Fuel 180 (2016) 591596

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Fuel
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Full Length Article

Solid fuel production by hydrothermal carbonization of water-like phase

of bio-oil
Yan Fu a,, Jun Ye a, Jie Chang a, Hui Lou b, Xianwei Zheng a
a
Key Laboratory of Heat Transfer Enhancement and Energy Conservation of Education Ministry, School of Chemistry and Chemical Engineering,
South China University of Technology, Wushan Road 381#, Guangzhou 510640, China
b
Institute of Catalysis, Department of Chemistry, Zhejiang University, Hangzhou 310028, China

h i g h l i g h t s

g r a p h i c a l a b s t r a c t

Hydrothermal carbonization was

applied in water-like phase of bio-oil.

Solid fuels and stable oxygen

containing liquid fuels were

successfully obtained and separated
easily.

Energy recovery efficiency of solid
fuel (hydrochar) was 50.38%.

a r t i c l e

i n f o

Article history:
Received 11 February 2016
Received in revised form 19 April 2016
Accepted 20 April 2016
Available online 26 April 2016
Keywords:
Solid fuel
Hydrothermal carbonization
Water-like phase
Bio-oil

a b s t r a c t
Hydrothermal carbonization was applied in water-like phase of bio-oil for the polymerization and
carbonization of sugars and sugar derivatives. The hydrothermal carbonization was carried out in an
autoclave from 130 to 230 C, and solid fuels and stable oxygen containing liquid fuels were successfully
obtained simultaneously. Results showed that with the temperature increased, polymerization and carbonization between sugars and sugar derivatives were accelerated and concurrent. The increase in final
pressure and yields of extraction phase when the temperature was over 190 C was mainly occurred by
depolymerization of the polymer. The maximum yield, energy recovery efficiency, and carbon recovery
efficiency of solid fuel (hydrochar) were 11.22 wt%, 50.38%, and 18.04%, respectively. The carbon content
of hydrochars ranged from 63.87 to 73.95 wt%, and the high heating value (HHV) of hydrochars ranged
from 25.51 to 30.48 MJ/kg. Compared with the water-like phase of bio-oil, the carbon content and high
heating value of hydrochars were increased 1.581.84 times and 4.355.29 times, respectively.
Combining the FT-IR spectra of hydrochars and ethyl acetate (EA) phase results, phenolic compounds
were detected to be incorporated with hydrochars and the incorporation of both phenol,
1,2-Benzenediol was occurred when the temperature increased to 190 C.
2016 Elsevier Ltd. All rights reserved.

1. Introduction

Corresponding author.
E-mail address: fuyan@scut.edu.cn (Y. Fu).
http://dx.doi.org/10.1016/j.fuel.2016.04.089
0016-2361/ 2016 Elsevier Ltd. All rights reserved.

Bio-oil, as a liquid product from the fast pyrolysis of biomass, is

considered to be the main source of fuels and chemicals in the
future [1]. Aromatics, sugars and sugar derivatives are the main

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Y. Fu et al. / Fuel 180 (2016) 591596

components of bio-oil, and they can be potentially upgraded to

fuels [2]. However, sugars and sugar derivatives that contain reactive compounds such as hydroxyl groups, carbonyl groups or conjugated p bonds, were found to be reactive toward polymerization
[3]. Furthermore, the polymerization of bio-oil even occurred at
ambient conditions during aging [4,5], leading to the high instability of bio-oil and limited for its further processing [6]. Recently,
according to a certain water-to-oil ratio, bio-oil could be separated
by adding water [7,8], and water-like phase which concentrated
with sugars and sugar derivatives could be obtained [9]. Sugars
and sugar derivatives in water-like phase could further convert
to value-added chemicals via acid-catalyzed conversion, but solid
deposit always concentrated on catalysts and consequently
decreased the efficiency of conversion [10]. Moreover, how to
selectively produce targeted chemicals from bio-oil and effectively
separate them are two main challenges due to the complexity of
bio-oil [9].
In order to improve the stability of fast pyrolysis derived bio-oil,
it is worthwhile to convert the troublesome sugars and sugar
derivatives into value added chemicals or fuels [9,10]. Now,
hydrothermal carbonization is mentioned as a promising technology to convert biomass into hydrochar and functionalization carbon material [1114]. The sources of carbonization include
agricultural residues [13], lignocellulosic biomass [14] and some
carbohydrates (such as glucose, cyclodextrins, fructose, sucrose,
cellulose, and starch) [1520]. Hydrochars has been considered
as coal substitute in gasification and combustion applications. In
our work, hydrochars is produced by hydrothermal carbonization
of sugars and sugar derivatives from water-like phase of bio-oil.
This method has three advantages: (1) separation and conversion
of troublesome sugars in bio-oil would not be necessary, (2) solid
and stable oxygen contained liquid fuels could be obtained simultaneously, and (3) the conversion products can be separated by filtering separation effectively and the stability of the rest bio-oil
would be obviously increased. Therefore, the object of this work
was to convert the troublesome sugar and sugar derivatives into
solid fuels and liquid fuel as a by-product. The aforementioned
methods put emphasis on polymerization mechanism of model
compounds of bio-oil water phase or used solid waste biomass
for producing solid biochar fuel only. Our work dealt with real
bio-oil from biomass pyrolysis factory and got solid fuel and liquid
fuel as a by-product and separated them easily.
2. Experimental section

Fig. 1. Separation of water-like phase products after hydrothermal conversion.

ative pressure through a preweighed quantitative filter paper. The

solid products (hydrochars) and filter paper were dried to constant
weight at 105 C. The aqueous phase was extracted with ethyl
acetate (EA) to form an EA phase. Yield of hydrochars was measured two or three times through weighing, respectively. The
hydrochars produced in X C were labeled as Hydrochar-X. Similarly, the EA phases produced at a temperature of X C were labeled
as EA-X and EA phases of water-like phase labeled as EA-W.
2.3. Analytical methods
The EA phase products were analyzed by Gas Chromatography
Mass Spectrometry (GCMS). GCMS analysis was tested on a
Shimadzu QP 2010 Plus system equipped with an Rxi-5 ms column
(30 m  0.25 mm  0.25 lm). The temperature of the injector was
set at 265 C. The column temperature program was 60 C (hold
3 min) ? 150 C (2 C/min, hold 1 min) ? 270 C (20 C/min, hold
5 min). The HHV of hydrochars was measured with calorimeter
(IKA-2000). The C, H, O, N and S elemental contents (weight percent)
were determined with an Elementer Vario EL III instrument. The
functional groups were analyzed by Fourier transform-infrared
spectroscopy (FT-IR) on a Nexus 670 (Nicolet, USA). The ash content
of hydrochar was tested according to previous reports [21].
2.4. The yields, energy recovery efficiency (ERE) and carbon recovery
efficiency (CRE) of hydrochars

2.1. Materials and chemicals

The bio-oil was purchased from Xinfa Gardon Engineering Co.,
Ltd. (Shandong, China) and obtained from pyrolysis of pine, aspen
wood meal and rice husk at 500700 C. The annual bio-oil yield
was 20,000 tons. Water-like phase was cut out from the distillate
fractions below 120 C, while the water content was 69.5 wt%
(detected by Karl Fischer moisture measurement), the total organic
carbon content was 430 g/L (detected by vario TOC instrument),
and the density was 1.067 kg/L. All chemicals used in this study
were of analytical grade and used without further purification.

The yields, energy recovery efficiency (ERE) and carbon

recovery efficiency (CRE) of hydrochars were calculated by Eqs.
(1)(3), respectively. m in the equation mean the weight of the
sample in the parentheses:

m Hydrochar
 100%
1
m water-like phase
Total HHV of Hydrochar
ERE %
 100%
2
Total HHV of water-like phase
Total carbon content of Hydrochar
 100% 3
CRE %
Total carbon content of water-like phase

Yields %

2.2. Methods
Hydrothermal conversion experiments were conducted in a
100 mL stainless steel 316 autoclave. The autoclave was loaded
with 60 g water-like phase of bio-oil. Nitrogen was used to purge
the autoclave for four times. The temperature was raised to the
set values (130230 C), and the autoclave was kept at the reaction
temperature for 20 h. The separation process of the hydrothermal
products is shown in Fig. 1. The products were filtered under neg-

3. Results and discussion

3.1. Yields of hydrochars and final pressure
The polymerization on heating up of bio-oil model compounds
[3] has revealed that the condensation of bio-oil was mainly due to
the reactive components of sugars (levoglucosan) and sugar

Y. Fu et al. / Fuel 180 (2016) 591596

593

Fig. 2. Yields of hydrochars and final pressure in different reaction time and temperature. (a) (Reaction condition: water-like phase 60 g, temperature: 190 C, time: 525 h).
(b) (Reaction condition: water-like phase 60 g, temperature: 130230 C, time: 20 h).

derivatives (including furfural, hydroxyl aldehyde and hydroxyl

acetone). The hydrothermal carbonization of biomass components
(cellulose, hemicellulose, and lignin) also revealed the decrease in
hydrochar due to deoxygenating reactions (e.g., dehydration,
decarboxylation) and simultaneously producing gaseous products
[22,23].
The yields of hydrochars and final pressure are shown in Fig. 2.
As is seen from Fig. 2a, final pressure increased with the reaction
time, and then gradually stabilized. The increased final pressure
indicated that hydrothermal carbonization of sugar polymer was
gradually increased. And this increase was gradually enhanced as
reaction time increased, and then stabilized eventually, and the
best reaction time was 20 h. The yields of hydrochars were changed simultaneously as the final pressure, and the maximum yield
was 10.45%.
As is seen from Fig. 2b, the yields of hydrochars increased at
first and are then dropped as temperature increased, and the maximum yield was 11.22 wt% (170 C). The final pressure was
increased as the temperature increased. This phenomenon was
mainly due to the polymerization and decomposition of sugars in
bio-oils. According to the previous report, the sugars (such as
levoglucosan) mainly underwent hydrolysis to glucose. With water
medium, the glucose could further undergo decomposition into

various small compounds that were very reactive toward their

own polymerization or with other compounds. Therefore, polymerization and carbonization of sugars and sugar derivatives were
concurrent as reaction temperature increased.
The yields of aqueous phase and yields of extraction phase are
shown in Fig. 3. The yields of aqueous phase ranged from 82.55%
to 75.95%, and decreased as temperature increased. The yields of
extraction phase were decreased and then increased as temperature increases.
The result demonstrated that with the temperature increased,
the polymerization between sugars and sugar derivatives was
accelerated. Simultaneously, the carbonization was increasing as
temperature increased, and both polymerization and carbonization
were concurrent. When the temperature was over 190 C, depolymerization of the polymer happened. The yields of extraction
phase and final pressure were further increased.
3.2. The elemental composition, HHV, CRE, ERE of hydrochars
As is shown in Table 1, it is clear to find that C, H, S content and
HHV were positively correlated with the temperature. The O content was negatively correlated with the temperature. The C content
increased and O content decreased was very distinctly, ranged

Fig. 3. The yields of aqueous phase and extraction phase.

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Y. Fu et al. / Fuel 180 (2016) 591596

Table 1
The properties of the feedstock and upgraded oil.

a
b

Sample

Ca,b (wt%)

Hb (wt%)

Ob (wt%)

Nb (wt%)

Sb (wt%)

Ash (wt%)

HHV (MJ/kg)

CRE (%)

ERE (%)

Water-like phase
H-130
H-150
H-170
H-190
H-210
H-230

40.30
63.87
63.90
64.81
66.88
71.61
73.95

5.81
5.82
5.87
5.94
6.22
6.41

28.15
26.87
25.01
22.28
21.04
18.47

0.55
0.59
0.59
0.60
0.59
0.60

0.06
0.13
0.14
0.15
0.15
0.15

3.94
8.56
11.02
11.82
5.96
2.18

5.76
25.51
25.79
25.87
26.99
29.07
30.48

14.45
15.32
18.04
17.11
16.31
15.74

39.69
43.26
50.38
48.30
46.98
45.37

The relevance (R2) between HHV and C content was 0.9946.

Dry basis.

from 63.87% to 73.95% and 28.15% to 18.47%, respectively. The C

content was about 1.581.84 times higher when compared to
water-like phase. The H, N, S content was slowly increased with
the temperature increase, and then maintained at a stable level,
and N, S content was quite lower than other biomass and black
liquor derived biochar [13,21]. The HHV of hydrochars ranged from
25.51 to 30.48 MJ/kg. Compared with the corresponding feedstock,
the HHV of hydrochars was 4.355.29 times higher. According to
Chinese National Standard (GB/T15224.3-2010) the HHV of hydrochars amounts to medium high-rank and high-rank coals. The HHV
was probably related to the increasing C content and the correlation between HHV and C content was very high (R2 = 0.9946).
The maximum value of CRE and ERE was 18.04% and 50.38%,
respectively, indicated that hydrothermal carbonization of waterlike phase was not only an effective way to remove the unstable
components of bio-oil but also a method to get hydrochars.
3.3. Properties of hydrochars and EA phases
Fig. 4 shows that the FT-IR spectra of hydrochars with different
temperature were basically the same. For more specific, the
absorption bands positioned at 3430 cm1 were attributed to the
stretching of OH (hydroxyl or carboxyl). The bands positioned
at 2967, 2930, 2865 cm1 were attributed to the asymmetric and
symmetric stretching of CH3, CH2. The bands positioned at
1690 cm1 was C@O stretching, 1616 cm1 C@C was stretching
of aromatic and furan rings, and 1450 cm1 was benzene ring
frame vibration. This indicated that phenols were incorporated
into the hydrochars. The bands positioned at 10001450 cm1
were CO (hydroxyl, esters, or ethers) stretching and OH bending
vibrations. The bands in 867755 cm1 were CH out-of-plane
bending vibrations, attributed to the existence of phenolic

Fig. 4. FT-IR spectra of hydrochars in different temperature.

Fig. 5. The relative areas of phenolic compounds in extraction phase.

compounds in hydrochars [22]. Therefore phenols in the water

phase of bio-oil were involved in the polymerization as other components like sugars also could be transformed into the species with
aromatic structures.
The relative areas of phenolic compounds in extraction phase
are shown in Fig. 5 and Table 2. As seen from the GCMS analysis,
esters, ketones, furans and phenols were the main compounds in
EA-W. The relative peak areas of the total phenols accounted for
56.53%. After hydrothermal carbonization, sugar derivatives (such
as furfural, 1-hydroxy-2-butanone) were aggregated with hydrochars and hardly to be detected in EA-X. From Fig. 5, the total phenols in EA-X were lower than those in EA-W. This phenomenon
also occurred in monophenols, diphenols, and the others. This indicated that phenol compounds were obviously incorporated into
the hydrochars. The phenol and 1,2-Benzenediol both increased
from EA-W to EA-X, and this increase also occurred as reaction
temperature increases. The obvious decrease of both the phenol
and 1,2-Benzenediol occurred in 190 C, and indicates that both
the phenol and 1,2-Benzenediol obvious incorporated into the
hydrochars.
The incorporation mechanism of phenols and sugars is
schematically illustrated by previous report. According to a recent
study, sugars are dehydrated into low molecular compounds and
then rapidly react with phenols via intermolecular dehydration
to produce polymers [22]. Based on this mechanism, after carbonization the other monophenol, other 1,2-Benzenediol and the
others were obviously incorporated into hydrochar in lower
temperature (130 C). The incorporation of both the phenol and
1,2-Benzenediol occurred in 190 C.

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Y. Fu et al. / Fuel 180 (2016) 591596

Table 2
The relative areas of phenolic compounds in extraction phase.
Rent. time (min)

Compounds (phenolics)

EA-W

EA-130

EA-150

EA-170

EA-190

EA-210

EA-230

6.38
8.287
8.609
9.265
9.65
10.228
10.77
11.605
13.45
13.943
14.602
15.026
15.185
16.349
16.525
16.932
17.285
18.654
19.227
20.446
20.771
21.157
22.054
22.681
23.75
25.759
26.039
26.171
26.451
27.262
28.469
28.919
29.303
29.597
29.76
31.31
32.176
34.044
34.327
34.483
35.05
37.103
38.999
40.69
44.606
45.193
48.475
48.703
55.869
56.51

Phenol
Benzyl alcohol
2-Hydroxy-benzaldehyde
2-Methyl-phenol
Acetophenone
4-Methyl-phenol
2-Methoxy-phenol
2,6-Dimethyl-phenol
2-Ethyl-phenol
2,4-Dimethyl-phenol
2,3-Dihydroxybenzaldehyde
4-Ethyl-phenol
3-Ethyl-phenol
2-Methoxy-4-methyl-phenol
3,4-Dimethyl-phenol
2,3,5-Trimethyl-phenol
1,2-Benzenediol
2,3,6-Trimethyl-phenol
1-Ethyl-4-methoxy-benzene
3-Methoxy-1,2-benzenediol
3-Methyl-1,2-benzenediol
1-(2,5-Dihydroxyphenyl)-ethanone
Hydroquinone
4-Methyl-1,2-benzenediol
3-Hydroxy-benzaldehyde
2-Methoxy-5-methylphenol
Methyl-hydroquinone
2,6-Dimethoxy-phenol
2-Methoxy-4-(1-propenyl)-phenol
4-Hydroxy-benzaldehyde
4-Ethyl-1,3-benzenediol
Vanillin
1-(3-Hydroxyphenyl)-ethanone
1,3-Benzenedicarboxaldehyde
l,4,5-Dimethyl-1,3-benzenedio
4-Hydroxy-2-methylbenzaldehyde
4-Ethyl-2-methoxy-phenol
4-Propyl-1,3-benzenediol
1-(4-Hydroxy-3-methoxyphenyl)-ethanone
4-Hydroxy-3-methylacetophenone
4-Ethyl-2-methoxy-phenol
Guaiacylacetone
2,3-Dimethyl-benzoic acid
3,4-Dihydroxy-5-methoxybenzaldehyde
4-Hydroxy-3,5-dimethoxy-benzaldehyde
4-((1E)-3-hydroxy-1-propenyl)-2-methoxyphenol
3-(4-Hydroxy-3-methoxyphenyl)-2-propenal
1-(4-Hydroxy-3,5-dimethoxyphenyl)-ethanone
3,5-Dihydroxybenzaldehyde
3,5-Dimethoxy-4-hydroxycinnamaldehyde
Phenol
1,2-Benzenediol
Monophenols (except phenol)
Diphenols (except 1,2-Benzenediol)
Others
Total phenols

3.8
0.42
0.26
3.06
0.41
2.42
0.72
0.18
0.18
0.78
0.15
0.44
0.19
0.33
0.14
0.22
20.93
0.34
0.7
0.56
3.03
0.22
1.3
4.78
0.3

5.22
0.15

6.1
0.11

7.03
0.1

6.31

5.82

4.57

2.26
0.14
3.05
0.91

2.65

2.48

2.35

1.93

2.8
1.17

2.93
0.1
2.68
1.42

3.04
1.59

2.56
1.64

2.94
1.7
0.3

0.66

0.51

0.5

0.87

0.53

0.73

0.42

0.4

0.82
0.27

0.4

0.42

0.45

0.3

0.77
0.2

22.59
0.57
0.31
1.7
0.52
2.39
3.23

22.7

1.26
0.37
2.44
2.48

23.99

19.29

17.95

13.19

1.51
0.36
2.61
3.51

0.54
1.79
0.41
2.79
3.84

0.29
1.61
0.43
3.08
4.28

0.64
1.45
0.23
2.29
4.25

0.23

0.23
1.79

1
0.3
0.15
3.19
1.28
0.16
0.16

0.98

1.05

1.14

1.19

1.47

0.3
1.99
0.61
0.32

1.96
0.22
0.27

2.37

2.37

2.49

2.37

0.42

0.34

0.39

0.42

0.31

0.43

0.18
0.2
0.49

0.2
0.32
0.54
0.63
0.35
0.51
0.12
0.39
0.14
0.38
0.24
0.26
0.22
0.17
0.16
3.8
20.93
11.8
8.37
11.63
56.53

0.39
0.41
0.4

0.48

0.6
0.98

0.46
0.7

0.72

0.18

0.25

0.21

7.03
23.99
9.07
5.02
7.92
53.1

6.31
19.29
10.5
6.17
7.32
49.6

5.82
17.95
9.63
6.18
7.63
47.2

0.21
0.17

0.18

5.22
22.59
9.54
5.24
8.04
50.6

6.1
22.7
8.6
3.74
5.85
46.9

4.57
13.19
8.32
6.34
8.4
40.82

4. Conclusions

Acknowledgments

Hydrothermal carbonization was an effective way to remove

the unstable components of bio-oil and simultaneously obtained
high energy-dense hydrochars. Under the conditions of 170 C,
20 h, the maximum yield, ERE, and CRE of hydrochars were
11.22 wt%, 50.38%, and 18.04%, respectively. Combining the FT-IR
spectra of hydrochars and EA phases results, phenolic compounds
(phenol, 1,2-Benzenediol) were deep incorporated into the hydrochars when the temperature was increased to 190 C. Considering
the combustion characteristic of hydrochar as a solid fuel and possible application as function materials, an overall research of this
new technique is required before the process may be considered
on an industrial scale.

This research was financially supported by the National Basic

Research Program of China (973 Program) (No. 2013CB228104)
and Natural Science Foundation of China (No. 21476090).

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