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Intensification of Biogas production using pretreatment based on

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Article  in  Ultrasonics Sonochemistry · November 2015

DOI: 10.1016/j.ultsonch.2015.11.009

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 Ultrasonics Sonochemistry 30 (2016) 79–86

Contents lists available at ScienceDirect

Ultrasonics Sonochemistry
journal homepage: www.elsevier.com/locate/ultson

Intensification of biogas production using pretreatment

based on hydrodynamic cavitation
Pankaj N. Patil a, Parag R. Gogate a, Levente Csoka b,⇑, Agota Dregelyi-Kiss c, Miklos Horvath c
a
Department of Chemical Engineering, Institute of Chemical Technology, Mumbai 400 019, India
b
University of West Hungary, Institute of Wood Based Products and Technologies, 9400 Sopron, Hungary
c
Obuda University, Donat Banki Faculty of Mechanical and Safety Engineering, 1081 Budapest, Hungary

a r t i c l e i n f o a b s t r a c t

Article history: The present work investigates the application of hydrodynamic cavitation (HC) for the pretreatment of
Received 6 October 2015 wheat straw with an objective of enhancing the biogas production. The hydrodynamic cavitation reactor
Received in revised form 6 November 2015 is based on a stator and rotor assembly. The effect of three different speeds of rotor (2300, 2500,
Accepted 6 November 2015
2700 rpm), wheat straw to water ratios (0.5%, 1% and 1.5% wt/wt) and also treatment times as 2, 4 and
Available online 7 November 2015
6 min have been investigated in the work using the design of experiments (DOE) approach. It was
observed that the methane yield of 31.8 ml was obtained with untreated wheat straw whereas 77.9 ml
Keywords:
was obtained with HC pre-treated wheat straw confirming the favourable changes during the pre-
Biogas
Hydrodynamic cavitation
treatment. The combined pre-treatment using KOH and HC gave maximum yield of biogas as 172.3 ml.
Process intensification Overall, it has been established that significant enhancement in the biogas production can be obtained
Chemical treatment due to the pretreatment using HC which can also be further intensified by combination with chemical
Anaerobic digestion treatment.
Ó 2015 Elsevier B.V. All rights reserved.

1. Introduction and carbohydrates are typically hydrolysed to amino acids, long-

Conventional sources of energy like fossil fuels and oil are
depleting at a very fast rate imparting the need of developing alter-
nate sources of energy. Biogas, a clean and renewable source of
energy, can be a good substitute for the conventional sources of
energy. Biogas can be produced using different approaches and
one of the sustainable approaches is based on the use of waste lig-
nocellulosic biomass including the agricultural residues which is of
considerable importance to the agriculturally dominated countries
like India. Wheat is grown in significant amounts in most of the
Indian, European and Chinese regions and after the main harvest-
ing, remaining straw offers a lucrative source of biomass to be used
for biogas production. Anaerobic digestion is the commonly
employed approach worldwide for commercial production of bio-
gas from organic materials including sustainable biomass. Anaero-
bic digestion is a biological method, typically including four steps,
in which organic material is disintegrated by a variety of microbes
under oxygen free conditions resulting into the production of bio-
gas [1–3]. In the first step of the process, the extracellular enzymes
produced by hydrolytic microbes hydrolyse the complex organic
polymers to simple soluble monomers. In this step, proteins, lipids,
⇑ Corresponding author.
E-mail address: levente.csoka@skk.nyme.hu (L. Csoka).
chain fatty acids, and sugars, respectively. In the next step, these
small molecules are converted by the fermentative bacteria to a
mixture of volatile fatty acids and other minor products such as
alcohol. In third step of the process, acetogenic bacteria convert
the volatile fatty acids to acetate, carbon dioxide, and/or hydrogen,
which provide direct substrates for methanogenesis, which is the
last step resulting in the production of biogas [4]. Methanogenesis
is commonly considered to be the rate-limiting step in the anaer-
obic digestion as methanogens are believed to have slowest growth
rate [5]. However, for the degradation of lignocellulosic biomass,
hydrolysis is more commonly observed to be the rate limiting step
[6] especially when refractory biomass such as waste residues is
used.
Lignocellulosic biomass like wheat straw mainly consists of
three types of polymers, namely cellulose, hemicellulose, and lig-
nin. The carbohydrate components i.e. cellulose and hemicellulose
are fermentable after hydrolysis, which makes lignocellulosic bio-
mass a suitable feedstock for biogas production. But, the inherent
characteristics of native lignocellulosic biomass, like structural
and chemical properties, make it resistant to biodegradation by
enzymes and microbes. Wheat straw pre-treatment earlier to
anaerobic digestion is generally required to reduce the structural
and compositional barriers present in the lignocellulosic biomass
and expose the polymer chains of cellulose and hemicellulose to

http://dx.doi.org/10.1016/j.ultsonch.2015.11.009
1350-4177/Ó 2015 Elsevier B.V. All rights reserved.
80 P.N. Patil et al. / Ultrasonics Sonochemistry 30 (2016) 79–86
microbial breakdown so as to enhance the rate of biomass degra-
dation and biogas yield. Because of the complexity and inconsis-
tency of biomass chemical structures, the optimal pre-treatment
method and conditions depend on the type of lignocellulosic
materials used for processing and cannot be generalised.
Pre-treatment methods can be broadly classified into three
types namely physical, chemical and biological. Physical pre-
treatment approaches do not use any chemicals or microorganisms
and includes techniques like comminution [7,8], liquid hot water
pre-treatment [9], steam-explosion [10,11], irradiation [12,13]
and extrusion [14]. In the case of liquid hot water pre-treatment,
pressure is used to keep water in the liquid state at higher temper-
atures. Biomass experiences high temperature cooking in water at
a high pressure and water can enter into the biomass cell structure,
hydrating cellulose, solubilising hemicellulose, and to some extent
removing lignin [15,16]. In steam explosion method, biomass
particles are heated with high-pressure saturated steam for a short
period of time and the pressure is rapidly reduced to stop the
reactions, due to which the biomass experiences an explosive
decompression. Steam-explosion was reported to be an efficient
technology for increasing methane yield from wheat straw by
20–30%, as compared to untreated wheat straw [17]. Irradiation
methods are based on the use of microwave, gamma-ray, and elec-
tron beam treatment. Jackowiak et al. [18] investigated the optimi-
sation of a microwave pre-treatment of wheat straw for methane
production and reported about 30% enhancement in the methane
yield as compared to untreated wheat straw. Extrusion is another
physical pre-treatment process where biomass is fed into one
end of the extruder and transported along the length of the barrel
with a driving screw. By means of the material passages along the
barrel, it is exposed to friction and vigorous shearing upon pressure
release at the finishing end [19] giving structural changes in the
processed straw enabling easy digestion in the subsequent step.
Chemical pre-treatment refers to the usage of chemicals, like
acids [20,21], bases [22,23], and ionic liquids [24] for alteration
of the physical and chemical characteristics of lignocellulosic bio-
mass. Due to the use of chemicals, this may not be a preferred
approach for sustainable processing. Biological pre-treatment for
improvement of biogas production in anaerobic digestion has
primarily focused on fungal pre-treatment [25], pre-treatment by
microbial consortium [26], and enzymatic pre-treatment [10].
Biological approaches, though sustainable, are often criticised by
the slowness of the process and significant costs associated with
the enzymes. A critical analysis of these pre-treatment approaches
directs that, while different biomass pre-treatment techniques
have been reported, each of the approaches have limitations as
use of toxic chemicals, significant treatment times, requirement
of very high temperatures and pressures or the energy intensive
operations. It is thus very important to develop energy efficient
as well as cost efficient pretreatment technique, which can be
applied for the intensification of the biogas production. Cavitation,
generated using ultrasound or hydrodynamic cavitation also offers
promise for intensification of different physical and chemical pro-
cessing applications [27]. Cavitation can be produced by passage of
ultrasonic waves through the liquid medium (acoustic cavitation)
or by making use of the alternations in the liquid flow in the
hydraulic systems (hydrodynamic cavitation). Ultrasound induced
cavitation has been generally applied for intensification of sludge
digestion and also for biogas production [28–30] though the use
of hydrodynamic cavitation has not been significantly investigated.
This is despite the fact that hydrodynamic cavitation offers energy
efficiency way of achieving physicochemical transformations
[31,32]. Some of the earlier studies dealing with application of
hydrodynamic cavitation for treatment of lignocellulosic materials
include delignification of wheat straw for paper manufacturing
[33] and delignification of wood to obtain cellulosic pulp fibres
[34]. The present work reports the use of hydrodynamic cavitation
for intensification of biogas production based on the pretreatment
of sustainable biomass. Structural and chemical properties of bio-
mass make it resistant to biodegradation by microbes. The collapse
of the cavities in the case of hydrodynamic cavitation, results in
release of large magnitudes of energy which helps in dissolution
of lignin in biomass and make it more suitable for subsequent bac-
terial decomposition possibly giving in higher yields of biogas dur-
ing the anaerobic digestion process. Milled wheat straw is used as
the sustainable substrate for the biogas generation. There have
been no earlier studies related to the use of hydrodynamic cavita-
tion and hence this forms the novel aspect of the current work. In
the case of pretreatment using hydrodynamic cavitation, the main
energy consuming part is only the motor used for rotation of the
rotor. So the operating cost is associated with only electricity
consumption by the motor which is relatively low and can be neg-
ligible compared to the extra biogas and methane yields that can
be obtained. KOH chemical costs contributes in some extent, but
compared to the reduction that can be obtained due to the use of
waste agricultural straw, overall it has no significant contribution
to the pretreatment cost.
2. Materials and methods
2.1. Materials
Milled wheat straw (finely chopped) with size over the range of
0.125–1 mm was used for the experimental investigations. Initially
wheat straw was chopped to 5 mm length using standard straw
chopper and then it was again chopped and screened to a size of
0.125–1 mm. Industrial sludge was obtained from South-Pest
Wastewater Treatment Plant, Budapest, Hungary, which is typi-
cally developed for the treatment of effluents from households.
The corresponding COD value of the used domestic sludge was
around the standard value, 1 g/ml. The finely chopped wheat straw
was pre-treated with the help of hydrodynamic cavitation device
and chemical retting.
2.2. Equipments
The hydrodynamic cavitation device used for the generation of
cavitation is a stator and rotor assembly. The diameter of the rotor
is 19 cm with ratio of diameter to height of the rotor as 1.9 and this
rotor is contained in a cylinder with diameter of 21 cm. Gap
between the stator and the rotor is fixed at 10 mm. Rotor is
attached to a gear assembly, which is connected to a variable fre-
quency drive (VFD). With the help of VFD, the rotor can be rotated
at different speeds of rotation in a restricted annular space and
chopped straw suspended liquid is passed through the opening
between the stator and the rotor. On the surface of the rotor,
indentations are provided which are responsible for generation of
cavitating conditions. There are a total 204 indentations equidis-
tant from each other. Each indentation is 12 mm in diameter and
20 mm deep. During the passage of liquids through the equipment,
the liquid at very high velocities enters to the indentation due to
rotary action of the cylinder and when liquid comes out from the
indentation due to centrifugal flow, a low pressure region is gener-
ated near the upper surface of the indentations which results into
cavitation [33]. The schematic representation of experimental
setup used for the investigations has been shown in Fig. 1 whereas
the schematic of an indentation on the rotor has been given in
Fig. 2. The intensity of the cavitational effect and its inception
can be established with the cavitation number and the calculations
related to the stator-rotor assembly has been presented in our
earlier work [35].
 P.N. Patil et al. / Ultrasonics Sonochemistry 30 (2016) 79–86
Fig. 1. Schematic representation of the experimental setup for pretreatment using hydrodynamic cavitation.
Fig. 2. Schematic representations of the indentations on the rotor.
2.3. Experimental procedure
The setup operates as a closed loop where the slurry from the
holding tank is pumped into the cavitating device by using an open
impeller type pump (7.5 kW) and the flow rate/pressure are con-
trolled using the flow control valves. The typical parameters
selected for investigating the effect of pre-treatment are the load-
ing of the wheat straw in feed (wt/wt%), time of treatment (circu-
lation time in min) and speed of rotation of the rotor (rpm). Design
of experiments was made and data for the selected levels of DOE
have been given in Table 1. All the experiments were performed
with tap water and at room temperature. Experiments were car-
ried out at a capacity of 15 L for the pre-treatment of the wheat
straw. The required amount of the pre-treated wheat straw was
then mixed with the industrial sludge in a 500 ml glass bottle as
per the VDI 4630 (Verein Deutscher Ingenieure) standards descrip-
tion [36]. This glass bottle was sealed with 3 mm silicone sealing at
Table 1
Settings for the parameter levels for the DOE.
Parameter Levels of factors
1 +1
Dry matter content (%) 0.5 1.5
Time of treatment (min) 2 6
Speed of rotation (rpm) 2300 2700
81
the top and the empty portion in the bottle was filled with nitrogen
to take out the oxygen present in the bottle. Second glass bottle
containing 500 ml distilled water was subsequently connected to
this first bottle with the rubber tubing so that the gas produced
in the first bottle will come into the second bottle. Second bottle
is connected to third empty bottle with rubber tubing, through
which the displacement of distilled water from second bottle to
third bottle takes place. Such an arrangement of bottles was made
for all the 9 samples pre-treated with hydrodynamic cavitation
under different sets of operating parameters. The 10th arrange-
ment of bottles was for positive control which contains the cellu-
lose instead of pre-treated wheat straw whereas another
arrangement contains only the untreated wheat straw. This batch
arrangement of three bottles was then placed in the thermostat
and temperature was maintained at 37 °C. Amount of biogas pro-
duced was measured at regular time intervals and methane con-
tents were also analysed at the same time. The process was
carried out till 16th day when no displacement of water was
observed after this time.
To study the effect of chemical pre-treatment on the biogas
enhancement, the chopped wheat straw was retted in alkaline
solution of 0.3 M potassium hydroxide (KOH), water to straw ratio
was 12, for 48 h for pre-softening of lignin cellulose complex at
room temperature. Mixing of this retted pulp was performed every
12 h during the chemical treatment to obtain well mixed condi-
tions. This retted wheat straw was then diluted to 1 wt% to be able
to pump the slurry into hydrodynamic cavitation reactor (pH of
the solution also came to about neutral during this dilution) and
then treated in hydrodynamic cavitation device in the same man-
ner as discussed above. This combination approach was also used
to check the efficacy of combined chemical/physical treatment
approaches.
2.4. Analysis
The COD value of the substrate pre-treated using hydrodynamic
cavitation device at different settings was determined by the per-
manganate method with sampling from the solution [37]. Biogas
produced in the first bottle is by displacing the water in second bot-
tle and this water comes into the third bottle. So the amount of bio-
Central point
gas produced was measured by water displacement method that is
0 by weighing the amount of water in the third bottle. For the analysis
1 of methane contents in the obtained biogas, GC – DANI Master Fast
4 Chromatograph with Restek Rt-U-BOND (15 m/0.53 mm ID/20 lm)
2500
column and FID – Flame Ionisation detector has been used.
82 P.N. Patil et al. / Ultrasonics Sonochemistry 30 (2016) 79–86

3. Results and discussion higher were the obtained COD values. If we compare the COD
obtained in second experiment (906.4 mg/dm3) with the COD
3.1. Design of experiments analysis obtained in fourth experiment (1334.8 mg/dm3), it can be observed
increase in the dry matter content from 0.5% to 1% has indeed a sig-
The parameter selection for actual studies using hydrodynamic nificant effect. This is even more important considering that the
cavitation device was based on the experimental results obtained treatment time is more in the case of second experiment (4 min)
for the Weissler reaction which measures the iodine liberation as as compared to fourth experiment (2 min) and the speed of rota-
a measure of the cavitational effects and can be considered as tion is constant at 2500 RPM. COD obtained in the case of experi-
quantitative measure of the cavitational intensity [38]. The maxi- ments one, two and three were 772.4, 906.4, and 1045.2 mg/dm3
mum cavitational activity as measured by the Weissler reaction at same value of dry matter content, which shows that the COD
was obtained at the speeds of rotation of the rotor as 2300, 2500 also increases with an increase in the speed of rotation of the rotor
and 2700 rpm. At lower speeds of rotation, it was observed that and treatment time. An increase in the RPM as well as the treat-
the velocities generated are not enough to create intense condi- ment time means that the processed material is subjected to
tions of cavitation and hence may not be sufficient for giving the higher intensity of cavitation giving enhanced degree of structural
required degree of the delignification of wheat straw based on changes in the processed material converting them into the easily
the cavitational effects. The equipment could also be operated at digestible compounds and hence is expected to be beneficial in the
a maximum of 3000 rpm which can also give more intense subsequent biogas processing step.
cavitation based on the trends but the equipment showed vibra-
tions and hence to avoid possibility of damage to the equipment, 3.3. Biogas formation with HCD based pre-treated wheat straw
it was decided to restrict the experiments at maximum speed of
2700 rpm. Considering this analysis, the three different speeds of Pre-treated wheat straw (substrate) was mixed with the indus-
rotation of the rotor selected for the DOE analysis were 2300, trial sludge and investigated for the formation of biogas. Table 3
2500 and 2700 rpm where higher cavitational effects were shows the actual values of all the experimental parameters as
observed. per VDI 4630 standards obtained in the investigations. The batch
Three different wheat straws to water ratio were selected for experiments were performed till 16 days and the obtained yields
the investigations as 0.5%, 1% and 1.5% wt/wt. Beyond 1.5%, it of biogas for different sets of experiments are reported in Fig. 3.
was difficult to run the cavitating device because at higher loading From Fig. 3, it can be observed that the amount of dry biogas
of wheat straw, clogging was observed in the cavitation chamber. obtained with untreated wheat straw is less than the biogas
Also three different treatment times were selected as 2, 4 and obtained with HCD pre-treated wheat straw in all the 9 experi-
6 min. These parameters were systematically varied in the design ments. The maximum biogas yield obtained using HCD is
of experiment (DOE) analysis to understand the effect of each fac- 241.3 ml which is much more as compared to the biogas yield
tor statistically. Each factor was varied at two levels ( 1, 1) and the obtained using untreated wheat straw. Fig. 4 shows the yields of
central point settings (0) were also examined. Similar approach of methane obtained in these sets. It can be observed that the
the design of experiment was also reported by Diószegi et al. [39]. methane yield of 31.8 ml was obtained with untreated wheat
Table 1 shows the settings of each parameter. After getting the straw whereas 77.9 ml was obtained with pre-treated wheat straw
results from DOE, different sets of experiments as shown in Table 2 in case of HCD experiment 1, which confirmed that maximum of
were performed at the capacity of 15 L for the pre-treatment of the 144% enhancement in the methane yield was obtained with HCD
wheat straw. based pre-treatment. Methane yield in each case of pre-treated
wheat straw was more as compared to the untreated wheat straw.
3.2. Selection of parameters for HCD The observed increase in the biogas and methane yield is attribu-
ted to the reduction in the structural and compositional barrier
The three parameters namely dry matter content, time of treat- of lignocellulosic biomass because of cavitating conditions of
ment and the speed of rotation were varied in the design of exper- intense turbulence as well as conditions of high shear. Due to these
iment and the obtained results of the experiments are summarised effects, polymer chains of cellulose and hemicellulose are exposed
in Table 2. The results indicate that it is the dry matter content that to microbial breakdown so as to enhance the rate of biomass
has a very significant effect on the chemical oxygen demand (COD) degradation and biogas yield. In the process of cavitation, water
value. Typically the dissolved COD specifies the oxygen quantity molecules are also dissociated to form OH_ and H_ due to cavitating
required for the complete oxidation of components of fermentation conditions. These OH radicals are very much reactive and could be
nutrients, thus reliably demonstrating the energy content of the responsible for the oxidation of lignin molecule to some amount
fermentation nutrients [39]. Therefore, as the COD value is higher, [33]. Cavitating conditions can also result in comminution of wheat
the yield of the biogas expected from the waste material will be straw which in turns results in particle size reduction of wheat
more. It was also observed that higher the dry matter content, straw. Biomass particle size reduction can alter the inherent struc-
ture of lignocellulosic biomass, increasing the accessible surface
area, reducing the degree of cellulose crystallinity, and decreasing
Table 2
the degree of cellulose polymerisation for improved digestibility
Parameters selected using DOE.
[40].
Expt. Dry matter content (wt/ Time Rotation COD (mg/ The intensification in the biogas production with an increase in
no. wt%) (min) (rpm) dm3)
the speed of rotation can be attributed to the fact that with an
1 0.5 2 2300 772.4 increase in the rotation speed of the rotor, the cavitational inten-
2 0.5 4 2500 906.4
sity increases based on the generation of higher number of cavita-
3 0.5 6 2700 1045.2
4 1.0 2 2500 1334.8
tion events as well as intense collapse of cavities [41]. An increase
5 1.0 4 2700 1480.8 in the cavitational intensity is expected to give more favourable
6 1.0 6 2300 1850 structural changes in the processed material as well as higher
7 1.5 2 2700 2240.8 extent of delignification leading to higher extent of biogas genera-
8 1.5 4 2300 2767.2
tion. It is also important to note that too much increase in the
9 1.5 6 2500 2807.2
speed of rotation is not recommended as an increase in the speed
 P.N. Patil et al. / Ultrasonics Sonochemistry 30 (2016) 79–86 83

Table 3
HCD based experimental parameters as per VDI 4630 standards.

Experimental parameters
HCD HCD HCD HCD HCD HCD HCD HCD HCD Positive Un-
Expt. 1 Expt. 2 Expt. 3 Expt. 4 Expt. 5 Expt. 6 Expt. 7 Expt. 8 Expt. 9 control treated
Material Wheat straw Cellulose Wheat
straw
HCD rpm 2300 2500 2700 2500 2700 2300 2700 2300 2500 – –
HCD operating time (min) 2 4 6 2 4 6 2 4 6 – –
Volume of fill (ml) 160 160 160 160 160 160 160 160 160 160 160
Total solids (TS) of sludge (%) 2.53 2.53 2.53 2.53 2.53 2.53 2.53 2.53 2.53 2.53 2.53
Total organic solids (oTS) of sludge (%) 61.17 61.17 61.17 61.17 61.17 61.17 61.17 61.17 61.17 61.17 61.17
oTS of sludge div. volume of fill (%) 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5
Total oTS of sludge (g) 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40
Required amount of sludge (g) 155.1 155.1 155.1 155.1 155.1 155.1 155.1 155.1 155.1 155.1 155.1
Total solids (TS) of substrate (%) 0.50 0.50 0.50 1.00 1.00 1.00 1.50 1.50 1.50 98.35 95.55
oTS of substrate (%) 94.19 94.19 94.19 94.19 94.19 94.19 94.19 94.19 94.19 99.91 94.19
oTS of 100 g substrate (g) 0.47 0.47 0.47 0.94 0.94 0.94 1.41 1.41 1.41 98.26 90.00
Required oTS of substrate (g) 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20
Required amount of substrate (g) 254.8 254.8 254.8 127.4 127.4 127.4 84.9 84.9 84.9 1.2 1.3
Ratio of substrate and sludge oTS (1) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5
Total solids of fill (%) 1.30 1.30 1.30 1.30 1.30 1.30 1.30 1.30 1.30 1.28 1.30

Fig. 3. HCD based normalised dry biogas yields referred to 1 g TS.

Fig. 4. HCD based normalised methane yields referred to 1 g TS.

of rotation also increases the slip between the water layer and the are generated and such a large numbers of cavities tend to dampen
rotor, which acts in detrimental manner for the extent of cavita- the collapse reducing the energy released by the neighbouring cav-
tion. At significantly higher speeds of rotation, supercavitation is ities [42]. Regarding the effect of time of treatment, it can be
likely to occur which means that very large numbers of cavities explained by the fact that as treatment time increases, exposure
84 P.N. Patil et al. / Ultrasonics Sonochemistry 30 (2016) 79–86

Table 4
Combination of HCD and KOH based experimental parameters as per VDI 4630 standards.

Designation HCD HCD HCD HCD HCD HCD HCD HCD Only Un- Positive
Expt.1 Expt.2 Expt.3 Expt.4 Expt.5 Expt.6 Expt.7 Expt.8 KOH treated control
Material Wheat straw Wheat straw + KOH Wheat Cellulose
straw
HCD rpm 2500 2500 3000 3000 2500 2500 3000 3000 – – –
HCD operating time (min) 2 4 2 4 2 4 2 4 – – –
Volume of fill (ml) 160 160 160 160 160 160 160 160 160 160 160
Total solids (TS) of sludge (%) 1.66 1.66 1.66 1.66 1.66 1.66 1.66 1.66 1.66 1.66 1.66
Total organic solids (oTS) of sludge (%) 66.31 66.31 66.31 66.31 66.31 66.31 66.31 66.31 66.31 66.31 66.31
oTS of sludge div. volume of fill (%) 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5
Total oTS of sludge (g) 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40 2.40
Required amount of sludge (g) 218.0 218.0 218.0 218.0 218.0 218.0 218.0 218.0 218.0 218.0 218.0
Total solids (TS) of substrate (%) 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 95.55 98.35
oTS of substrate (%) 93.57 93.57 93.57 93.57 93.57 93.57 93.57 93.57 93.57 93.57 99.91
oTS of 100 g substrate (g) 0.47 0.47 0.47 0.47 0.47 0.47 0.47 0.47 0.47 89.41 98.26
Required oTS of substrate (g) 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20
Required amount of substrate (g) 256.5 256.5 256.5 256.5 256.5 256.5 256.5 256.5 256.5 1.3 1.2
Ratio of substrate and sludge oTS (1) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5
Total solids of fill (%) 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.21

Fig. 5. Combination of HCD and KOH based normalised dry biogas yields referred to 1 g TS.

time of lignin-cellulose complex to cavitation also increases, which
in turn increases the overall delignification [33], which directs
higher yields of biogas.
3.4. Intensification of biogas formation with combination of KOH and
HCD based pre-treated wheat straw
Alkaline pre-treatment using bases such as KOH, NaOH, and Ca
(OH)2 also intensifies the removal of lignin, hemicellulose, and cel-
lulose. Due to this removal, lignocellulosic biomass becomes more
degradable to microbes and enzymes. Dong et al. [43] reported that
KOH and NaOH pretreatment to rice straw resulted in achievement
of enhancement of biogas yield of 50%. Use of KOH offers environ-
mental benefits as compared to NaOH and Ca(OH)2 based on the
fact that the waste stream containing KOH, which may be pro-
duced after treatment can be used as a fertiliser [4]. Under alkaline
conditions, H2O2 dissociates to form the hydroperoxy radical
which can again react with the residual H2O2 to form highly reac-
tive OH radicals and superoxide (O2) [33]. Stabilised lignin and its
intermediates also under series of radical reactions described as
lignin condensation with the hydroxyl and hydroperoxy radicals
to form organic acids, carbon dioxide and other low molecular
weight organic products through the side chain elimination, ring
opening and demethoxylation process [44]. Use of only KOH is
incapable of significant pre-treatment of wheat straw in short span
of time and hence the present work investigated the combined pre-
treatment of wheat straw in alkaline conditions with hydrody-
namic cavitation. The experimental parameters selected in the pre-
sent study for this combination have been reported in Table 4.
Fig. 5 shows the yields of biogas obtained with the combination
of KOH and HCD for the pre-treatment of wheat straw. It can be
observed that untreated wheat straw gave 110.8 ml whereas
KOH pre-treated sample gave 146.1 ml yield of biogas which
clearly shows that yield of biogas can be enhanced by pre-
treating the wheat straw with KOH. HCD experiments 1–4 were
performed without using KOH pre-treatment. Yields obtained in
case of experiment 1 and 3 shows that yield of biogas obtained
in the case of experiment 1 (121.5 ml) is greater as compared to
experiment 3 (116.4 ml) which means that 2500 rpm of rotor is
better as compared to 3000 rpm. Also yield of biogas obtained in
2 min pre-treatment is less than that obtained with 4 min of oper-
ation which shows that higher pre-treatment time results in more
yields of biogas.
HCD experiments 5–8 are performed with KOH pre-treatment
and it can be observed that the yields obtained with combine
pre-treatment are more as compared to individual KOH and HCD
based pre-treatment. Maximum of 172.3 ml biogas was obtained
in the case of HCD experiment 6 as compared to 110.8 ml biogas
 P.N. Patil et al. / Ultrasonics Sonochemistry 30 (2016) 79–86
Fig. 6. Combination of HCD and KOH based normalised methane yields referred to 1 g TS.
obtained without pre-treatment. Hence it can be established that
the combination of chemical pre-treatment and cavitation based
treatment results in the significant process intensification benefits
for yields of biogas.
Fig. 6 shows that the methane yields obtained with different
experimental conditions and it can be observed that the methane
yield obtained in the case of untreated wheat straw (25.9 ml) is
lower as compared to 40.2 ml obtained with KOH pre-treated
wheat straw. Similar trends have been reported in the literature.
Wheat straw pre-treated with 4% NaOH (g/g TS) at 37 °C for 5 days
showed an increase in methane yield of 112% compared with
untreated material in anaerobic digestion [45]. It is important to
note that no study related to the combination of hydrodynamic
cavitation and chemical treatment can be observed in the open lit-
erature to the best of our knowledge. To give credence to the
observed intensification in the present work, some similar results
obtained for the combination of ultrasound with chemical
treatment has now been presented which also works on similar
mechanism of intensification. Packyam et al. [46] have studied
the effect of sonically induced deflocculation on the efficiency of
ozone mediated partial sludge disintegration for improved produc-
tion of biogas and reported that the sonic pretreatment resulted in
enhanced release of the organic matters from inner fractions
(TB-EPS and LB-EPS) to outer fractions (slime-soluble). Prell et al.
[47] have reported the influence of ultrasound treatment of fer-
mentation broth under optimised intensity to improve and acceler-
ate biogas production. Oz and Uzun [48] have compared the biogas
and methane production rates of anaerobic batch reactor fed with
the ultrasound pre-treated olive mill wastewater (OMW) samples
with the results of control reactor fed with untreated OMW in
order to determine the effect of sonication. It has been reported
that the application of low frequency ultrasound to OMW signifi-
cantly improved both biogas and methane production in anaerobic
batch reactor fed with the wastewater.
4. Concluding remarks
Hydrodynamic cavitation provides a promising approach which
can be applied for increasing anaerobic digestion efficiency of lig-
nocellulosic biomass like wheat straw. Hydrodynamic cavitation
devices are comparatively easy to scale up and various operating
parameters such as rotation speed of the rotor, percentage of bio-
mass and the time of treatment can be easily optimised depending
upon the different types of biomass. In the case of wheat straw to
water ratio, it was observed that beyond 1.5% it was difficult to run
the cavitating device because at higher percentage the clogging
85
was observed in the cavitation chamber. Optimisation of speed of
rotation using the Weissler reaction revealed that the maximum
cavitational activity is obtained at 2300 and 2500 rpm. Biogas
and methane yields in each case of pre-treated wheat straw were
more as compared to untreated wheat straw. It was also estab-
lished that the maximum biogas yield obtained using HCD under
optimum conditions is almost double as compared to the biogas
yield obtained using untreated wheat straw. Use of only KOH
was observed to be not significantly efficient for the pre-
treatment of wheat straw but combination of alkaline treatment
with hydrodynamic cavitation resulted in generation of additional
hydroxyl and hydroperoxy radicals required for delignification
reaction thereby intensifying the overall rates of reactions. The
maximum biogas produced using HCD based pre-treatment is
241 ml which is almost double as compared to the biogas produced
using untreated wheat straw (128 ml). Overall it can be concluded
that hydrodynamic cavitation is an efficient pre-treatment strategy
for enhancing the production of biogas from wheat straw using the
route of anaerobic digestion.
Acknowledgement
PRG would like to acknowledge the support of TEQIP-Center of
Excellence in Process Intensification for the visit leading to this col-
laborative research.
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