological degradation during the anaerobic process (Ribeiro et al., 2015).

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Various types of reactors have been developed for photocatalysis, including: the common flat
photocatalytic reactor; the annular photocatalytic reactor; the fluidized bed photocatalytic
p

reactor; the film type photocatalytic reactor; and the optical fiber photo-catalytic reactor.
ce

However, these reactor designs are specifically for the treatment of wastewater, and only a few
photocatalytic reactors for sludge treatment have been reported in the literature, including: the
Ac

sloping trough circulating bed photocatalytic reactor (Liu et al., 2012b); circulating bed
photocatalytic reactor (Liu et al., 2013a) and the solar fluidized tubular photocatalytic reactor
(Liu et al., 2013b).

Liu et al. (2012) demonstrated that the photocatalytic pretreatment of waste activated sludge, in
a sloping trough circulating bed photocatalytic reactor, improved the hydrolysis process and
achieved seventeen times higher biohydrogen production in comparison to that in untreated
sludge. A simultaneous photocatalytic and biogas-producing reactor was developed by Liu et al.
(2013b), which is also known as the solar fluidized tubular photocatalytic reactor. It was found
that the use of AgX/TiO2 photocatalyst in the above noted reactor achieved a 69.1% removal of

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Page 18 of 53
 chemical oxygen demand, with a hydrogen production of 7866.7mmol H2/l sludge. Similarly, an
increase in biogas production was also observed using on-site photocatalytic pretreatment of
waste-activated sludge, in which the anaerobic digestion process demonstrated methane
production up to 1266.7 ml/l of sludge and volatile removal up to 67.4% (Liu et al., 2014).

Photocatalysis pretreatment is not only suitable for increased sludge solubalization and biogas

t
production, but it can also be used to remove a variety of contaminants, toxic compounds and

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pathogens from sludge. Various studies have revealed that the use of solar TiO2 pre-treatment

cr
has the potential to remove a considerable amount of phenols (Gernjak et al., 2004) and heavy
metals (Herrmann, 1999) from the system. The process has also found to be efficient for the

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removal of microbial contamination, primarily due to the formation of hydroxyl radicals (OH°),
thus enabling the removal of a large variety of pathogenic bacterial, fungal, algal and even viral
strains. Furthermore, photocatalysis is also highly effective in treating the spores of the disease-

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causing Clostridium perfringensand Escherichia coli species (Kim et al., 2003). Hinkova et al.,
(2015) report that surfactants present in food industry sludge (e.g., anionic sodium dodecyl
sulphate and cationic N-Cetyl-N,N,N-trimethyl ammonium bromide) can be removed by UV-
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titanium dioxide catalyst (P25, Degussa) phtotocatalysis, as these compounds have the potential
to hinder the process of biodegradation. Most recently, a new photocatalyst (i.e., Ag–AgCl/ZnO
d

nanorods) has been developed by Li et al. (2015), for the disintegration of the lignin compound,
achieving efficient lignin degradation within 120 minutes of photocatlysis, with the biogas yield
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subsequently rising to up to 325 ml/g TOC during the anaerobic digestion process.
p

1 5.1.7. Other Pretreatment Methods

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Sludge pretreatment has been investigated under controlled conditions through various treatment
Ac

processes. These include electrochemical, free nitrous acid, focused pulsed, enzyme based
pretreatments, and physical methods like Freezing/Thawing.

(a) Electrochemical: This process involves the fragmentation of sludge coagulates along with
the breakdown of microbial cell walls that helps in the breakdown of large organic molecules
particularly those associated with microbial cells, this breakdown could also be done by
electrolysis (Yuan et al., 2011). The process has high significance in wastewater treatment as it
completely breakdown the pollutants through strong oxidizing specie like hydroxyl radical
(OHo) without formation of any toxic compound. Considerable number of studies have been
performed on electrochemical technique as pretreatment for sludge stabilization. In a study, Yu
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Page 19 of 53
et al., 2014 reported that soluble COD (sCOD) increased 5.2 times owing to electrochemical
pretreatment. Furthermore, approximately 647 L/kg of volatile solids (VS) of biogas were
obtained after electrochemical pretreatment which were nearly 63.4% higher than that of control
group. In another study with the use of Ti/RuO2 anode in electrochemical process potentially
converted high molecular weight biopolymer to the respective low-molecular-weight

t
substances, therefore increased the ease of their degradation. Further this process also enhanced

ip
the dewaterability of sludge (Yuan et al., 2011)

cr
(b) Free Nitrous acid (FNA): Pre-treatment of sludge by free nitrous acid represented better
performance in anaerobic digestion of sludge and increasing the methane production (Wang and

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Yuan, 2015). Free nitrous acid (FNA = HNO2) has been identified as biocide for bacterial cells;
therefore this property could effectively be utilized to break the bacterial flocks in the sludge
and thus increases the provision of available organic content. In few recent studies. it has been

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observed that even a minute amount (ppm) of FNA, is a strong biocide agent (Wang et al., 2013)
and can decrease up to 50%-80% fraction of microbial cells (Pijuan et al., 2012: Wang et al.,
2014). Effectiveness of FNA pretreatment through its biocidal activity has further been
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confirmed by a recent study Wang and Yuan, 2015 where 2.0mg/L FNA pretreatment for only
24 hours increased the degradation rate. Around 50% of the sludge was degraded in 14 days
d

compared to 32% degradation in untreated sludge.

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(c) Focused pulsed: Focused Pulsed (FP) is a novel pre-treatment technology that exploits a
rapid pulse (kHz), of high-voltage (20–30 kV) to disintegrate the complex organic pollutants,
p

cell membrane and macromolecules (Lee et al., 2010). The process works by introducing a high-
ce

energy pulsed electric field (PEF), thus particularly affect the building blocks of cell membrane
and cell wall that are phospholipids and peptidoglycan repectively (Seltmann and Holst, 2002).
This focused disruption exposes the intracellular organic fraction of the cell and also breakdown
Ac

the large flocks in the sludge. The breakdown process converts the complex organic
macromolecules to the simpler compounds and increases the ease of their biodegradation (Lee
and Rittmann, 2011).

(d) Freezing and Thawing: This pretreatment process involves an irreversible compaction of the
sludge flocks (Chu et al. 1999). The process may improve the dewaterability of the sludge but
has high energy demanding process due to requirement of regular freezing of the sludge (Perez-
Elvira et al., 2006). (e) Enzymatic conversions: The enzymatic breakdown of sludge is

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Page 20 of 53
biological treatment method in which, enzymatic actions break down the cell wall. This type of
pretreatment process is highly effective in increasing the degradation rate of volatile suspended
solids (VSS). The process also efficiently increases the soluble chemical oxygen demand
(sCOD) of the sludge (Jang et al., 2013). (f) Stirred ball mills: Amongst physical pretreatments
of sludge another method is stirred ball mills. This method involves crushing of the sludge by

t
cylindrical grinding chamber which is almost completely occupied with grinding beads. These

ip
grinding beads exert shear pressure and force on the micro-organisms and disrupt the cell
structure (Perez-Elvira et al., 2006).

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5.2. Combined Pretreatment Approach

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Sludge solubilization and flocs disintegration can be performed through the pretreatment
methods discussed above. A variety of further methods of pretreatment are reported in the

an
literature, using a combined pretreatment approach. This section has reviewed a number of
potential combined pretreatment technologies. Table 3 provides a summary of some of the
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reported combined pretreatment method.

5.2.1. Thermal combined pretreatment

d

The pretreatment of sludge with thermal hydrolysis has a positive effect on sludge stabilization.
te

A number of researchers have used thermal hydrolysis combined with other pretreatment
technologies to obtain high levels of efficiency, including thermal-alkaline and thermal-H2O2,
p

thermal. Na et al. (2011) achieved a significant disruption of microbial flocs and sludge
reduction using thermal-alkaline pretreatment. The combination of thermal-alkaline
ce

pretreatment increased the pH up to 13, which upsurged the intracellular organic components
generated by the destruction of microbial cells in the system. Furthermore, the soluble COD of
Ac

the sludge can be increased up to as much as 100 times as that of untreated sludge. The high
soluble COD content is suitable for the efficient anaerobic digestion process of sludge, with Xu
et al. (2014) having observed an increase in biogas production of up to 52.78%.

Recent developments have revealed that thermal hydrolysis can also be combined with
advanced oxidation processes, although very few examples have been reported. Abelleira et al.
(2012) have reported the use of thermal hydrolysis with hydrogen peroxide, based on
simultaneous direct steam injection and peroxidation. This method has three main advantages
over the single thermal or Fenton’s reagent (Ferrous + H2O2): (1) it requires mild operating

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Page 21 of 53
conditions with a low input of energy; (2) it does not (unlike Fenton’s reagent) require the
addition of a catalyst; and (3) there is no need to adjust the pH of the system. Furthermore, the
researchers found that the increased degradation of volatile solids improves the potential for
methane production. However, it should be noted that methane potential decreases at a
temperature above 170oC.

t
5.2.2. Microwave Combined pretreatment

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Microwave irradiation is recognized as an efficient technology, due to its considerable

cr
advantages, e.g., low cost, flexible control, and high COD. Recently, it has been suggested that
microwave pretreatment should be combined with further methods to improve the disintegration

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of the sludge and sanitization from pathogens (Ya-wei et al., 2015). Various studies have
revealed the synergistic effect of microwave combined with alkali pretreatment (Qiao et al.,

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2008; Dogan and Sanin, 2009; Chang et al., 2011). Chang et al. (2011) found that the
pretreatment of sludge with microwave-alkali increased the solubilization rate by 20%, in
comparison to that in a single treatment. This increased the aerobic treatment efficiency up to a
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point at which a 93% reduction in sCOD was achieved in just sixteen days of retention. Thus,
the pretreatment can also decrease the retention time in the reactor. When it comes to
microwave-alkali, various types of bases can be used, including NaOH, KOH and Ca(OH)2.
d

Tyagi et al. (2012) have established that the use of NaOH with microwave demonstrates a high
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rate of sludge solubilization in comparison to KOH. Sodium hydroxide achieves sludge

solubilization up to 52.5%, approximately 4% higher than with KOH. However, both achieved
p

bases demonstrate a 20% higher rate of efficiency in comparison to a single treatment. In

ce

addition to alkali, microwave can also assist with ultrasound pretreatment to increase the
anaerobic digestion and biogas production, i.e., Yeneneh et al. (2015) achieved a 31% higher
removal of total solids in comparison to microwave alone. Similarly, the enhanced biogas
Ac

production increased biogas production by as much as 15%.

Overall, the positive aspects of combined microwave pretreatments include the high rate of
sludge solubilization, biogas production and lower retention times. Furthermore, the process
requires a low level of energy input, ensuring the process is more economical in comparison to
microwave alone.

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Page 22 of 53
5.2.3. Ultrasonic combined pretreatment

Ultrasonic pretreatment forms a powerful method used for sludge disintegration and microbial
cell disruption. In order to improve the efficiency of the process, a number of modifications
have been suggested, which use the approach of combining ultrasonic pretreatment with other
methods, including acid, alkali, ozone and microwave, etc. In ultrasonic-acid pretreatment, the

t
pH of the system decreases to a very low level, which accelerates the sludge disintegration, due

ip
to the highly acidic conditions. Sahinkaya (2015) demonstrated that the ultrasound power

cr
density of 1.0 W/mL for a duration of ten minutes, combined with a pH value of 2.0, are the
optimum conditions for sludge solubilization under ultrasonic-acid pretreatment. However, the

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use of a highly concentrated sludge can limit sludge solubalization (Liu et al.,2008; Sahinkaya,
2015). On the other hand, the use of alkali with ultrasonic, instead of alkali alone, also has an
optimal result on sludge disintegration. The use of alkali promotes the hydrolysis of

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extracellular polymer substances and gels solubilization, which remains protected in a single
ultrasonic pretreatment (Yiying et al., 2009).
M
Further treatment methods (e.g., ultrasound with ozone) have also been found to demonstrate a
synergistic effect on sludge solubilization. Tian et al. (2015) employed ultrasound-ozone
pretreatment for domestic sludge, achieving a 25.7% increase in sludge biodegradability in
d

comparison with individual treatments. The pretreated sludge further showed an increase in
te

methane potential from 3.53 to 4.54 ml/d during the anaerobic treatment process. Likewise, the
use of ultrasound with microwave irradiation for sludge pretreatment also has a positive effect
p

on biodegradability and biogas production. Yeneneh et al. (2013) applied microwave at 2450
ce

MHz for three minutes, followed by ultrasonic at a density of 0.4 W/mL for six minutes to
different types of sludge. They found that pretreatments increase the cumulative methane
production (66.5 ml/g tCOD) to a greater degree in excess activated sludge, as compared to the
Ac

methane yield from mixed sludge. In general, integrating ultrasound with further treatment
methods can increase soluble organics within the system, providing a lesser effect of various
factors, including extracellular polymeric substances, re-flocs and gel formation.

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Page 23 of 53
5.2.4. Fenton Combined pretreatment

The Fenton process has been proposed as a promising option by a number of scientists, however
only a small number of studies have reported the improved Fenton process through a
combination with other methods, i.e., ultrasonic, and bioleaching (Ramteke and Gogate, 2015;
Liu et al., 2015c). Bioleaching consists of a microbial technology used as an alternative to

t
traditional chemical acidification. Combined with the Fenton-bioleaching pretreatment of

ip
sludge, bioleaching decreases the pH of the system to its highest optimal range, while the

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Fenton process oxidizes the organics efficiently at a low pH. In addition, bioleaching can
provide a number of further benefits, including pathogen destruction (Couillard and Mercier,

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1991), leaching of heavy metals (Kim et al., 2005), low odor and volume (Filali-Meknassi et al.,
2000). (Liu et al., 2015c) report that the bioleaching for two days can drop the pH to as low as
2.5, which further enhances the Fenton process under optimum dosage to Fe2+ and H2O2 (0.036

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mol/L and 0.12 mol/L).

The Fenton process combined with ultrasonic pretreatment of sludge is also advantageous, due
M
its high destruction of microbial flocs and removal of extracellular polymeric substance. Ning et
al. (2014) found that the use of the Fenton-ultrasonic pretreatment for ten minutes increased the
production of hydroxyl radical (2.90 mol/l) in comparison to the Fenton single treatment. An
d

increase in the production of hydroxyl radical will increase the oxidation of sludge components
te

(Gong et al., 2015). Furthermore, the optimum range of ultrasonic density for Fenton hydroxyl
radical production was found to be 0.12 to 0.16 W/ml (Ning et al. 2014). The sludge
p

disintegration under Fenton-ultrasonic pretreatment can also increase the release of nutrients,
ce

e.g., carbon, nitrogen and phosphorous (Gong et al., 2015), which can play synergistic effect in
the biological treatment of sludge.
Ac

The combined pretreatment of sludge using Fenton with other methods is currently gaining high
acceptance, due to the use of iron being less costly, and non-toxic, whereas hydrogen peroxide
can yield a high level of oxidants. Furthermore, it is possible to hinder the issues associated with
a single Fenton process (i.e., low acidic requirements and toxic sludge treatment in the final
biological treatment) by combining the Fenton process with further treatment methods (Ramteke
and Gogate, 2015).

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Page 24 of 53
 1 6. Evaluation of Pretreatments and Energy Balance
2

3 For biological stabilization processes anaerobic digestion is more accepted technology (Perez-

4 Elvira et al., 2006) as compared to the aerobic digestion and compositing. This is due to the

5 requirement of lower energy footprint, and low cost. Anaerobic digestion is specialized for

t
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6 production of methane which could be used as biofuel and also assist in GHG emission

7 reduction. On the other hand aerobic digestion and compositing process is usually demand high

cr
8 energy input and workforce due to continues supply of air and mixing requirements. Although,

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9 the byproduct (compost) of composting could have field application as organic fertilizer, but

10 have various concern associated with lower quality and toxicity of the biosolids, especially if it

11 is produced form industrial sludge.

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12 Table 4 demonstrates an overall evaluation of various pretreatment methods with respect to their

13 advantages, disadvantages, energy (temperature, electric or power) and chemical requirements.

d

14 Most of the pretreatments methods such as microwave, ultrasounds, UV-photocatalysis and

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15 focused pulsed etc. demands high energy in the form of electricity. A net return of this energy

16 could be achieved, if the subsequent stabilization is performed by anaerobic digestion. The

p

17 energy from biogas would lead to a lower foot-print; however, the net profit would be decreased
ce

18 because of energy requirement and low potential green electricity (Cano et al., 2015). Pre-

19 treatment has capability to enhance biogas energy by 40% and leading to efficiencies above
Ac

20 60% (Fdz-Polanco et al., 2008). However, in a typical biogas engines 15% of the biogas energy

21 is dissipated and, from the remaining, only 35% is converted in to electricity while 65% is

22 converted in to thermal energy (Cano et al., 2015). Thus, for anaerobic digestion of sludge the

23 feasibility is lower for pretreatment method that requires needs electricity as compared to the

24 pretreatments which does not need energy in the form of electricity. For instance, the viability of

25 thermal hydrolysis and heat pre-treatments is comparatively more, because the potential of

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Page 25 of 53
 1 biogas to produce heat energy (65%) is quite sufficient for this purpose. In combine

2 pretreatment the energy demand can be lowered which ultimately could have a positive effect on

3 energy balance. This can be observed in study of Chang et al., (2011a), where the use of

4 microwave with power of 600W is less effective for sludge solubilization compared to the

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5 combine microwave-alkali pretreatment with same power. Combine pre-treatment make it

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6 possible to achieve a good balance in either way by decreasing the initial energy requirement or

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7 by increasing conversion of sludge soluble COD to methane with energy requirement same as in

8 single pre-treatment. Furthermore, combine pretreatment method may sometime demands no

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9 energy input if it is operated as combination of biological and chemical methods such as

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10 bioleaching-Fenton reported by (Liu et al., 2015c). Thus, combine pre-treatments are more

11 favorable with respect to energy requirement and efficiency of the process, however, to operate
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12 two treatment simultaneously is difficult at full scale plant and need more research to optimized

13 and apply at larger scale.

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14 The selection of pretreatment method could be influence by other factors. In biological

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15 pretreatment the use of enzymatic process or bioleaching (Kavitha et al., 2013) could be

efficient but takes longer time and difficult to optimize conditions. Microwave and thermal
p

16
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17 pretreatment could achieve a high temperature in a short duration but these are less favorable

18 due high energy consumption and their capability to kill aerobic and anaerobic bacteria present
Ac

19 in the sludge. Comparatively, ultrasonic is widely applied technology even at full scale setups.

20 The shear forces of ultrasonic have capability to remove pathogens, increase sludge

21 solubilizaon, decreased clogging and odour problems. Recently, UV-photocatalysis is emerged

22 as a pretreatment method for sludge but it requires UV radiation which increases the cost of the

23 process. Work is now underway to apply visible light photoctalaysis as pretreatment method so

24 that the ample source of solar radiation could be utilized as energy demand instead of use of

25 high capital artificial energy. This could be result in higher efficiency as compared to the other

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1 single pre-treatment and combine pretreatment method. Liu et al. (2013b) have achieved some

2 success in this regard. The idea of the vis-photocatalysis is to use solar radiation as energy

3 sources where the capability of recovery and reusability of the catalyst also decrease the demand

4 for costly chemicals.

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7. Conclusions

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The modification of conventional sludge treatment, combined with the implementation of a
pretreatment method, has a number of positive effects on sludge minimization, degradation,

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detoxification, and bioenergy production. The application of an appropriate pretreatment has the
ability to increase sludge solubilization by disintegrating complex organics, extracellular
polymeric substances and cell walls. These soluble contents are subsequently easily accessible
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for microbial degradation in subsequent biological treatments. Thus, the sustainable
management of sludge, along with an integrated system for sludge management, is suggested for
d

wastewater treatment plants.

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Despite confidence in the efficacy of employing a pretreatment approach for sludge

disintegration, a question remains in relation to the selection of an appropriate pretreatment
p

method. In the literature, a number of efficient pretreatment technologies have been proposed,
ce

although each contains a specific limitation, e.g., high energy and cost (microwave, ultrasonic);
low acidic requirement (Fenton); excess water utilization (wet oxidation); and catalyst recovery
(Catalytic oxidation). These issues can be resolved by the use of either a combined pretreatment
Ac

approach or emerging technology (i.e., photocatalysis). The combined pretreatment (e.g.,

ultrasound-alkali, Fenton-bioleaching) can use the benefit of two simultaneous treatments and
increase the efficiency of the process, particularly in relation to energy and capital requirements.
On the other hand, vis-photocatalysis has been widely used for the treatment of wastewater, and
has recently been established as highly effective for sludge disintegration and increased biogas
production during the anaerobic digestion of sludge. Furthermore, no additional energy source is
required, as the process utilizes sunlight.

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1 Table 1: Chemical characterization of various types of Sludges

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Type of sludge pH TS VS COD TN AN TP References
(mg/l) (mg/l)
(g/l) (g/l) (mg/l) (mg/l)

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Secondary sewage sludge 6.46 53.2 39.8 4195(s) 109 (t) 88 334 Jin et al., 2015

Dewatered activated 7.82 220.8 108 158312 (t) 9239 (t) 431 NR Zhang et al., 2015
sludge
1518 (s)

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Mix pri and waste 6.38 59.7 40.2 62000 (t) 2840 (t) 150 NR Souza et al., 2013
activated sludge
5500 (s) 3400 (s)

Sewage Sludge (Sludge

Thickining Tank)
6.5 57.6

ed 42.2 1615 (s) 173 (t) NR NR Liu et al., 2011

pt
Secondary Sewage 6.30 55.7 41.2 2310 (s) 141 (t) 104 301 Xu et al., 2013:
Sludge
ce

Sewage Sludge (Sludge 6.9 55.2 34.6 425 (s) 105 (t) 98 NR Liu et al., 2012a
Thickining Tank)

Aerobic granular sludge NR 18.8 14,5 23600 NR NR NR Palmeiro-Sanchez

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et al., 2013

Waste Activated Sludge 6.38 22.87 17.26 NR 1523 (t) 197.7 NR Shao et al., 2013

Secondary Sewage 6.5 13.1 9.4 11000 (t) NR NR NR Tyagi and Lo.,
Sludge 2012)
60.7 (s)

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Mixed primary and 6.61 NR 35.5 (WB) 71.35 (t) 4510 (t) 900 1810 Jang et al., 2014
secondary sludge

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7.96 (s)

Belt filtration sludge 7.70 150 542/TS 1740 (t) NR NR NR Huang et al., 2015

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Thicken sewage sludge 6.83 15.4 10.2 (WB) NR NR NR NR Liu et al., 2015c

Excess sludge 6.82 12 NR 17868.4 (t) 98.8 (t) NR 268.8 Gong et al., 2015

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Raw Sludge 6.2 51 695/TS NR NR NR NR Lloret et al., 2012

Sewage Sludge 7.72 138 96 (WB) 128000 (t) 8335 (t) NR 4400 Serrano et al., 2015

Slaughtering processing
sludge
7.4 10.6

ed744 (DB) 4239 (t) NR NR NR Erden et al., 2013

pt
Primary sludge 7.2 20 888 (DB) 30500 (t) NR NRs NR Yeneneh et al.,
2013
ce

Waste Activated Sludge 6.7 7.48 5.0 (WB) 18249 (t) NR 5006 NR Liu et al., 2013a
1752 (s)
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Waste activated sludge 6.83 7.48 5.0 (WB) 16249 (s) NR 132.6 NR Liu et al., 2012b

1 WB: Wet basis, DB: Dry basis, s=Soluble, t= total, NR= Not reported

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1 Table 2: Effect of various pretreatment methods on sludge solibilization and subsequent biological treatment

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Pretreatment Method Subsequent Biological Treatment Reference
S# Types of
Sludge Method Conditions Results Method Results

an
1. Waste bacterial Strains =Bacillus Extracellular polymeric Anaerobic Suspended solids Kavitha et al., 2013
activated enzymatic jerish substance decrease to digestion reduction = 48.5%
sludge pretreatment 40 mg/L COD
EDTA dosage = 0.2

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solubilization =
g/g SS
47.3%

2. Waste Microwave Power = 600 W COD solubilization up NR* NR Chang et al., 2011a

ed
activated to 8.5%
Temp = 85 oC
sludge
Duration = 2 min

3. Mix pri. And Ultrasound Energy = 480 W Dissolution of chemical Thermophilic VSS removal Chang et al., 2011b
pt
sec. sludge oxygen demand up to aerobic digestion efficiency = 55%
Duration = 30 min
44.4%
Retention Time= 3
ce

days

4. Waste Fenton Catalyst iron Sludge disintegration Anaerobic Total methane Sahinkaya et al.,
activated dosage = 4 g/kgTS, increased up to 23.6% Digestion production 2015
Ac

sludge H2O2dosage = 40 increased = 26.9%

g/kgTS , pH = 3
Duration= 60 min

5. Sewage sludge Thermal Temp:120 oC, Soluble carbon Anaerobic Increase in Serrano et al., 2015
digestion methane
Pressure = 2atm concentration, nitrogen,
production =29%
and phosphorus
Duration = 15 min
increased by 165%,
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16%, and 24%,
respectively

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6. Waste Alkali NaOH Dosage = 157 Pre-treatments reduced Anaerobic Increase in Ruiz-Hernando et
activated g /kg TS the viscosity of the digestion methane al., 2014
sludge sludge production = 34%

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7. Waste Low thermal Temp= 70 and 90 Sludge disintegration Anaerobic batch Increase in Ruffino et al., 2015
o
activated C, rate was increased up to digestion methane

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sludge 25% production = 21%
Duration= 180 min

8. Waste Mechanical Mixing= 5000 rpm Sludge disintegration NR NR Ruffino et al., 2015

ed
activated rate was increased up to
Duration= 10 min
sludge 1.5 %

9. Waste high pressure Temp= 150 oC 36% of Aerobic digestion Increase in total Burger and Parker,
activated thermal Pressure = 3 bars activeHeterotrophs mass= 21% 2013
pt
sludge hydrolysis converted to readily
Duration = 30 min
biodegradable COD
ce

and 64% remaining to

slowly biodegradable
COD
Ac

10.Mix waste UV- Catalyst= TiO2 Soluble COD Anaerobic Methane Liu et al., 2014
activated and Photocatalysis concentration increased digestion production=
Duration: 4h daily
digested from 1087.2 to 1451.6 1266.7 ml/l-
sludge Temperature= 35 oC, mg/l for 8 h sludge, VS
UV intensity= 0.7 pretreatment reduction = 67.4%
mW/cm2 ,Total COD
reduction= 60.5%

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11.Waste Visible- Increase COD Anaerobic Up to 7866.7 Liu et al., 2013b
Activated Photocatalysis degradation up to digestion mmol H2/l-sludge

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Sludge 61.1% of hydrogen
production were
achieve

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1 *NR: Not Reported

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pt
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1 Table 3: Effect of various combined pretreatment methods on sludge solibilization and subsequent biological treatment

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Combine Pretreatment Method Subsequent Biological Treatment Reference
S Type of
# Sludge Method Conditions Results Method Results

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Power= 600W
1 Waste Microwave- COD solubilization Aerobic Soluble COD Chang et
Duration= 2 min
activated Alkali increased up to 46% digestion reduction = 93% al., 2011a
sludge VSS reduction= 63%

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2 Thicken Bioleaching Bioleaching= 2 days Volatile solids NR* NR Liu et al.,
sewage -Fenton H2O2 dosage= 0.12 mol/l reduction up to 36.93 2015c
Fe2+ dosage= 0.036 mol/l

ed
sludge %. Sludge resistance
Duration = 60 min
to filtration was 3.43 ×
108 s2/g.
Increased dewater
pt
ability by 4%.
ce

3 Waste Microwave- Power= 900W Sludge solubilization Mesophilic COD degradation = Tyagi, and
activated Alkali Temp= 95oC-pH = 12 increased from 0.5% aerobic 81.1% Lo, 2012
Ac

sludge (NaOH) (raw) to 52.5% (pre- digestion VSS degradation =

treated) 72.4% VSS Retention
time = 20 days

4 Textile Ultrasonic- Ultrasonic density= 0.14 The floc structure NR NR Ning et

dying Fenton W/ml , pH < 3.0, disruption, increased al., 2014
sludge from 1.48% to 6.96%

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5 Secondar Ultrasonic- Ultrasonic density= 10 Sludge disintegration NR NR
y sludge Acid W/mL, Duration= 10 increased up to 40%

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min, pH= 2.0 . Sahinkaya
, 2015

6 Meat Alkaline- Temp= 140 oC Sludge disintegreation Anaerobic Increase in biogas Erden et

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processin Microwave Duration= 30min degree increased up to digestion production= 44.5% al., 2013
pH= 13
g 54.9.VS solubilization
wastewat increased up to 42.5%
er sludge

M
7 Excess Ultrasonic- Ultrasonic density= 720 Soluble COD NR NR Gong et
sewage Fenton W/l increased up to 2.1 al., 2015
Duration= 20 min

ed
sludge folds
Fe2+dosage = 0.4 g/l
H2O2 dosage = 0.50 g/l
Duration= 20 min
Mix NaOH- NaOH dosage = 100 g/kg Soluble COD Aerobic Increase in organic Yiying et
pt
8
aerobic- Ultrasonic Duration= 30 min increased from 275 to digestion matter degradation = al., 2009
Ultrasonic energy= 7500
thicken 6797 mg/l 50.7%
kJ/kg
ce

sewage
sludge

9 Primary Microwave- Microwave power =, 800 Increase in Anaerobic Methane production Yeneneh
Ac

sludge Ultrasound W, 2450 MHz disintegration of flocs digestion = 11.9 ml/g tCOD et al.,
Duration= 3 min
and extracellular 2013
US density = 0.4 W/ml
Intensity =150 W polymeric substances.
Duration= 6min.

10 Waste Free nitrous Nitrous acid = 0.52-1.11 sCOD increased and Anaerobic Methane production (Wang et
acid-heat al., 2014)
activated pre-treatment mg N/L found between 0.16- digestion increased by = 17-
sludge and 0.28 mg 26%
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sludge Temp = 70 oC and 0.28 mg 26%
sCOD/mg VS

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1 *NR: Not Reported

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3

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1 Table 4: Evaluation of various sludge treatment technologies.

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2

Pre-Treatment Energy Chemical Advantages Disadvantages

Requirement Requirement

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Biological Pre-Treatment No energy EDTA  Minimize the risks of  Difficult to maintain optimum
required pathogenic microorganisms conditions during the process
(Kavitha et al., 2013)  Energy and chemical for microorganism

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requirement is low
 Low GHG emission potential
 No significant improvements in
terms of biogas volumes

Microwave

(Chen et al., 2011 b)

Power: 600W

Temp: 85oC
ed
No chemical is
used
 MW heating can reach the
desired temperature more
rapidly
 Consumes less energy
 Microwave kill the indigenous
aerobic and anaerobic bacteria
which may reduce the
subsequent biological
pt
 Lower hazardous emission stabilization
potential  May have GHG potential due
 No addition of chemicals to consumption of energy
ce

required
Ultrasound 397 kJ/g SS No chemical is  Increase in temperature  High energy Consumption
used facilitate sludge disintegration compared to microwave
(Chen et al., 2011 b)  Pathogen removal due increase  Erosion in the sonotrode
Ac

in temperature
 Successfully applied at
industrial level  May have GHG potential due
 No addition of chemical to consumption of energy
required
 No odour generation.
 No clogging problems.
Fenton type process No energy Fe Catalyst  Production of chemical  Requirement of chemical
(Sahinkaya et al., 2015) required Fenton sludge is lesser as increase the process cost
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(Sahinkaya et al., 2015) required H2O2 compared to conventional
Fenton process

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H3PO4  No GHG emission potential  Difficulties to recover Fenton
reagent/catalyst
Thermal Temp:120 oC, No chemical  Complete sludge disinfection  High energy consumption
requirement  Produce acids during thermal
Pressure = 2atm

an
(Serrano et al., 2015) hydrolysis decreased biological
stabilization

 High temperature may formed

M
recalcitrant non-biodegradable
compounds

ed
 Fouling of heat exchangers in
full scale application
pt
 May have GHG potential due
to consumption of energy
Alkali No Energy NaOH  Alkaline pre-treatment is more  Not all solubilized organic
ce

requirement effective in terms of organic components are biodegradable

(Ruiz-Hernando, et al., matter solubilization as
2014) compared to thermal hydrolysis
 No GHG emission potential
Ac

UV- Photocatalysis Temperature= 35 TiO2  High recovery of chemical  High energy demand due to
o
C, catalyst requirement of ultraviolet light
(Liu et al., 2014)  Low GHG emission potential  UV radiation may kill
UV intensity= 0.7 indigenous microorganisms
mW/cm2  Recovery of catalyst is difficult
 No full scale application

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Vis-Photocatalysis Solar energy AgX/TiO2 films  Low energy requirement due to  No full scale application
dependency on solar energy  Catalyst may have

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(Liu et al., 2013b)  Catalyst can be recover and antimicrobial property
reused
 No GHG emission potential

an
Focused pulsed 34 kWh/m3 NaCl  Rapid pulsing degrade complex  Requires high high-voltage
organic compounds easily electric field
(Lee and Rittmann,

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2011)

Combine thermal with Temp: 70 oC Nitrous acid  High energy recovery as  Demands energy for high
Free nitrous acid (Wang compared to that in single temperature
Duration = 24 h  Chemical requirement increase

ed
et al., 2014b) pretreatment
the process cost
1 *The advantages and disadvantage are provide on overall technology basis not only from respective citation mentioned in the table

2
pt
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