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Renewable Energy 36 (2011) 3313e3318

Contents lists available at ScienceDirect

Renewable Energy
journal homepage: www.elsevier.com/locate/renene

Evaluation of biogas production from different biomass wastes with/without

hydrothermal pretreatment
Wei Qiao a, b, *, Xiuyi Yan c, Junhui Ye c, Yifei Sun d, Wei Wang e, Zhongzhi Zhang a, b
a

College of Chemical Engineering, China University of Petroleum, Beijing 102249, China

State Key Laboratory of Heavy Oil Processing, China University of Petroleum, Beijing 102249,China
c
College of Geosciences, China University of Petroleum, Beijing 102249, China
d
School of Chemistry and Environment, Beihang University, Beijing 100191, China
e
School of Environment, Tsinghua University, Beijing 100084, China
b

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 3 February 2011
Accepted 7 May 2011
Available online 26 May 2011

Municipal biomass waste is regarded as new available energy source, although it could cause serious
environmental pollution. Generally, biogas recovery by anaerobic digestion was seen as an ideal way to
treat biomass waste. Different types of biomass waste have different biogas production potential. In this
paper, cow manure, pig manure, municipal sewage sludge, fruit/vegetable waste, and food waste were
chosen as typical municipal biomass waste. In addition, hydrothermal pretreatment was used to accelerate digestion and increase biogas production. Biochemical methane potential (BMP) test was used to
evaluate biogas production for raw biomass and hydrothermal treated waste. Raw materials of fruit/
vegetable and food waste show higher methane production than that of cow manure, pig manure, and
municipal sewage sludge. After hydrothermal pretreatment at typical condition (170
C at 1 h), the biogas
production of pig manure, cow manure, fruit/vegetable waste, and municipal sewage sludge increased by
7.8, 13.3, 18.5, and 67.8% respectively. While, for treated food waste, the biogas decrease by 3.4%. The
methane yield of pig manure, fruit/vegetable waste, and municipal sewage sludge increased by 14.6, 16.1,
and 65.8%, respectively. While, for treated cow manure and food waste, the methane decrease by 6.9%
and 7.5%.
2011 Elsevier Ltd. All rights reserved.

Keywords:
Biomass waste
Biogas production
Hydrothermal pretreatment

1. Introduction
Municipal sewage sludge, fruit/vegetable waste, and food waste
are typical municipal biomass waste. Municipal sewage sludge is
the by-product of the wastewater treatment process. In China, the
annual production of dewatered dry sludge cake reached 8.9
million tons in 2009 [1]. Fruit/vegetable waste includes refused
fruits and vegetables from the municipal terminal market. Generally, 20e50% of municipal solid waste come from fruit/vegetable
waste in cities. Annually, there were 100 million tons of fruit/
vegetable generated [2]. Food waste generated from households,
hotels, restaurants, and canteens of large enterprises and schools.
In China, annual food waste production reached 60 million tons [3].
Cow manure and pig manure produced in nearby cities are also
included in municipal biomass waste. Livestock manure comprises

* Corresponding author. China University of Petroleum, College of Chemical

Engineering, Beijing 102249, China.
E-mail address: qw04@mails.tsinghua.edu.cn (W. Qiao).
0960-1481/$ e see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.renene.2011.05.002

the highest share of the aforementioned biomass waste. In China,

annual livestock manure production is about 2.5e3.0 billion tons,
which surpass the total amount of industrial solid waste of 1.0
billion tons. Cow manure and pig manure account for a vast
majority of livestock waste (45.3 and 32.2%, respectively) [4]. For
biomass waste, there are different disposal routes for biomass
waste, while, anaerobic digestion plays an important role because
of its abilities to transform organic matter into biogas. The rural
biogas utilization of agricultural crops in china is regarded as
typical waste treatment for energy utilization. In this eld, many
studies have been conducted on biomass waste. Not only for sole
substrate but also co-digestions process have attracted much
attention. Callaghana [5] studied the co-digestions of cattle slurry
with fruit/vegetable waste and with chicken manure. Under mesophilic conditions, the retention time was kept at 21 days, and the
organic loading rate (OLR) was maintained at 3.19e5.01 kgVS/m3$d.
The possible use of potato tuber and its industrial by-products
(potato stillage and potato peels) on farm scale co-digestion with
pig manure was evaluated in a laboratory experiment [6]. The
results show that a successful digester operation can be achieved

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W. Qiao et al. / Renewable Energy 36 (2011) 3313e3318

with feed containing potato material up to 15e20% of the feed

versus co-digestion of organic fraction of municipal solid waste
with manure under thermophilic wet digestion systems. This
results in a hydraulic retention time (HRT) of 14e18 days and an
OLR of 3.3e4.0 kgVS/m3$d [7]. Adapting the co-digestion process to
an organic fraction of municipal solid waste (OFMSW) manure ratio
of 50% (VS/VS) was established over six weeks. The two-phase
digestion consisted of of co-digestion of dairy cow manure,
OFMSW, and cotton gin waste [8]. The thermophilic digestion
performance of garbage, swine manure, dairy cattle manure, and
mixtures of waste show that swine and dairy cattle manure have
lower volatile solid (VS) removal and methane yields than garbage
[9]. The organic removal rate of swine manure signicantly
increased when it was digested with garbage. For food waste, the
methane production of korean food waste was evaluated using the
batch biochemical methane potentials (BMP) test [10].
Methane production from biomass waste has attracting more
and more interest. While, the conventional digestion process
directly accepting raw waste using continuous stirred tank reactor
needs a long HRT and has a low VS removal rate. So, usually the
digestion of biomass waste could not give satised results. Appels
provide a detailed and comprehensive review of sludge anaerobic
digestion. The researcher point out that hydrolysis is recognised as
rate-limiting step in the complex anaerobic digestion process [11].
Under this principle, pretreatment was necessary to lysis sludge
cell to release organic materials from inside bacterial. The
pretreatments including ultrasonic [12,13], ozone [14], chemical
oxidation [15], alkaline treatment [16] and acid treatment [17]
could be used as methods to improve the rate-limiting hydrolysis.
Among these methods, hydrothermal process has been used in
municipal sewage sludge digestion in industrial operation. With
hydrothermal pretreatment, municipal sewage sludge was dissolved into a liquid phase that skips the slow biological enzyme
hydrolysis. In 1968, Brooks [18] started hydrothermal process
research, and then other processes have subsequently been
developed. In1995, the Cambi thermal hydrolysis process promoted
the technology to industrial application. According to Cambi website, the hydrothermal process has been chosen to treat sluge of
UKs largest wastewater treatment works. In China, to give alternative way for serious municipal sewage sluge treatment and
disposal, hydrothermal pretreatment has also been developed. The
rst hydrothermal pilot plant was built in 2002 [19]. In 2008,
another hydrothermal equipment was built in a municipal wastewater treatment plant [20]. In these two units, hydrothermal
process was used to get dry municipal sewage sludge cake. At the
beginning of hydrothermal technology development, researchers
used high temperature and pressure to remove water from sludge
even to oxidate organics. To achieve those goals, Porteous process,
Zimpro and Low pressure oxidation process was developed [21].
At 1978, Huang use hydrothermal process to improve sluge digestion biogas production. His result show that heating sluge at 175
C
could increase biogas production by 60e70% [22]. Li and Noikeal
evalutated hydrothermal effect at different temperature and heating time [23]. With the industrial application, as a mothod for
improve sludge digestion performance, hydrothermal pretreatment was recognized.
Although biomass waste is seen as new available energy, there has
not direct test of different materials for biogas production potential.
In addition, there was not evaluation of hydrothermal effect for
different biomass waste. So, it was necessary to assess energy
recovery rate with/without hydrothermal pretreatment. In this
paper, to investigate the biogas and methane production with/
without hydrothermal pretreatment, cow manure, pig manure,
municipal sewage sludge, fruit/vegetable waste, and food waste were
chosen to be tested using the biochemical methane potential test.

2. Materials and methods

2.1. Materials
Typical biomass waste used in the experiments includes cow
manure, pig manure, municipal sewage sludge, fruit/vegetable
waste, and food waste. Cow manure and pig manure were collected
from two breed plants in a suburban district in Beijing city. Municipal sewage sludge was sampled from the Beixiaohe municipal
wastewater treatment plant. This plant treated 10  104 cubic
meters of wastewater per day from households. In this plant, two
biological A/O process and membrane bioreactor were used. Fruit/
vegetable waste was taken from a farmers market in Beijing city,
where fruit/vegetable waste was centralized collected. Food waste
was collected from the student canteen in Tsinghua university. The
sampled food waste was a mixture of lunch and supper residues.
2.2. Methods
For cow manure, pig manure, and sludge, these three materials
were diluted by adding equivalent tap water before heating. Fruit/
vegetable waste was crushed before hydrothermal heating. The
collected food waste was rstly screened to remove bones, plastic
and metals and then crushed before heating. The procedure of BMP
test for different biomass wastes was shown in Fig. 1. Hydrothermal
treatment was carried out in 8 stainless kettles. Those reactors were
heated by oil batch. Volume of the reaction kettle was 1 L. The
parameters for hydrothermal treatment were 170
C for 1 h according to reported literature [24]. When the oil bath reached 170
C,
the kettles were put in it for 1 h, including 0.5 h for temperature
rising and 0.5 h for stable heating. After hydrothermal treatment,
the reaction kettles were taken out and put into the cool water
bath.
The soluble COD was determined by the potassium dichromate/
ferrous ammonium sulphate method by a detector (ET3150B). Total
organic carbon (TOC) was measured by TOC5000 (Shimadzu).
Volatile fatty acids (VFAs) were measured by a gas chromatography
with a FID detector (Shimadzu 2010). NH4-N, total nitrogen (TN),
PO43-P and total phosphorus (TP) were measured according to
national standard [25]. The pH was determined by a Mettler-toledo
pH detector (FE20). Gas ow meter (BSD 0.5) was used to record
biogas amount.

Fig. 1. Procedure of BMP test for different biomass wastes.

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W. Qiao et al. / Renewable Energy 36 (2011) 3313e3318

3315

Table 1
Characteristics of raw materials.

Cow manure
Pig manure
Sludge
Fruit/vegetable waste
Food waste

pH

TS
(%)

VS
(%)

VS/TS
(%)

TN
(g/Kg)

TP
(g/Kg)

Fibers
(%TS)

Lipids
(%TS)

Proteins
(%TS)

8.57
6.91
7.15
4.06
4.41

34.66
28.14
14.58
9.15
19.71

19.52
22.26
10.63
7.72
17.04

56.32
79.10
72.91
84.37
86.45

23.80
42.77
51.27
36.50
35.15

4.63
25.24
17.23
4.97
3.94

18.7
14.2
21.5
35.2
20.2

0.6
5.2
14.4
12.9
29.9

12.3
17.9
20.0
15.2
17.3

According to Heo research, a 250 mL serum bottles with

temperature of 37  1
C were used as BMP reactor, which contained the well adapted seed inoculums from the pilot scale
digestion reactor [26]. All assays were shaken two times per day
and the volume of gas produced was recorded every day. To
compare the performance of all materials, the samples added into
the BMP reactors had the same amount of 1 g VS for solid all
biomass wastes. While for centrifuged liquid materials from
hydrothermal treated samples, the adding volume was controled
with containing 1.5 g COD. To insure the accuracy of the experiments, duplicates were run for all samples with/without hydrothermal treatment.
3. Results and discussion
3.1. Characteristics of raw biomass waste
The composition of waste determine biogas yield and gas
quality. The order of biogas volume produced by degradation per
unit of organic matter is as follows: lipids > carbohydrates >
proteins, the order for methane production is as follows:
lipids > proteins > carbohydrates. The composition of the reaction
samples was different; thus, biogas and methane production could
be predicted according to different compositions. TS and SS present
the solid content of biomass waste. The VS comprise biodegradable
volatile solids fraction and refractory volatile solids [27]. Biodegradable volatile solids include saccharine, starch, organic acids,
cellulose, lipids, and proteins. Refractory volatile solids are
composed of lignin and other non-biodegradable substances.
Usually, the VS to TS rate is seen as organic content. Table 1 shows
that pig manure, fruit/vegetable waste, and food waste have
organic content as high as 80%. This value is higher than municipal
sewage sludge.
3.2. Characteristics of hydrothermal treated biomass waste
For hydrothermal pretreatment, with organic matters dissolving
and hydrolyzing, parts of solid organic matters are liqueed as
a form of low molecular weight organic matter; thus, the COD in
supernatants increased. Table 2 gives the characteristics of hydrothermal treated materials. Concentrations of COD increased by 11.9
and 25.9% for fruit/vegetable waste and food waste, respectively.

Under the hydrothermal reaction, biomass waste would release

organic carbon into the liquid phase. TOC in the supernatant in the
fruit/vegetable waste and food waste increased after treatment,
especially for food waste, in which it increased from 45.72 to
59.08 g/L. The TN in the supernatants is relatively high. Parts of
nitrogen were released during heating after comparing the results
of the fruit/vegetable and food waste. The hydrothermal treatment
disrupt the cells, thus phosphorus will be released from the
biomass waste. In this research, the total phosphorus in the
supernatants of treated fruit/vegetable waste and food waste was
relatively low.
Massive VFAs, amino acids, and ammonia nitrogen, which could
signicantly affect pH, are generated during heating. The pH of
treated materials tend to decrease for almost biomass waste,
especially for cow manure and municipal sewage sludge, which
change from alkaline to acid substrate after hydrothermal treatment. High concentration of VFAs can inhibit the activity of the
methanogenic bacteria. Vieitez [27] pointed out that anaerobic
digestion would stop when the concentration of VFAs exceeds
13,000 mg/L. The 1.0 g of acetic acid, propionic acid, butyric acid,
and valeric acid were equivalent to 1.07, 1.51, 1.82, and 2.04 g COD,
respectively. VFAs account for 41, 62, 42, 37, and 13% of total COD in
the supernatant of treated cow manure, pig manure, municipal
sewage sludge, fruit/vegetable waste, and food waste, respectively,
after we converted the VFAs into COD. The percentages of VFAs/
COD are relatively high except for food waste.

3.3. Methane production potential of biomass waste

3.3.1. Biogas production potential of cow manure
The BMP test of raw and treated cow manure show that after
170
C/1 h hydrothermal pretreatment, the cumulative biogas
production increase from 210 to 238 mL/g VS. After 14 days
anaerobic digestion, the biogas volume curve become smooth
indicating that the biodegradable parts of the organic matter had
already been digested. The daily biogas production show that peak
biogas production occurred on the rst day for all samples of cow
manure, at 130 mL for the treated supernatant, 45 mL for the
treated sample, and 25 mL for the raw sample. Methane production
is calculated after the biogas composition determined; the ultimate
methane productions for treated supernatant, treated sample, and
raw sample were 262.1 mL/1.5 g COD, 130.2 mL/g VS, and 139.8 mL/

Table 2
Characteristics of supernatant of treated biomass wastes.

Treated cow manure

Treated pig manure
Treated sludge
Raw fruit/vegetable
Treated fruit/vegetable waste
Raw food waste
Treated food waste

pH

VFA (g/L)

COD (g/L)

TOC (g/L)

TN (g/L)

TP (g/L)

C:N:P

6.81
6.46
6.47
4.06
4.17
4.41
4.30

10.93
23.51
8.34
6.77
13.34
7.66
13.36

30.0
43.8
30.0
e
48.6
e
134.0

11.69
18.88
9.27
13.41
13.74
45.72
59.08

1.62
3.82
1.74
1.69
1.77
1.48
3.08

0.212
0.522
0.219
0.307
0.249
0.783
0.537

63.8:7.6:1
39.9:7.3:1
48.6:7.9:1
47.9:5.5:1
60.8:7.1:1
63.6:1.9:1
112.3:5.7:1

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W. Qiao et al. / Renewable Energy 36 (2011) 3313e3318

400

600

350

500

Biogas production(mL/g-VS)

Biogas production(mL/g-VS)

3316

300
250
200
150
100

1gVS raw cow manure

1gVS treated cow manure
1.5g COD supernatant

50
0

10

12

400
300
200
100
0

14

1gVS raw sludge

1gVS treated sludge
1.5gCOD supernatant

10

12

14

16

Time(d)

16

Fig. 4. Cumulative biogas production of municipal sludge.

Time( d)
Fig. 2. Cumulative biogas production of raw cow manure.

g VS, respectively. The methane yield did not increase after

hydrothermal pretreatment, but decreased by 6.9%. The proteins in
the cow manure are lowest among the biomass waste. Biogas
production of cow manure is shown in Fig. 2.
3.3.2. Biogas production potential of pig manure
The ultimate biogas productions were 385 mL/g VS, 415 mL/g
VS, and 556 mL/1.5 g COD for the raw sample, treated sample, and
supernatant, respectively. The biogas production of pig manure
increased by 7.8% through the hydrothermal reaction. After
analyzing the composition of the produced biogas, the methane
yields were calculated. The methane productions of pig manure
increased by 14.6% from 253.8 to 290.8 mL/g VS after the hydrothermal treatment. The supernatant had the highest methane yield
at 391 mL/1.5 g COD. The digestion degree of the tested samples
was relatively high compared with that of cow manure. This can be
explained by the higher contents of lipids and proteins in pig
manure. Biogas production of pig manure is shown in Fig. 3.
3.3.3. Biogas production potential of municipal sewage sludge
The differences of ultimate biogas amount among the three
municipal sewage sludge samples are great, demonstrating that
hydrothermal treatment greatly affect municipal sewage sludge.
This can be related to the cell structure of the municipal sewage
sludge, cells disrupted by the heating process, and massive soluble
organic matters released, causing higher biogas production for the

Biogas production(mL/g-VS)

700

400
300
200

1gVS raw fruit/vegetable waste

1gVS treated fruit/vegetable waste
1.5gCOD supernatant

100
0

10

12

14

16

Time(d)
Fig. 5. Cumulative biogas production fruit/vegetable waste.

treated rather than the raw sample. Ultimate biogas increase by

67.8% from 202 to 339 mL/g VS. Peak biogas productions ended on
the rst three days for all samples. The highest daily biogas
productions takk place on the rst day, at 175 mL for the supernatant, 137 mL for the treated sample, and 32 mL for the raw
sample. Methane contents are detected, and an increase of 65.5% in
the methane production from 155.5 to 257.3 mL/g VS are observed
after the municipal sewage sludge heating. The lipid and protein
contents are relatively high compared with the other materials.
Biogas production of municipal sewage sludge is shown in Fig. 4.

900

500

Biogas production(mL/g-VS)

Biogas production(mL/g-VS)

500

600

400
300
200
1gVS Raw pig manure
1gVS Treated pig manure
1.5gCOD Supernatant

100
0

600

10

12

14

Time( d)
Fig. 3. Cumulative biogas production of pig manure.

16

750
600
450
300

1gVS raw food waste

1gVS treated food waste
1.5gCOD supernatant

150
0

10

12

14

Time(d)
Fig. 6. Cumulative biogas production of food waste.

16

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W. Qiao et al. / Renewable Energy 36 (2011) 3313e3318

3317

Table 3
Biogas and methane production of biomass waste.
Raw materials

Cow manure
Pig manure
Sludge
Fruit/vegetable waste
Food waste

Hydrothermal treated materials

Supernatant of hydrothermal treated materials

Biogas
(mL/geVS)

Methane
content (%)

Methane
(mL/geVS)

Biogas
(mL/geVS)

Methane
content (%)

Methane
(mL/geVS)

Biogas
(mL/1.5g-COD)

Methane
content (%)

Methane
(mL/1.5g-COD)

182.0
385.0
202.0
443.0
781.0

66.6
65.9
76.9
63.4
68.0

139.8
253.8
155.5
280.9
531.3

238.0
420.0
339.0
525.0
754.0

54.7
70.1
75.9
62.1
65.1

130.2
290.8
257.3
326.0
491.1

350.0
556.0
554.0
675.0
723.0

74.6
70.4
69.5
66.6
65.9

261.1
391.2
384.9
449.7
476.1

3.3.4. Biogas production potential of fruit/vegetable waste

The BMP test of fruit/vegetable waste show that cumulative biogas
production increased by 18.5% from 443 to 525 mL/g VS for raw waste
after the hydrothermal treatment. The biogas volume did not change
in the last few days, indicating that the biodegradable parts of fruit/
vegetable waste had been digested thoroughly. The peak biogas
productions of raw sample, treated sample, and supernatant ended at
the same time. A small amount of biogas was generated during the
last days, revealing that hydrothermal treatment had little impact on
digestion time. The daily biogas productions showed that the highest
biogas productions occurred on the rst day and there was little
difference with the three tested samples, at 205 mL for the supernatant, 200 mL for the treated sample, and 175 mL for the raw sample.
The methane contents were determined, and the results showed that
methane production increased by 16.1% from 280.9 to 326.0 mL/g VS
after fruit/vegetable waste was heated. Methane production was
449.7 mL/1.5 g COD for the supernatant. The methane yields
accounted for 48.8, 56.6, and 85.7% of the theoretical values for the
raw sample, treated sample, and supernatant, respectively. The lipid
and protein contents of fruit/vegetable waste were at a medium level,
and the content of crude bers was highest among all tested materials. The biodegradable volatile solids were higher than the refractory volatile solids in crude bers. Biogas production of fruit/
vegetable waste is shown in Fig. 5.
3.3.5. Biogas production potential of food waste
Ultimate biogas production decrease by 3.5% from 781 to
754 mL/g VS for food waste after hydrothermal treatment. The
methane production of three tested samples are completed in the
rst two days, indicating that hydrothermal treatment had little
impact on digestion time. The biogas productions of food waste are
different from the other materials. The biogas production of the
supernatant have the lowest value of 723 mL/g VS, with 754 mL/g
VS for the treated sample and 781 mL/g VS for the raw sample,
indicating that the barrier effect occurred on the anaerobic digestion of food waste by hydrothermal treatment. The peak biogas
productions take place in the rst two days. The highest daily
biogas productions are on the rst day, at 275 mL for the raw
sample and 250 mL for the treated sample and the supernatant.
After the second day, biogas production increase slightly. The
methane content in biogas are analyzed and the ultimate methane
productions are 531.3 mL/g VS for the raw sample, 491.1 mL/g VS for
the treated sample, and 471.6 mL/1.5 g COD for the supernatant,
which accounted for 78.8, 72.9, and 89.8% of the theoretical values,
respectively. The digestion degree of the three tested samples is
high, but the efciency of the anaerobic digestion did not improve
with the hydrothermal treatment; methane production decreased
by 6.9% after treatment. The high methane yields of food waste can
be closely integrated with its composition; lipid and protein
contents are very high, and lipid content was 2e50 times higher
than that of the other materials. Biogas production of food waste is
shown in Fig. 6. Table 3 compares the biogas and methane
production amounts for raw and hydrothermal heated materials.

4. Conclusions
For different waste, the composition determine the biogas
production. As tested in this paper, for per gram VS of raw biomass
waste, the order of biogas produciton potential are as follows: food
waste > fruit/vegetable waste > pig manure > municipal sewage
sludge > cow manure. With hydrothermal heating, organic dissolving into liquid phase increased the COD, VFA and TOC
concentration. That improve the biodegradation of biomass waste.
For per gram VS of hydrothermal heated biomass waste, the order
of methane production is same as the raw materials. The amount of
methane productions of treated pig manure, fruit/vegetable waste,
and municipal sewage sludge increased by 14.6, 16.1, and 65.5%,
respectively. Municipal sewage sluge give the highest increasing
rate.On the contrary, after heated treatment, the methane
production of food waste and cow manre decreased.

Acknowledgement
This work was supported by the following grant: National High
Technology Research and Development Program of China (863
program) (No. 2008AA062401; No. 2009AA064701), Major Project
on Control and Rectication of Water Body Pollution (No.
2008ZX07313-004), and Beijing Municipal Natural Science Foundation (No. 8102024).

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