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Research article
A R T I C LE I N FO A B S T R A C T
Keywords: Hard lignocellulosic structure of wheat straw is the main hindrance in its anaerobic digestion. Thus, a laboratory
Thermal pretreatment scale batch experiment was conducted to study the effect of thermal pretreatment on anaerobic digestion of
Wheat straw wheat straw. For this purpose, different thermal pretreatment temperatures of 120, 140, 160 and 180 °C were
Lignocellulosic material studied and the results were compared with raw wheat straw. Significant differences in biogas production were
Biogas production
observed at temperature higher than 160 °C. Highest biogas yield of 615 Nml/gVS and volatile solids reduction
Kinetic model
of 69% was observed from wheat straw pretreated at 180 °C. Wheat straw pretreated at 180 °C showed 53%
higher biogas yield as compared to untreated. Further, FTIR analysis revealed change in chemical bonds of
lignocellulosic structure of wheat straw. Modified Gompertz model was best fitted on biogas production data and
predicted shorter lag phase time and higher biogas production as the pretreatment temperature increased.
Overall, change in lignocellulosic structure and increase in cellulose content were the main reason in enhancing
biogas production.
1. Introduction hence limits its biodegradation rate. Thus, suitable pretreatment is re-
quired to enhance digestibility of lignocellulosic wheat straw.
Energy is a vital element for continued economic growth and de- Various pretreatment methods are used for increasing the anaerobic
velopment. Unfortunately, Pakistan is facing numerous problems due to digestibility of lignocellulosic waste. These include dilute acid pre-
energy deficiency. To overcome severe power crisis the country is treatment (Schell et al., 2003), mechanical pretreatment for size re-
looking for different renewable and sustainable energy options. In this duction (Mshandete et al., 2006), microbial pretreatment (Mustafa
scenario bioenergy can play a crucial role since bioenergy is considered et al., 2016) and microwave pretreatment (Sapci, 2013). These pre-
as fourth largest energy resource in the world. Enormous source of treatments alter the lignocellulosic structures by breaking the chemical
agricultural biomass is available for bioenergy production in Pakistan. bonds, which may increase the potential of cellulose hydrolysis and
It is estimated that the country generates around 69 million tons of field biogas production (Fang et al., 2015; Jaffar et al., 2016; Wang et al.,
based agricultural crop residues annually (Raheem et al., 2016). Wheat 2016). However, there are certain limitations in the use of these pre-
straw is one of crop residue types produced in huge quantities from treatments. For instance, chemical pre-treatment produces secondary
agricultural fields. Pakistan produces approximately 25 million tons of pollution and biological pre-treatment conditions are difficult to con-
wheat straw every year (Arshadullah et al., 2012). trol, and combined pre-treatment usually has the disadvantages of both
Anaerobic digestion of wheat straw could be a promising way of chemical and biological methods. In comparison, physical pre-treat-
bioenergy production as it reduces various problems originated from its ment methods are most commonly used due to operational convenience
inadequate disposal. However, the process consists of many stages in- and low investment (Haghighi Mood et al., 2013).
cluding hydrolysis, acidogenesis and methanogenesis, out of which Thermal pretreatment is a type of physical pretreatment in which
hydrolysis is considered as the rate-limiting step in anaerobic digestion the lignocellulosic biomass is subjected to heating at a certain tem-
of wheat straw due to its lignocellulosic nature. In a lignocellulosic perature and pressure. The temperature range for this purpose could be
biomass like wheat straw, the connected structure of lignin and hemi- 50–240 °C. Depending on the type of heating method, it could be called
cellulose provides physical barrier to degradation of cellulose and as thermal pretreatment, hydrothermal pretreatment, steam explosion
∗
Corresponding author.
E-mail addresses: zeshansheikh@iese.nust.edu.pk, zeshan90@gmail.com (Zeshan).
https://doi.org/10.1016/j.jenvman.2018.05.011
Received 12 December 2017; Received in revised form 29 April 2018; Accepted 5 May 2018
Available online 26 May 2018
0301-4797/ © 2018 Elsevier Ltd. All rights reserved.
A.A. Rajput et al. Journal of Environmental Management 221 (2018) 45–52
Table 1
Overview of effect of thermal pretreatment on AD of lignocellulosic biomass.
Biomass Pretreatment Pretreatment conditions Findings References
Wheat straw Thermal pretreatment 150–220 °C for 1–15 min 20% increase in methane production Ferreira et al. (2013)
Wheat straw Steam explosion 180 °C for 15 min Increased 20% methane yield Bauer et al. (2009)
Washed vinegar residue Hydrothermal 80, 120 and 160 °C for 160 °C pretreated biomass showed 55.99% higher Ran et al. (2018)
pretreatment 30 min methane yield
Rice straw Hydrothermal 90, 150, 180 and 210 °C for 3% increase in biogas yield at 90 and 180 °C and 30% Wang et al. (2018)
pretreatment 15 min decrease at 210 °C compared to control
Urban and industrial waste Thermal 60, 80, 100, 120 °C for Increased in biogas yield of 27 and 37% at 120 °C Ennouri et al. (2016)
activated sludge Pretreatment 30 min
Dewatered sludge Thermal 160 °C and 0.55 Mpa for 45.7% increase in biogas production Chen et al. (2018)
Pretreatment 30 min
Wheat straw and sugarcane Thermal pretreatment 121 °C for 60 min 29% increase in methane production from wheat Bolado-Rodríguez et al.
bagasse straw and 11% from sugarcane bagasse (2016)
or microwave heating (Table 1). Menardo et al. (2012) studied the ef- 2.2. Thermal pretreatment
fect of thermal pretreatment on anaerobic digestion of wheat, barley
and rice straw and maize stalk at pretreatment temperature of 90 and The thermal pretreatment of wheat straw was performed in a
120 °C for 30 min and found 64.2, 40.8, 32.4 and 7.1% increase in 250 mL stainless steel reactor with an inserted Teflon box. In Teflon
methane yield respectively at 120 °C compared to untreated control. inserted reactor, 80 g sample of wheat straw was taken, and 20 g of
Similarly, hydrothermal pretreatment of wheat straw at 200 °C for distilled water was added into it to avoid burning of dry biomass during
10 min showed 20% increase in methane yield (Chandra et al., 2012). pretreatment. The stainless-steel reactor was fully tightened and placed
Another study reported 27% increase in methane yield from thermally in a high temperature box resistance furnace – x series (SX-5-12, China).
pretreated wheat straw at 200 °C for 5 min as compared to control Thermal pretreatment temperatures were set at 120, 140, 160 and
(Ferreira et al., 2014). Most of the studies mentioned here and in 180 °C, and after 60 min of thermal pretreatment the reactor was cooled
Table 1 used high temperature with a short pretreatment time. On the down using cold water. Finally, the pretreated wheat straw samples at
other hand, a relatively long pretreatment time of 60 min at lower different temperatures were dried and stored in a vacuum plastic bag
pretreatment temperatures of 60, 70, 80, 90 and 100 °C has been used until use. Thermal pretreatment of wheat straw was performed in tri-
in a recent study (Chen et al., 2017) for thermal pretreatment of textile plicate.
dying sludge, in which the highest methane yield was produced from
the sludge pretreated at 100 °C. Thus, effect of thermal pretreatment of 2.3. Batch anaerobic digestion experiments
wheat straw at medium temperatures and long residence time on biogas
production has not been studied before and it may produce new in- In this study, wheat straw pretreated at four different thermal pre-
formation in the area. treatment temperatures was compared for biogas production. Serum
Mathematical kinetic models play vital role in design and optimi- bottles of 300 mL with working volume of 225 mL were used as batch
zation of any process (Batstone, 2006). To assess the performance of reactors. Calculated quantities of substrate and pre-incubated inoculum
anaerobic digestion (AD) process, several kinetic models have been (20% of working volume) were taken in reactors to achieve the organic
used by researchers, which include Chen and Hashimoto model (Chen loading of 10 gVS L−1 at substrate to inoculum (S/I) ratio of 1 (on gVS
and Hashimoto, 1980), Monod model (Zamanzadeh et al., 2013), first basis). After taking the substrate and inoculum, the reactors were flu-
order model (López et al., 2015), substrate mass balance model (Zhang shed with nitrogen gas for ensuring anaerobic condition. The reactors
et al., 2015), and modified Gompertz model (Syaichurrozi and were tightly closed with rubber stopper and alumina crimp cap and
Sumardiono, 2013). Modified Gompertz model is considered very effi- placed in an incubator at 35 °C for 45 days. Mixing was provided to
cient in explaining lag phase time and sigmoidal growth curves (Pham every reactor twice a day for 2–3 min. A glass gas syringe was used to
et al., 2014) of methane production. As pretreatment of biomass affects measure daily biogas production from reactors. No external nutrients
lag phase time of the anaerobic process, it could be well explained by were added, all the required nutrients were provided by fresh inoculum
Gompertz model. The proposed kinetic models would be helpful to (digested manure). The experiment was carried out in triplicate. To get
address the theoretical contextual for AD experimental data and hence the biogas production from untreated substrate, control reactor of un-
the effectiveness of the applied pretreatment. treated wheat straw was also prepared and run. Therefore, five sets of
The overall objective of the study is to assess the effect of thermal reactors were prepared viz., untreated wheat straw, pretreated wheat
pretreatment on the biogas production of wheat straw. In addition, straw at 120, 140, 160 and 180 °C.
chemical and structural changes due to thermal pretreatment were also
studied. Further, biogas production rate was assessed in relation to 2.4. Analytical parameters
various thermal pretreatment temperatures by using experimental data
with the help of three different kinetic models. Analyses for total solids (TS), volatile solids (VS) and total kjeldahl
nitrogen (TKN) of wheat straw before and after pretreatment were
2. Materials and methods carried out according to standard methods (APHA, 2005). Total organic
carbon (%TOC) was calculated by dividing the value of volatile solid
2.1. Inoculum and substrate content (%VS) with a factor of 1.8 (Adams et al., 1951). Biogas was
collected in gas collection bags and methane content in biogas was
Digested manure was used as an inoculum in the study. Fresh di- analyzed using gas analyzer (Biogas 5000, Geotech, UK).
gested manure, collected from local biogas plant, was sieved to obtain a Lignin, hemicellulose and cellulose contents in different wheat
uniform particle size of less than 2 mm and pre-incubated under straw samples were measured with the help of chemical method as
anaerobic conditions at 35 °C for 14 days to remove residual organic described in Li et al. (2004). The detail of the analysis is as follows.
matter. Wheat straw was used as a substrate and collected from local First, the amount of extractives in the biomass was determined by using
farmer near the study area. solvent extraction, for which, 60 mL acetone was used for 1 g of dried
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A.A. Rajput et al. Journal of Environmental Management 221 (2018) 45–52
Table 2 Rm . e
Initial characteristics of substrate and inoculum. M = Pb × exp ⎧ −exp ⎡ (λ − t ) + 1⎤ ⎫
⎨
⎩ ⎢
⎣ Pb ⎥
⎦⎬⎭ (2)
Parameter Digested Manure Wheat Straw Wheat Straw (Elsayed et al.,
2016) Transference function model that follow first order curve for re-
lating microbial community with biogas production (Redzwan and
pH 6.9 ± 0.11 5.9 ± 0.1 – Banks, 2004) was also used in the study as shown in Eq. (3)
TS % 6.8 ± 0.1 90 ± 0.25 90.82 ± 0.20
VS 70.7 ± 0.26 94.4 ± 0.23 95.64 ± 0.05 R . (t − λ ) ⎞ ⎫
TOC 41 ± 0.11 54.7 ± 0.11 47.62 ± 0.58 M = Pb ⎧1 − exp ⎛− m ⎜ ⎟
⎨
⎩ ⎝ Pb ⎠⎭⎬ (3)
TKN 4.2 ± 0.1 1.11 ± 0.11 0.30 ± 0.04
Logistic function model as shown in Eq. (4) was also used to predict
the kinetics of biogas production.
wheat straw sample at a constant temperature of 90 °C for 2 h. After
that biomass sample was oven dried at 105 °C until constant weight was Pb
M=
achieved. The weight difference before and after extraction gave the
amount of extractives. For determining hemicellulose content in dif-
1 + exp { 4 . Rm . (λ − t )
Pb
+2 } (4)
ferent wheat straw samples, 150 mL of sodium hydroxide (NaOH) so- where M is the biogas yield (NmL/gVS) with respect to time t (days), Pb
lution was added to 1 g of extractive-free dried biomass, which was kept is the maximum biogas potential (NmL/gVS), Rm is the maximum
at constant temperature of 80 °C for 3.5 h. After that the biomass sample biogas production rate (NmL/gVS/d), λ is lag phase (days) and e is a
was washed with deionized water until the value of pH approached 7. Euler's function equal to 2.7183.
The sample was then dried to constant weight. The weight difference
before and after the treatment gave the content of hemicellulose. Lignin 2.6. Statistical analysis
was determined by using 30 mL of 98% sulfuric acid for each gram of
extractive-free dried biomass sample. After that sample was kept at All the experiments and analyses were performed in triplicate and
ambient temperature for 24 h and then boiled at 100 °C for 1 h. The results were reported as average values. Analysis of variance (ANOVA)
mixture was then filtered, and residues were washed until the ions of was performed on results of biogas production and solids removal by
sulfate was detectable by titration of 10% solution of barium chloride. using SPSS 16 software at 5% level of significance to know the differ-
The sample was then dried until constant weight is achieved. The ences between the treatments. The kinetics fitting was performed in
weight difference before and after the treatment gave lignin content. SPSS 16.
Cellulose content was calculated by difference method as it was as-
sumed that extractives, lignin, hemicellulose and cellulose are the only 3. Results and discussion
components in biomass.
Fourier transform infrared (FTIR) spectrophotometer (Alpha pla- 3.1. Feedstock characteristics
tinum ATR, Bruker, Germany) was used to analyze the change in
functional groups before and after thermal pretreatment. The spectra Feedstock characteristics are very important parameters in design
were formed from 4000 to 500/cm with 32 times scanning. Essential and operation of an anaerobic digester. The initial characteristics of
FTIR and Origin Pro 6 software were used for the analysis. X-ray dif- feedstock strongly affect startup, process stability and biogas produc-
fraction (XRD) analyses of pretreated and untreated wheat straw were tion during anaerobic digestion. Initial pH of wheat straw was 5.9,
performed at an angle of 2θ, for the determination of crystallinity index while it was 6.9 for digested manure. Table 2 presents the character-
(C.I). For this purpose, Bruker D8 Advance diffractometer (Bruker, istics of pre-incubated digested manure and raw wheat straw and its
Germany) was used. The C.I was used to describe the crystallinity of comparison to the results of another study (Elsayed et al., 2016). Wheat
pretreated and untreated samples based on reflected intensity, com- straw had very high volatile solid (VS) content, i.e., 94.4% as compared
puted with the help of Eq. (1) described by Segal et al. (1959). to digested manure. The VS in the manure was low as it had already
undergone through the process of digestion. C/N ratios of individual
C . I (%) = (I002 − Iam)/ I002 × 100 (1)
substrates used in this study were either lesser or greater than that of
optimum range of C/N ratio for anaerobic digestion i.e., 20–30. C/N
where, I002 = Peak intensity at crystalline region; Iam = Peak intensity
ratio of wheat straw was 49, which was comparatively higher than that
at amorphous region.
of digested manure (9.76). Low C/N ratio of digested manure might
have adjusted the C/N ratio of wheat straw to optimum range without
addition of any external nutrients.
2.5. Kinetic study
Table 3
Comparison of chemical characteristics for untreated and pretreated wheat straw.
Conditions pH TS (%) VS (%) TOC (%) TKN (%)
Untreated 5.9 ± 0.1 90 ± 0.25 94.4 ± 0.23 54.7 ± 0.11 1.11 ± 0.11
120 °C 5.6 ± 0.23 91.4 ± 0.23 94.9 ± 0.1 55 ± 0.10 1.11 ± 0.01
140 °C 5.6 ± 0.1 92.1 ± 0.05 95.2 ± 0.17 55.2 ± 0.09 1.08 ± 0.01
160 °C 5.2 ± 0.11 94.1 ± 0.1 95.6 ± 0.34 55.4 ± 0.2 1.02 ± 0.01
180 °C 4.8 ± 0.26 96.8 ± 0.1 97.9 ± 0.2 56.7 ± 0.15 0.98 ± 0.02
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A.A. Rajput et al. Journal of Environmental Management 221 (2018) 45–52
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A.A. Rajput et al. Journal of Environmental Management 221 (2018) 45–52
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A.A. Rajput et al. Journal of Environmental Management 221 (2018) 45–52
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A.A. Rajput et al. Journal of Environmental Management 221 (2018) 45–52
Table 4
Kinetic parameters of different models for untreated and pretreated wheat straw.
Pretreatment condition Rm (mL/gVS-d) Pb (mL/gVS) λ (d) R2 Kinetic Model
Biogas production rate of pretreated wheat straw predicted by modified chemical, physical, biological and combination of all these should also
Gompertz model was higher as compared to untreated wheat straw as be assessed to get the best available pretreatment for treating lig-
shown in Table 4. Modified Gompertz model predicted shorter lag nocellulosic biomass to enhance biogas production and cost effective-
phase time of 3.37 days for wheat straw pretreated at 180 °C as com- ness. Energy balance and material balance in overall pretreatment and
pared to that of untreated wheat straw, which was 12.69 days. The anaerobic digestion of lignocellulosic materials should be studied.
coefficient of determination R2 values of modified Gompertz model for Moreover, the environmental issues caused using different pretreatment
biogas production data of the untreated and thermally pretreated wheat methods should also be thoroughly studied.
straw were in the range of 0.992–0.999. Veluchamy and Kalamdhad
(2017) used three different models on data of methane production from 4. Conclusion
thermally pretreated lignocellulose waste material to examine the effect
of F/M ratio. They found that modified Gompertz model was the one This study used thermal pretreatment to enhance the biogas pro-
with the best fit followed by logistic function and transference function duction of wheat straw. Significantly high biogas production and vo-
models, which is in line with the results of present study. Abudi et al. latile solids reduction was observed at thermal pretreatment tempera-
(2016b) also best predicted biogas production kinetics with modified ture of 180 °C as compared to untreated control. Considerable reduction
Gompertz model. in hemicellulose and lignin was observed due to thermal pretreatment
which also contributed to higher biogas production. Chemical bonds of
3.6. Practical application and future research direction wheat straw changed with thermal pretreatment. The modified
Gompertz model showed the best fit followed by logistic function
Huge quantity of agricultural biomass is produced annually in an model.
energy deficient country such as Pakistan, which can be used for pos-
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Features of promising technologies for pretreatment of lignocellulosic biomass.
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