Fuel 103 (2013) 10031009

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Biomethane production by anaerobic digestion of organic waste

A. Molino a,, F. Nanna a, Y. Ding b,, B. Bikson b, G. Braccio a
a
b

ENEA, National Agency for New Technologies, Energy and Sustainable Economic Development, UTTRI S.S. 106 Ionica, km 419+500, 75026 Matera, Italy
PoroGen Corporation, 6C Gill Street, Woburn, MA 01778, USA

h i g h l i g h t s
" Production of biomethane from biogas produced from anaerobic digestion of organic matter.
" Possibility to use biomethane in the grid injection.
" Use of polymeric membrane for biogas upgrading.
" Cleaning biogas.

a r t i c l e

i n f o

Article history:
Received 10 May 2012
Received in revised form 30 July 2012
Accepted 31 July 2012
Available online 23 August 2012
Keywords:
Biomethane
Anaerobic digestion
Biomass
Landll gas
Organic waste

a b s t r a c t
Anaerobic Digestion (AD) is a biological process that takes place naturally when bacteria break down
organic matter in environments with or without oxygen. Controlled anaerobic digestion of organic waste
in enclosed landll will generate methane. Almost any organic material can be processed with AD, including waste paper and cardboard (of a grade that is too low to recycle because of food contamination), grass
clippings, leftover food, industrial efuents, sewage and animal waste. AD produces biogas which is comprised of around 60% methane (CH4) and 40% carbon dioxide (CO2). This biogas can be used to generate
heat or electricity and/or can be used as a vehicular fuel. If the intended use is for power generation the
biogas must be scrubbed to remove a number of impurities. After conditioning the biogas can be used for
onsite power generation, to heat homes or can be added to the national natural gas grid. In recent years
several research groups have shown the possibility of upgrading the biogas for biomethane production
[1]. This study will show the feasibility of integrating anaerobic digestion plant with onsite polymeric
membrane purication system for conditioned biomethane production.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
The anaerobic digestion is the technology that can convert the
agro-industrial waste chain, the municipal solid waste and/or
wastewater sludge into renewable energy. There are multiple characteristics that make this technology applicable to industrial energy generation processes. Nevertheless, improvements in both
environmental characteristics and overall process economics are
still required to make the technology acceptable broad base. An
important economic consideration is the fact that the biogas can
be produced at the biomass production site reducing transportation costs. The AD plants can be scaled down that makes the process ideal for rural area development. The biogas can be used in
a cogeneration system or used for biomethane production which
in turn can be sent to national natural gas network or used as a
biocombustible fuel in the automotive sector.
Corresponding authors. Tel.: +39 (0)835 974736; fax: +39 (0)835 974210
(A. Molino).
E-mail address: antonio.molino@enea.it (A. Molino).
0016-2361/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.fuel.2012.07.070

The process of upgrading biogas realizes a carbon negative

chain because the biomethane substitutes the fossil natural gas
and the carbon dioxide can be captured and used in industrial
processes [1].
The objective of the paper is the feasibility of a biomethane production plant from anaerobic digestion of organic waste and the
upgrading of biogas with polymeric membrane.

2. The process
Anaerobic digestion is a natural biological process when bacteria break down organic matter in environments with little or no
oxygen. A controlled enclosed version of the anaerobic breakdown
of organic waste is a landll process which releases methane as
one of end products. Several research groups have shown that
the AD process can be split into three main stages: hydrolysis, acidogenesis and methanogenesis as show in Fig. 2.1 [2].
Anaerobic fermentation signicantly reduces the total mass of
waste, generates solid or liquid fertilizer and yields energy. It can

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A. Molino et al. / Fuel 103 (2013) 10031009

In the second stage, acetogenic bacteria, also known as acid

formers, convert the products of the rst phase to simple organic
acids, carbon dioxide and hydrogen.
The principal acids produced are acetic acid (CH3COOH), propionic acid (CH3CH2COOH), butyric acid (CH3CH2CH2COOH), and ethanol (C2H5OH). The products formed during acetogenesis are due
to a number of different microbes, e.g. syntrophobacter wolinii, a
propionate decomposer and sytrophomonos wolfei, a butyrate
decomposer. Other acid formers are clostridium spp., peptococcus
anerobus, lactobacillus, and actinomyces.
The acetogenesis reaction is shown below:
Fig. 2.1. Schematics of anaerobic digestion process.

be maintained at psychrophilic conditions (1216 C, e.g. in landlls, swamps or sediments), mesophilic conditions (3537 C, e.g.
in the rumen and in anaerobic digester) or thermophilic conditions
(5560 C; e.g. in anaerobic digesters or geothermally heated ecosystems). Disadvantages of the thermophilic anaerobic fermentation are the reduced process stability and reduced dewatering
properties of the fermented sludge and the requirement for large
amounts of energy for heating, whereas the thermal destruction
of pathogenic bacteria at elevated temperatures is considered a
big advantage [2]. The slightly higher rates of hydrolysis and fermentation under thermophilic conditions have not led to a higher
methane yield. No signicant change in the total methane yield
from the organic matter for fermentation temperatures ranging
from 30 C to 60 C have been reported [3,4].
In the rst stage of hydrolysis, or liquefaction, fermentative bacteria convert the insoluble complex organic matter, such as cellulose, into soluble molecules such as sugars, amino acids and fatty
acids. The complex polymeric matter is hydrolyzed to monomers,
e.g. cellulose to sugars or alcohols and proteins to peptides or amino acids, by hydrolytic enzymes, (lipases, proteases, cellulases,
amylases, etc.) secreted by microbes. The hydrolytic activity is of
a signicant importance in the high organic content waste and
may become rate limiting. Some industrial operations overcome
this limitation using chemical reagents to enhance the performance of the hydrolysis process. The application of chemicals to
enhance the rst step has been found to result in a shorter digestion time and it provides a higher methane yield [5].
2.1. Hydrolysis/liquefaction reactions
Lipids ? Fatty Acids
Polysaccharides ? Monosaccharides
Protein ? Amino Acids
Nucleic Acids ? Purines & Pyrimidines

C6 H12 O6 ! 2C2 H5 OH 2CO2

Finally, in the third stage the methane is produced by bacteria
called methane formers (also known as methanogens) in two
ways: either by means of cleavage of acetic acid molecules to
generate carbon dioxide and methane, or by reduction of carbon
dioxide with hydrogen. Methane production is higher from reduction of carbon dioxide but limited hydrogen concentration in
digesters that results in acetate reaction as the primary producer
of methane [6].
The methanogenic bacteria include methanobacterium, methanobacillus, methanococcus and methanosarcina. Methanogens can
also be divided into two groups: acetate and H2/CO2 consumers.
Methanosarcina spp. and methanothrix spp. (also, methanosaeta)
are considered to be important in AD both as acetate and H2/CO2
consumers. The methanogenesis reactions can be expressed as
follows:

CH3 COOH ! CH4

acetic acid

methane

CO2
carbon dioxide

2C2 H5 OH CO2 ! CH4 2CH3 COOH

ethanol

CO2

4H2
hydrogen

! CH4 2H2 O
water

The biogas products from the anaerobic digestion contain methane, carbon dioxide, hydrogen, hydrogen sulde, ammonia, siloxanes and other substances that may inhibit the anaerobic
digestion process or cause corrosion problems in pipelines of
plants or in the distribution network [79].
Several research groups have summarized technologies for biogas purication, in particular, for hydrogen sulde, ammonia and
siloxane removal [10]. At the end of the purication process the
biogas still contains hydrogen, carbon dioxide and trace of sulphidric acid and ammonia (<100 ppm) that must be removed from the
stream to produce biomethane.

Fig. 2.2. Process scheme for biogas upgrading.

A. Molino et al. / Fuel 103 (2013) 10031009

1005

BIOMETHANE

FEED BIOGAS

PERMEATE

Fig. 2.3. PEEK-SEP membrane for biogas upgrading.

A number of studies have shown the industrial feasibility of

upgrading biogas with polymeric membranes [11,12]. Membrane
technology was used to separate carbon dioxide from the biogas
in order to obtain biomethane of suitable quality for placing into
the national distribution network. Most of the literature related
to the use of polymeric membranes for carbon dioxide removal,
however, is directed to natural gas purication.
State of the art polymeric membranes are economically competitive in separating CO2 and H2S from the biogas as compared
to conventional technologies in both capital and operating costs
[13,14]. However, commercially available polymeric membranes
are typically susceptible to degradation by a number of biogas
components such as ammonia and thus require extensive feed
gas pre-treatment to protect membranes from degradation which
increases purication cost.
For several years ENEA Trisaia has been working on biogas production from various agro-industrial wastes or municipal solid
waste. Recently we have initiated a project for biogas upgrading
with polymeric membranes to increase caloric value of the gas
and to purify the gas to natural gas pipeline specications. ENEA
has selected membrane technology from PoroGen Corporation as
a main component of biogas upgrading system. PoroGens membrane technology was selected because of the superior membrane
chemical durability (membranes do not require specialized pretreatment to protect from aggressive biogas components that can
caused degradation of most commercial membrane systems), because of the compact membrane module size and high membrane
separation efciency. Initial process simulation has indicated that
to attain biogas product with methane concentration higher than
95% (by volume) combined with a high methane recovery it was
necessary to deploy a two stage membrane system as further described below. The schematic of the membrane separation system
is shown in Fig. 2.2. To generate driving force for membrane separation process the feed gas is compressed from the atmospheric
pressure to 31 barg.

The separation system is comprised of the feed biogas compressor to upgrade biogas pressure derived from anaerobic digestion
from atmospheric pressure to 31 barg; the compressed biogas is
stored in a rst tank to stabilize feed pressure and to regulate
the gas ow to rst stage membrane module. The stabilized feed
gas is directed into the rst membrane module that removes carbon dioxide, water vapor and some additional impurities (hydrogen, hydrogen sulde, oxygen, ammonia) by permeation and
generates the non-permeate (retentate) product biogas comprised
primarily of methane. The product gas is generated at the target
methane purity, it is dried and is collected at about 30 barg pressure. To increase methane recovery the permeate gas from the rst
stage membrane module is processed through a second stage
membrane system.
The rst membrane module splits the feed gas stream into two
gas streams, the biomethane product non-permeate gas stream
with methane content higher than 95% by volume collected at a
high pressure of about 30 barg and the permeate gas stream that
contains majority of carbon dioxide, water vapor and additional
impurities collected at a low pressure of 2 barg.
This one can be recirculated at the compression stage and after
this it can be fed at the second stage membrane. With this second
membrane module it is possible to recover additional product
stream with methane concentration greater than 85% and a second
stage permeate with a low methane content can be used as a fuel
as shown in Fig. 3.5. The permeate stream from the second stage
can be alternatively vented since it contains all impurities removed
from the biogas, i.e. most of carbon dioxide, water vapor, hydrogen,
ammonia, sulphidric acid, and some nitrogen.
Polymeric membrane modules utilized in the two stage process
were provided by PoroGen Corp., a US based company that specializes in industrial separation process. PEEK-SEP hollow ber
membranes composed of poly (ether ether ketone) polymer were
used. The membranes are designed to remove acid gases and water
vapors from raw natural gas or biogas to improve gas quality.

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A. Molino et al. / Fuel 103 (2013) 10031009

Table 3.1
Load to the anaerobic digester.

Fig. 2.4. Rendering of the upgrading plant.

The membrane modules used for biogas upgrading are shows in

Fig. 2.3.
Fig. 2.3 shows the polymeric membrane used in this upgrading
plant built by Porogen Corporation, that has a technology based on
melt extruded porous poly (ether ether ketone), PEEK, membranes.

PoroGen products are made from VICTREX PEEK high performance

polymers and are used in the most demanding separation applica
tions. The VICTREX PEEK polymer was chosen for its outstanding
combination of high heat and chemical resistance. Membrane pore
size and surface chemistry of each membrane product is tailored to
meet a specic separation application. For high precision separation composite membranes are manufactured by depositing an
additional ultra-thin separation layer on top of the porous PEEK
membrane. Composite membrane technology platform enables rapid commercialization of new applications by tailoring separation
layer material characteristics towards the target application.
PEEK-SEP membranes offer the best overall property prole of
any polymeric membrane on the market today-allowing it to perform in the most demanding environments. PEEK-SEP membranes can operate at temperatures as high as 200 C and are not
affected by aggressive chemicals present in real life process
streams. PoroGen membranes are inexpensive, yet sufciently
durable to be employed in industrial applications (high temperature gas separations, natural gas treatment, and aggressive solvent
ltration) under operating conditions in which other polymeric
membranes cannot be used.
The ENEAs biomethane plant was initially commissioned with
only one rst stage membrane module unit. The plant conguration is shown in Fig. 2.4.
The plant is automated and is controlled by a PLC system that
provides for data acquisition and valve control.

Days of load

Type of biomass

Volume
loaded (l)

Total volume
into reactor (l)

1
4
6
7
8
11
12
13
14
15
18
19
20
21
22
25
26
27
28
29
32
33
34

Pig manure
Pig manure
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables
Fruit and vegetables

200
200
16
16.5
22
22
22
24
25
26
27
28
29
30
31
32
33
34
36
38
40
42
45

200
400
416
432.5
454.5
476.5
498.5
522.5
547.5
573.5
600.5
628.5
657.5
398.5
718.5
750.5
783.5
817.5
853.5
891.5
931.5
973.5
1018.5

Fig. 3.2. Experimental results for DA. Methane concentration and biogas production vs days of experimental test.

3. Experimental results
The ENEA Trisaia research center operates anaerobic digestion
plant of plug ow technology type, PFR, with throughput of 70 kg

Fig. 3.3. Biomethane upgrading plant.

Upgrading Plant
Fig. 3.1. Anaerobic digestion plant.

Control room

Plug Flow Reactor for

Anaerobic Digestion

Fig. 3.4. Integrated AD plant coupled with polymeric membrane upgrading.

A. Molino et al. / Fuel 103 (2013) 10031009

1007

Fig. 3.5. Two congurations for biogas upgrading with polymeric membrane system.

Table 3.2
Wobbe index specications for town gas, natural gas and LPG.
Family

Type of gas

Wobbe index
range (MJ/Sm3)

Wobbe number
range from [13]

1
2L
2H
3

Town gas/syngas
Natural

22.530
3945
45.555
73.587.5

2429

LPG

4853
7287

Table 3.3
Gas specications for gas grid injection in Germany.
Parameter

Unit

Value

Wobbe index

MJ/Nm3

Relative density
Dust
Water dew point
CO2
O2
S

C
vol.%
vol.%
mg/Nm3

46.156.5 H
37.846.8 L
0.550.75
Technically free
<t2 (where t is the earth temperature)
<6
<3 (in dry distribution grids)
<30

per day. The plant has been in operation for several years. The plug
ow reactor is comprised of a stainless steel cylinder 70 cm in
diameter and 350 cm long with an internal volume of about of
1.3 m3; the reactor is inclined at a 20 angle and contains a
40 dm3 gasometer at the elevated section of the reactor. The AD
plant in show in Fig. 3.1.

The Anaerobic Digestion plant at ENEA Trisaia Research Centre,

Fig. 3.1, is arranged to enable material sampling from three different reactor zones. The reactor is heated to 3545 C under mesophilic conditions. The thermal heat is provided through electric
resistances distributed within the reactor in order to ensure in
greater load near the feed.
A number of different mixtures of fermentable organic substances were tested including animal waste and agroindustrial residue The composition of fermentable sources evaluated are shown
in Table 3.1.
The biogas produced was a gas mixture comprised mostly of
methane and carbon dioxide with additional gas components
hydrogen sulde, nitrogen, hydrogen, mercaptans and oxygen.
At regime the experimental results showed that the methane
contained in the biogas is in the range of 5060% by volume [15]
(see Fig. 3.2).
As can be seen, after the rst 5 days of operation, the concentration of methane reaches concentration of about 5560% by
volume. The rest of the biogas was composed by 4050 vol.%
in Carbon dioxide, 13 vol.% in nitrogen and the same for
Hydrogen.

4. Future developments
Recently the biogas production system was upgraded and the
reactor was coupled with membrane gas separation system. Initial
process simulation shows that the gas generated by the reactor

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A. Molino et al. / Fuel 103 (2013) 10031009

can be efciently processed by membrane system to generate

biomethane 96vol.%. The feed gas is compressed to 40 barg and
treated by membrane system to generate biomethane product
stream (retentate) at about 38 barg and permeate waste stream
at about 2 barg. The product biomethane is dry and essentially
hydrogen sulde free. The permeate contains carbon dioxide,
hydrogen sulde, water vapor, most hydrogen and some nitrogen
with balance methane. The biogas upgrading plant comprised of
bioreactor coupled with membrane separation system is shown
in Figs. 3.3 and 3.4.
As noted previously, process simulation has shown that to obtain a high product purity combined with a high methane recovery
it is necessary to deploy a two stage membrane system. In fact with
a single stage there is a methane content about of 28 vol.% For each
one double stage conguration was xed the purity in methane to
95% in volume.
Methane recovery utilizing two stage system will depend on the
specic system conguration. In this paper, two different conguration have been analyzed a two stage tandem design and a two
stage cascade design, as you shown in Fig. 3.5.
In the rst case, the biogas produced by AD is combined/mixed
with the retentate gas stream generated in the second stage membrane module, after an intermediate compression stage. With the
tandem conguration, xed the biogas in inlet to the upgrading
plant, the energy consumption is about of 0.32 kW/kg h of biomethane at 31 barg.
The two stage cascade design is composed by two membrane in
series with the recycling after compression of the permeate stream
in output at the second stage. For this conguration is necessary a
power consumption about of 0.14 kW/kg h of biomethane at the
same pressure to respect the previously conguration.
At the end you can see that the cascade conguration is more
competitive than the tandem conguration because the compression work of this one is greater than the cascade conguration.
Another conguration was simulated in order to verify the effect of the pressure on the tandem design.
Started from a biogas with a pressure about of 17 barg, the compression work was of 0.11 kW/kg h but, at the other hand, the
biomethane pressure was lower than the other congurations.
Fixed the biomethane purify and the mass ow rate in inlet to
the biogas upgrading plant, the pressure inuence on the outlet
pressure, compression work and methane content in the permeate
ow, infact in the low pressure cascade conguration the methane
content in the permeate ow is about of 24% in volume, higher
than the same conguration at high pressure that is 20% in volume.
In Fig. 3.5 are reported the different congurations for biomethane production fuelled by biogas.
The parameter typically used to determine the combustible
quality of the gas is the Wobbe index.
The Wobbe Index (WI) or Wobbe number is an indicator of the
interchangeability of fuel gases such as natural gas, liqueed petroleum gas (LPG), and town gas and is frequently dened in the specications of gas by customers and utilities.
If Vc is the higher heating value, or caloric value, and Gs is the
specic gravity, the Wobbe Index, Iw is dened as:

Iw V c =Gs 0:5
The Wobbe Index is used to compare the combustion energy
output of fuel gas of different quality for use in an appliance (re,
cooker, etc.). If two fuels have identical Wobbe Indices then for given pressure and valve settings the energy output will also be
identical. Typically variations of up to 5% are allowed as this would
not be noticeable to the consumer.
The Wobbe Index is a critical factor to minimize the impact of
the changeover when analyzing the use of substitute natural gas
(SNG) fuels such as propaneair mixtures.

There are three ranges or families of fuel gases that have been
internationally agreed upon based on the Wobbe index. Family 1
covers manufactured gases, family 2 covers natural gases (with
high and low ranges) and family 3 covers liqueed petroleum gas
(LPG). Combustion equipment is typically designed to burn a fuel
gas within a particular family: hydrogen-rich town gas, natural
gas or LPG.
The simulation results show that the biomethane produced by
cascade conguration has the Wobbe index in the range of 46
51 corresponding to the family 2H, i.e. similar to the natural gas.
It is thus possible to use this biomethane in the natural gas grid.
Currently there are no unied, European technical standards
which regulate the conditions for injecting biogas into the natural
gas grid [14].
The European Commission is currently working on developing
such standards and determining quality specications for the
biomethane (see Table 3.2). The regulations allows for injection
into natural gas grid of two types of biogas: Type H (High), a
gas having a high caloric value and type L (Low) having a
low heating value.
In some European Union countries, such as Germany, the quality specication for the biogas (biomethane) is based on natural
gas specications. Table 3.3 shows German biogas specications
for gas to be injected into gas grid.
As one can see the biomethane produced by AD process [16,17]
has the prerequisite quality for the gas grid injection, in fact the
only problem can be caused by the sulfur content in the biogas, because typically the sulphidric acid content in the biogas is 0.01
0.2% by volume depending on the organic matter processed. With
the POROGENs PEEK-Sep membrane is also possible to remove
H2S from the biomethane and obtain a product stream with suphidric acid content lower than 30 mg/Nm3.
5. Conclusions
Biomethane produced from biogas generated by anaerobic
digestion of organic matter is an alternative gas source to that of
the natural gas. The European Directive 2003/55 has authorized
connection to the natural gas grid. Of particular interest is the possibility to inject biomethane, rened biogas with quality comparable to that of natural gas (CH4 concentration greater than 95%),
which can be used in place of fossil fuels in all its network applications, and in transportation. To produce pipeline quality biomethane starting from the biogas generated by AD process it is
necessary to remove water, sulfur compounds, halogenated organic molecules, carbon dioxide, oxygen and metals.
Several research groups have shown that the biogas can be produced at about 810 cent per cubic meter of biogas, depending on
the organic matter source, with the methane content of 5560% (by
volume) while the upgrading cost is about of 78 cent considering
the cost of kWh of about 20 cent the total process cost is about
2022 cent for cubic meter of biomethane compressed to gas
grid at 30 bar. Italys market price of natural gas is xed by the
national authority for the electrical energy and gas use and is equal
to 40.09 cent/Nm3 referred to January 2010, will justify the
industrial feasibility of this process.
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