Available online at www.sciencedirect.
com
Hydrothermal conversion of biomass to fuels and
energetic materials
Andrea Kruse1,4, Axel Funke2 and Maria-Magdalena Titirici3
Available biomass, preferentially residues, can be divided in
two groups: biomass with a high or natural water content (‘wet’
or ‘green’ biomass) and biomass with low water content such
as wood and straw. In ‘dry’ biomass gasification processes,
originating in most coal processing technologies, biomass of
low water content is necessary to avoid the energy loss by
water evaporation. In contrast, hydrothermal processes need
water as reaction medium; therefore, these processes are
preferentially used for wet or ‘green’ biomass.In this review
paper we will describe the main research directions in the
hydrothermal conversion of biomass into fuels and carbon
throughout gasification to produce H2 or CH4, liquefaction to
produce crude oils and phenols from lignin as well as
carbonization to produce carbonaceous materials which can
be either used as fuels (carbon negative chars) or interesting
energetic materials (hydrothermal carbons).
Addresses
1
Kahrlsruhe Institute of Technology, Karlsruhe, Germany
2
Leibniz-Institut für Agrartechnik Potsdam, Germany
3
Queen Mary University of London, School of Materials Science and
Engineering, London, UK
4
University of Hohenheim, Stuttgart, Germany
Corresponding author: Titirici, Maria-Magdalena
(m.m.titirici@qmul.ac.uk)
Current Opinion in Chemical Biology 2013, 17:515–521
This review comes from a themed issue on Energy
Edited by Michael D Burkart and Stephen P Mayfield
For a complete overview see the Issue and the Editorial
Available online 23rd May 2013
1367-5931/$ – see front matter, # 2013 Elsevier Ltd. All rights
reserved.
http://dx.doi.org/10.1016/j.cbpa.2013.05.004
Introduction
Dry thermochemical conversion processes have been
used by mankind since centuries and recent develop-
ments increased the quality of these processes to make
them available for the urgent required shift from fossil to
renewable resources. They are readily applicable to pro-
duce high quality gaseous, liquid, and solid fuels. How-
ever, dry conversion processes can only work with high
efficiency when dry feedstock is used, which in general
represents a fuel with a comparable good quality. In order
to increase the energetic use of moist biomass, which is
often regarded as waste biomass because it is difficult to
be processed with good efficiency, hydrothermal pro-
cesses are investigated. These processes are capable of
www.sciencedirect.com
producing high quality fuels and materials with different
characteristics than their dry counterparts.
Hydrothermal processes take place in liquid water at
elevated temperatures, that is, the pressure in the system
must be at or above saturated pressure. They can be
classified by different regions above the vapor–pressure
curve and the critical point in the phase diagram of water
(see Figure 1). Hydrothermal gasification dominates at
high temperatures in near and supercritical conditions
whereas carbonization takes place at comparably mild
temperatures. Under subcritical hydrothermal conditions,
increasing temperature always means an increasing pres-
sure due to the conditions set by the vapor–pressure
curve. In contrast to hydrothermal processes, steam
assisted pyrolysis is represented by different conditions
below the vapor–pressure curve, that is, the state of
aggregation of water is dry steam.
Chemistry of hydrothermal processes
The dramatic change of the properties of water at elev-
ated temperatures, even in the subcritical region, is well
known. Water becomes an excellent reaction environ-
ment, reactant and solvent for a diverse range of reactions,
for example, the increasing ion product in subcritical
conditions favors reactions that are typically catalyzed
by acids or bases. The initial reaction taking place when
biomass is heated up in water is the hydrolysis of cellulose
to glucose, which is the decisive difference to dry thermo-
chemical conversion [2] (see Figure 2). The hydrolysis
gives way to homogeneous reactions in an aqueous
solution, which are not limited by heat and mass transfer.
Same holds true for the destruction of lignin to its main
product phenol. Further dehydration of glucose to a wide
range of potentially interesting substances has been the
topic of many excellent reviews and will not be discussed
in detail here. Some key substances are indicated in
Figure 2 as representatives. This mixture of organic acids,
different ketones, and phenols represents the liquid
product ‘biocrude’ from hydrothermal liquefaction. As
free radical reactions become more important toward
the critical point of water, gasification for the production
of hydrogen and methane is favored:
C6 H12 O6 þ 6H2 O ! 6CO2 þ 14H2 (1)
C6 H12 O6 ! 3CH4 þ 3CO2 (2)
The formation of hydrogen is endothermic and that of
methane slightly exothermic [3]. Therefore, hydrogen for-
mation predominates over methane formation at high tem-
peratures according to the LE CHATELIER principle.
Current Opinion in Chemical Biology 2013, 17:515–521
516 Energy

Figure 1 In order to produce a solid product, reaction temperature

must be limited in order to avoid gasification and lique-
35 faction (see Figure 1). Important insights have been
gained in the past years about the formation process of
30 H2
CH4 HTC coal. The dehydration of glucose to 2,5-hydroxy-
25 methylfurfuraldehyde (HMF) and subsequent aldol con-
densation/addition has been promoted and supported by
20 further evidence as a model to describe this formation
p / MPa

process, which is characterized by carbon spheres

15
"Oil" [4,5,6]. Investigations with the aim to produce sym-
10 metric compounds for the use as monomers in sustainable
Chemicals polymers concentrate on the chemistry of HMF, mainly
5 reactions on the hydroxymethyl group (esterification,
H2
0
etherification and oxidation) and the formyl group
C (reduction, oxidation, aldol reactions and aldol-like reac-
100 200 300 400 500 600 700 tions) [7]. Additionally, solid–solid formation mechanisms
ϑ / °C similar to torrefaction have to be considered for the
Current Opinion in Chemical Biology conversion of biomass because it is not completely solved
at low temperatures [8]. The existence of two major
Schematic overview concerning different biomass conversion processes reaction pathways via liquid state to form ‘coke’ and solid
and their typical temperature and pressure ranges. In addition, the state to form ‘char’ [4] has been supported by detailed
vapor–pressure curve of water is shown. investigations of the chemical composition of HTC coal
Taken from [1].
[9] (see Figure 2).

Figure 2

Hemicellulose Cellulose Lignin

Hydrolysis

Pentoses Hexoses Polysaccharides

Dehydration
Catechol/
Phenols Solid-solid reactions
Furfurals Organic acids

Aromatization Decarboxylation

Benzene

H2O Liquid fragments of biomacromolecules CO2

‘biocrude’

Polymerization Reforming Hydrogenation

Fraction i H2 Producer gas CH4

Reaction
HTC-coal ...
(By-) product Fraction n
Current Opinion in Chemical Biology

Principle reaction pathways of hydrothermal carbonization.

Adapted from A Funke, PhD thesis, Technische Universität Berlin, 2012.

Current Opinion in Chemical Biology 2013, 17:515–521 www.sciencedirect.com

 Hydrothermal conversion of biomass to fuels and carbon Kruse, Funke and Titirici 517
All these reactions are contributing to the final formation
of the HTC structure, that is, HTC coal is a generic term
for different product fractions. A detailed analysis of
hydrothermal carbons with a combination of FT-IR,
XRD, Raman, Electron Microscopy, TG-IR and N2
adsorption indicates a material with polar oxygenated
functionalities coexisting with an aromatic amorphous
type of carbon structure [10]. Thus HTC is able to
produce a product which is not available by a dry
process.
Hydrothermal gasification
As indicated in Figure 1, hydrothermal gasification of
biomass is characterized by different reaction con-
ditions and typically divided into three main types.
All of them represent one-pot conversion processes
for the production of methane or hydrogen, which
is not possible to achieve with dry thermochemical
conversion.
1. Aqueous phase reforming (APR) [3,11,12] of degra-
dation products from carbohydrates (glucose, sorbitol,
glycerol, methanol, glycol) at around 215 to 2658C to
mainly hydrogen and carbon dioxide: APR only works
at low concentrations and in the presence of a
heterogeneous catalyst (Pt, Ni, Ru, Rh, Pd, Ir). As
such, it is not technically feasible unless the hydrogen
is used in situ for the hydrogenation of biomass-derived
organic compounds. By this process, termed ‘hydro-
genolysis’, platform chemicals and biofuels can be
produced [13].
2. Near-critical catalytical gasification of biomass or its
degradation products to mainly methane and carbon
dioxide at around 350–4008C [14]: typically, a
heterogeneous catalyst for the hydrogenation of carbon
monoxide to methane is necessary.
3. Supercritical water gasification (SCWG) of biomass or
its degradation products to mainly hydrogen and
carbon dioxide at around 600–7008C. Heterogeneous
catalysts (e.g. Ni, Pt and Cu base catalysts [15]) are
used; however, SCWG can also be performed without
the addition of a catalyst [12].
In addition to the catalysts added to the reactor, catalytic
effects of salts contained in the biomass, especially
alkali salts, are important. It has been observed that
they catalyze the water–gas shift reaction to form hydro-
gen but the detailed mechanisms are not known yet
[16]. In turn, salts have been recognized to be a chal-
lenge in the reactor system because they have a low
solubility in the supercritical range and plugging may
occur [17,18]. Therefore, the use of a cyclone or other
separations techniques is necessary [19]. It is pointed
out that the different hydrothermal gasification pro-
cesses have been demonstrated also in large scale and
the current trend is investigating more complex process
designs [20].
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Hydrothermal liquefaction
Hydrothermal liquefaction of biomass at 300–3508C and
15–20 MPa is a well-known process for the production of a
liquid ‘biocrude’, which in turn can be used for the
production of biofuels. Products of this process are two
liquid phases (biocrude and an aqueous solution with
dissolved organics) and a gas phase mainly consisting
of carbon dioxide. The oil produced by hydrothermal
liquefaction is similar to its counterpart in dry thermo-
chemical conversion ‘flash pyrolysis’. However, oil from
hydrothermal liquefaction is dominated by phenols and
exhibits a lower content of polar compounds like acids
and sugars [14] (see Figure 2). It should be noted that no
significant char/coke formation is observed during hydro-
thermal liquefaction in contrast to flash pyrolysis. The
most current published studies are focused on increasing
the oil yield by decreasing the amount of organics dis-
solved in the aqueous solution. Typically, alkali hydrox-
ides, hydrogen carbonates, and carbonates are used as
catalysts (Figure 3) [21,22,23].
A particular application of hydrothermal liquefaction is
the splitting of lignin, which is a waste material from the
paper industry known as ‘black liquor’, at temperatures
around 4008C under hydrothermal conditions. Reaction
kinetic studies have been performed both based on lignin
and lignin derived model compounds, that is, guaiacol
[24]. Lignin depolymerization was also studied in super-
critical water, both as bulk component and model phe-
nolic compounds [25]. A formal kinetic model of lignin
degradation in ethanol/formic acid [26] could be adjusted
for the use under hydrothermal conditions [27].
Hydrothermal carbonization
At comparably low temperatures ranging from 160 to
2508C [5], liquefaction and gasification can be limited
in order to increase the yield of a solid material termed
HTC coal [28,29]. This hydrothermal carbonization pro-
cess can be used to convert a variety of feedstock to a solid
fuel with a carbon content similar to lignite at mass yields
from 35 to 60% [4,30,31–35]. The highest carbon losses
are due to dissolved organics in the aqueous phase and
only a minor amount of gas is produced [4,30,33,36].
The product distribution is primarily dependent on the
feedstock and process temperature [5,28,30,33], but
there is also an influence of the reaction time and the
solids load [32,33].
HTC coal as a fuel
The heating value of the feedstock is increased signifi-
cantly due to the carbonization. Additionally, the mech-
anical dewatering capability is increased [36,37] which is
an important aspect for the conversion chain efficiency
from moist biomass to heat [38]. Calculations of different
conversion chains both revealed positive and negative
impacts of incorporating HTC as an additional conversion
step [39,40]. Therefore, one focus of current research is
Current Opinion in Chemical Biology 2013, 17:515–521
518 Energy
Figure 3
O O
CH3—CH2OH
COOH
CH3—COOH
O O
OH
O O
OH
OH OCH3
O
OH
Typical products of hydrothermal biomass liquefaction [14].
the increase of the process efficiency of HTC. Promising
experiments showed an important influence of process
liquor recirculation, which both increases the solid yield
and the dewatering capability [37]. Additionally, the
solids load proved to have a significant impact on the
auxiliary energy required [38,41] while positively affect-
ing the product distribution [32,33]. Internal heat recov-
ery is an important aspect of the process design
[38,39,41,42], especially because the heat of reaction of
HTC was measured to be comparably low [43].
Material use of HTC coal for electricity generation and
storage
Energy storage becomes more important with increasing
use of renewable energy sources such as wind and
photovoltaics. Basic research has shown that carbon-
aceous materials produced from HTC coal have prom-
ising properties for the application as supercapacitators
and as anode and cathode material for batteries and fuel
cells.
Analyses of HTC coal from cellulose, starch, and sawdust
activated at 700 and 8008C with KOH recorded the
highest capacitance ever reported for porous carbons in
a symmetric two-electrode configuration using an organic
electrolyte (1 M TEABF4 in acetonitrile) [44]. They
exceeded the specific capacitance of commercially acti-
vated carbons by 100% and were even capable of retain-
ing 64–85% when the current density was increased
(Figure 4). N-containing HTC coals activated at 6008C
with KOH also exhibited excellent electrochemical per-
formances [45].
Current Opinion in Chemical Biology 2013, 17:515–521
OH COOH
O
O
O O
O COOH
O
O
OH
OH OH
OH
OH
COOH O
Current Opinion in Chemical Biology
HTC nanospheres have been successfully tested as
anodes in Li+ and Na+ batteries [46,47]. Their reversible
capacity was higher than that of traditional graphite
electrodes and reached up to 370 mAh g1 at a 1 C rate.
A one-step solvothermal method can even be used for the
challenging production of cathode materials with superior
storage performance [48].
Nitrogen doped carbons prepared by hydrothermal
carbonization may also play an important role for the
reduction of noble metals used as catalysts in fuel cells
[49,50]. They can either enhance the performance of
nonprecious metal catalysts [51] or show methanol toler-
ant oxygen reduction [52]. Such carbonaceous materials
can even be a step toward the development of metal free
catalysts, both for the anode and cathode material [53].
Future perspectives (100)
Hydrogen and methane can be produced from biomass in
one-step hydrothermal gasification with nearly complete
gasification. This conversion technology is well investi-
gated and ready for technical application. Further
research on suitable and stable catalysts is required to
increase its economical feasibility. Results on lignin split-
ting have been very promising for the production of resins
and chemicals but further research is required to increase
yields. High organic load in the aqueous phase of hydro-
thermal liquefaction and carbonization is a challenge. It is
generally feasible to treat the waste stream from hydro-
thermal carbonization both aerobically and anaerobically
[36,54] but further research is required before a technical
application. One major issue for the combustion/cofiring
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 Hydrothermal conversion of biomass to fuels and carbon Kruse, Funke and Titirici 519

Figure 4

(a) 10 mV/s (b) AC-C700

1 mV/s AC-W800 250
300 AC-C800
Specific Capacitance / F g-1

Specific Capacitance / F g-1

AC-S700
200
200 AC-W700

100 AC-W800
100 mV/s
0 150
increase in scan rate
-100
100
-200

-300 YP-17D
50
-2 -1 0 1 2 0 5 10 15 20
Voltage / V Current density / A g-1
Current Opinion in Chemical Biology

Electrochemical characterization of HTC-derived activated carbons in 1 M TEABF4 solution in acetonitrile at room temperature: (a) cyclic
voltammograms (CV) of the activated carbon obtained from sawdust at 8008C (AC-W800) and (b) capacitance retention with current density in
comparison with that of commercially available YP-17D activated carbon [44].

of biomass is its low ash melting point. HTC coal can have
a similar ash melting point as lignite [42] although the
minerals are retained to some extent in the solid product
and do not seem to change their ash melting behavior
significantly [40]. Further research on the behavior of
minerals during hydrothermal carbonization is required.
Materials produced from hydrothermal carbonization in
laboratory scale have shown promising properties with
varying morphologies, functionalities and porosities.
They can have important applications in various modern
fields such as electrode materials in supercapacitors, Li-
ion batteries, and metal free catalysts in the oxygen
reduction reaction in fuel cells
References and recommended reading
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Current Opinion in Chemical Biology 2013, 17:515–521
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