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Bioresource Technology: Omid Norouzi, Sajedeh Jafarian, Farid Safari, Ahmad Tavasoli, Behnam Nejati
Bioresource Technology: Omid Norouzi, Sajedeh Jafarian, Farid Safari, Ahmad Tavasoli, Behnam Nejati
Bioresource Technology
journal homepage: www.elsevier.com/locate/biortech
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
a r t i c l e
i n f o
Article history:
Received 26 June 2016
Received in revised form 3 August 2016
Accepted 5 August 2016
Available online 8 August 2016
Keywords:
Cladophora glomerata
Pyrolysis
Bio-char
Bio-oil
Macroalgae
a b s t r a c t
Conversion of Cladophora glomerata (C. glomerata) as a Caspian Seas green macroalgae into gaseous, liquid and solid products was carried out via pyrolysis at different temperatures to determine its potential
for bio-oil and hydrogen-rich gas production for further industrial utilization. Non-catalytic tests were
performed to determine the optimum condition for bio-oil production. The highest portion of bio-oil
was retrieved at 500 C. The catalytic test was performed using the bio-char derived at 500 C as a catalyst. Effect of the addition of the algal bio-char on the composition of the bio-oil and also gaseous products was investigated. Pyrolysis derived bio-char was characterized by BET, FESEM and ICP method to
show its surface area, porosity, and presence of inorganic metals on its surface, respectively. Phenols were
increased from 8.5 to 20.76 area% by the addition of bio-char. Moreover, the hydrogen concentration and
hydrogen selectivity were also enhanced by the factors of 1.37, 1.59 respectively.
2016 Elsevier Ltd. All rights reserved.
1. Introduction
Industrial development during the last centuries has made a
leap in the progress of human life. However, recently, the alarming
effects of this development on the environment is being appeared
dramatically (Dincer and Rosen, 2012; Akalin et al., 2012). Climate
change and energy security are among the most important con Corresponding author at: School of Chemistry, College of Science, University of
Tehran, Tehran, Iran.
E-mail addresses: tavasoli.a@ut.ac.ir, a-tavasoli@srbiau.ac.ir (A. Tavasoli).
http://dx.doi.org/10.1016/j.biortech.2016.08.017
0960-8524/ 2016 Elsevier Ltd. All rights reserved.
cerns of the recent era (Jones and Warner, 2016; Shoja et al.,
2013). Production of energy carriers with a minimum carbon content in the combustion process would be promising (Ali et al.,
2013). Moreover, availability and renewability of the primary
resources are crucial. In the recent decade, extensive research
has been carried out on the production of gaseous and liquid
energy carriers from bio-renewable resources (Krishnan and
McCalley, 2016). Biomass feedstocks are rich in carbon and hydrogen and can be converted into valuable fuels and chemicals
(Phillips et al., 2016). However, agricultural wastes as the second
generation of feedstocks are dependent on landing availability
644
O% 100 C% H% N% S% Ash%
The amount of protein in the sample was recognized in accordance with National Standard in China GB/T 6432-1994 by the
method of Kjeldahl, while the amount of lipid was determined
via the method of solvent extraction in accordance with National
Standard in China GB/T 6433-2006 (Zhao et al., 2015). Carbohydrate content was calculated by mass balance method by Eq. (3).
645
For carbon balance, the amount of carbon in the bio-oil and biochar was analyzed by a TOC analyzer (Shimadzu, TOC-L) and a
CHNS analyzer, respectively. Moreover, the amount of carbon in
the gas phase was calculated as the total moles of carbon in
carbon-containing gaseous products in mass basis.
2.4. Product analysis
The volume of collected gasses was measured from the displacement of the solution in the column. The quality and quantity
of produced gaseous mixture were analyzed using gas chromatography technique (Varian 3400 and Teyfgostar-Compact). The biooil in glass condenser and char left inside the reactor were
measured by measuring the difference in weights of glass condenser and reactor before and after the reaction. Considering the
small reactor volume and feedstock quantity added into the system, reported data are the averages of several observations for
each experiment in order to make results more statistically confident. Also, the accuracy of data collection and comparison between
means of compositions and yields from the processing of two samples was studied through ANOVA (analysis of variance). The statistical level was 5% with p < 0.05.
2.4.1. Gaseous product analysis
Gas samples were taken by tight syringes and injected into Gas
chromatographs column. A gas chromatograph (Varian 3400 and
Teyfgostar-Compact) had been equipped with PORAPAK Q-S
80/100 (30 m long, 0.53 mm I.D) column, a methanizer and Flame
Ionization Detector (FID). Argon was used as carrier gas and oven
temperature program was in the following: 40 C isothermal for
5 min, an increase in the temperature from 40 to 75 C in
17.5 min and isothermal in 75 C for 5 min. The methanizer option
646
Concentration v=v%
CGE
9
10
Mj
f33:5 C 142:3 H 15:4 O 14:5 Ng 0:01
kg
Hydrogen Selectivity
Concentration of H2
Concentration of other gasses
Carbon liquefaction efficiency (CLE), Carbon solidification efficiency (CSE) and Carbon gasification efficiency (CGE) are mentioned below as Eqs. (7)(9) to obtain the total carbon balance
(Norouzi et al., 2016; Safari et al., 2016a)
CLE
CSE
647
Table 1
Effect of temperature on the product distribution and main gaseous component of the pyrolysis of C. glomerata.
Reactors temperature (C)
400
500
600
Products (wt%)
Concentration (v/v%)
Bio-oil
Bio-char
Gas
H2
CO
CO2
CH4
35
39
34
44
40
39
21
22
28
15.93
27
37.1
12.53
12.9
12.4
68.03
56.09
45.19
3.51
4.01
5.31
648
Table 2
Compounds identified by GCMS in C. glomerata derived bio-oil produced by catalytic and non-catalytic pyrolysis.
No.
RT (min)
Compound
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
1.385
1.417
1.66
2.107
2.226
2.482
2.607
2.638
3.191
3.416
4.216
4.282
4.789
6.225
6.562
7.159
7.535
7.671
7.82
7.879
8.02
8.169
8.21
8.45
8.97
9.353
9.46
9.491
9.55
9.81
10.11
10.67
10.85
11.11
11.51
12.48
12.68
12.78
12.9
12.97
13.08
13.24
13.31
13.47
13.58
13.72
13.81
13.94
14.06
14.18
14.58
15.28
15.41
15.85
15.911
16.02
16.24
16.347
16.52
16.659
16.7
16.91
17.051
17.1
17.32
17.46
17.66
17.862
17.944
18.008
18.28
19.07
19.37
Trimethylamine P183
Acetone
Methylamine, N,N-dimethylAcetic acid
2-Propanone, 1-hydroxyPyrazine
2,4-Pentadienenitrile
Pyridine
Dimethylformamide P185
Phenol
Dimethylacetamide
Carbramal
Amitrol
Mepivacaine
2-Cyclopenten-1-one, 2-hydroxy-3-methylp-Cresol
Tridecane
Quinuclidine-3-ol
Perhexiline AC P859
ETHYLCYCLOPENTENOLONE
2-Pentyn-1-ol
N,N-DIMETHYLHOMOSERINE LACTONE
Pyridine
Pyrrole
Cyclopentanone
Methylpentynol P191
Pyridine, 2-methyl2,3-Anhydro-D-mannosan
Pyrazine, methyl1-Propanamine
2-Furanmethanol
1-Pentene, 2-methyl
Ethanone, 1-(2-furanyl)Pyridine, 2,4-dimethyl
2-Cyclopenten-1-one, 3-methylPhenol, 2-methylPhenol, 3-methyl2,5-Pyrrolidinedione, 1-methyl4-Hydroxy-2-hydroxyaminopyrimidine
Phenol, 2,6-dimethylMaltol
Octane, 2,7-dimethylPhenol, 2,4-dimethylPhenol, 3-ethyl1-(2-Pyrazinyl)-1-ethanol
Pyrazine, methyl-5-(1-propenyl)-, (E)Methyl Tanol
2-Propenoic acid, 2-methyl-, ethyl ester
Benzenepropanenitrile
Quinoline
5H-1-Pyrindine
1H-Indole, 5-methylNaphthalene, 2,7-dimethyl1H-Benzimidazole, 2-ethylTetradecanoic acid
Indolizine, 1,2-dimethylDecanoic acid
Pyrrolo[1,2-a]piperazine-3,6-dione
2-Formyl-1-thiocromone
Phytol
1,4-Dimethylindan-1-ol
1H-Pyrazole, 3-methyl-5-phenyl7-Thiaprotoadamantane
NEOPHYTADIENE
Pyridine, 3-(1-methyl-1H-pyrrol
2,4-Azetidinedione, 3,3-diethylTridecane, 7-methylene
Pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl)n-Hexadecanoic acid
3,9-DIAZATRICYCLO[7.3.0.0(3,7)]DODECAN-2,8-DIONE
Thiazolo [4,5-f]quinoline
2-Pentyadecanone, 6,10,14-trimethyl
9H-Fluorene, 9-methylene
Area%
Non-catalyst
Catalytic
3.08
4.4
2.15
26.88
2.09
0.67
1.6
2.1
0.68
4.23
0.59
0.94
2.56
4.66
4.52
1.68
2.77
0.5
3.29
0.1
5.72
8.35
4.325
2.25
0.76
1.01
0.44
0.91
0.64
0.5
0.96
0.51
0.67
0.53
0.37
0.56
2
0.87
4.12
1
0.12
2.88
9.91
0.14
0.31
3.01
3.778
1.209
0.791
1.99
0.85
0.88
0.67
0.38
0.36
2.532
0.33
0.97
1.35
0.28
0.75
0.38
0.83
2.2
3.79
0.84
0.34
0.69
1.11
1.11
0.97
1.99
0.88
0.61
0.59
2.23
0.78
0.4
1.95
1.96
0.53
0.62
7.72
0.37
0.51
0.35
1.41
0.49
0.41
0.36
1.08
0.52
5.68
0.97
0.35
0.3
0.37
0.714
2.241
649
RT (min)
Compound
Area%
74
75
76
77
78
79
80
81
82
83
84
19.53
19.85
19.92
20.16
20.75
21.33
21.48
21.73
22.79
23.07
25.22
Tetrahydroionone
6,6-Dimethyl-cyclooct-4-enone
Hexadecanenitrile
Hexadecanoic acid, methyl ester
Z-11-Pentadecanol
2-Hydroxy-3,5,5-trimethyl-cyclohex-2-enone
9-Hydroxybutyl-3,9-diazabicyclo(3,3,1)nonane
N,N-dimethyloctanamide
2-Heptanone, O-methyloxime
Methyl 7,9-tridecadienyl ether
9-Octadeconoic acid
Non-catalyst
Catalytic
3.56
0.31
0.94
0.64
2.03
0.58
0.85
0.45
0.45
0.64
2.19
Table 3
Effect of bio-char catalyst on the product distribution and the main gaseous products of C. glomerata pyrolysis.
Tests at T = 500 C
No catalyst
Bio-char catalyst
Products (wt%)
Concentration (v/v%)
Bio-oil
Bio-char
Gas
H2
CO
CO2
CH4
39
30
40
35
22
35
27
37.08
12.90
11.8
56.09
47.09
4.01
4.03
in Fig. 3, the addition of algal bio-char as a catalyst results in producing more interesting compounds. This part has been focused on
some noteworthy compounds based on the functional groups such
as acids, phenols, ketones, N-compounds, furans and alcohols, in
the terms of area%. As seen in Fig. 3, the main effect of bio-char
on the bio-oil component is the decrement in acids (28.55
23.09% for C. glomerata) which is followed by a decrease in ketones
which could be in association with the ketonization reactions, in
which acids in the pyrolysis vapor convert to ketones (Liu et al.,
2014). Moreover, the phenols were increased with the addition
of algal bio-char catalyst (8.520.76%). The furans content of the
bio-oil from C. glomerata was found to decrease from 3% to 2.1%
with the addition of bio-char. This effect can be attributed to the
presence of alkali metals (K, Na), which was reported earlier by
Mahadevan et al. (2016) this effect can be associated with decarbonylation and oligomerization reactions to produce olefins and
aromatic hydrocarbons in the presence of bio-char as a catalyst
(Mahadevan et al., 2015). These results were in agreement with
those reported in the literature (Ren et al., 2014).
3.1.3.3. Effect of the algal bio-char on the hydrogen selectivity. Hydrogen selectivity increased by the increasing of Temperature. The
highest hydrogen selectivity of 0.59 was obtained at a pyrolysis
temperature of 600 C. In addition, in the presence of algal biochar at the temperature of 500 C, H2 selectivity increased slightly
due to the catalytic effect of algal bio-char.
3.1.3.4. Effect of the algal bio-char on the bio-oil quality. The composition of bio-oil obtained from the pyrolysis of C. glomerata and its
blends with algal bio-char as a catalyst is shown in Table 2. As seen
650
Table 4
Carbon conversion efficiencies for catalytic and non-catalytic pyrolysis of C. glomerata.
Test#
Catalyst
Temperature
CGE
CSE
CLE
Carbon
balance
1
2
3
4
0.4 g bio-char
400
500
600
500
26.78178
26.23513
23.97984
35.38647
19.36
18.16
18.02
17.1
48.7
51
54.1
46.2
94.84177836
95.39512575
96.09983563
98.68647388
4. Conclusion
C. glomerata as green macroalgae of Caspian Sea showed a
promising performance for production of bio-oil and hydrogen.
Non-catalytic Pyrolysis of this green macroalgae resulted in acidrich bio-oil while the addition of its bio-char as a catalyst
promoted the production of phenolics. In addition algal, bio-char
enhanced the hydrogen production and hydrogen selectivity.
FESEM, BET and ICP analysis demonstrated the porous structure
and the presence of AAEMs in the bio-char which makes it suitable
for utilization as a catalyst or catalyst support in the industry.
Acknowledgements
The authors would like to thank Dr. Ali Karimi from Research
institute of Petroleum Industry (RIPI), for his kind support for
providing facilities for characterization of materials and Sharif
University of technology, for providing the FESEM device for characterization of bio-char surface.
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