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Center of Research Excellence in Nanotechnology, King Fahd University of Petroleum & Minerals, Dhahran, Saudi Arabia
Chemical Engineering Department, King Fahd University of Petroleum & Minerals, Dhahran, Saudi Arabia
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 6 November 2013
Received in revised form
3 June 2014
Accepted 6 June 2014
Available online xxx
The numerous challenges associated with declining fossil fuel reserves as energy sources, have accounted
for a shift to biofuels as alternatives. However, transesterication of animal fats and edible vegetable oils
using homogeneous acids and bases for biodiesel production is recently considered unsustainable by
industries, particularly due to food versus fuel competition, and economic and environmental challenges
associated with the feedstocks and catalyst systems, respectively. The paper therefore presents a critical
review on the prospects of non-edible oil (i.e. algae oil) for biodiesel production via heterogeneous
catalysis. It covers the advantages of algae oil exploitation over edible oil feedstocks, progress made in
the oil extraction, available heterogeneous catalyst systems and reaction mechanisms, optimum transesterication conditions and the way forward. As the economic feasibility of biodiesel production from
algae is supported by the valorization of glycerol as by-product, we have also highlighted key available
heterogeneous catalysts to upgrade glycerol into more useful industrial products.
2014 Elsevier Ltd. All rights reserved.
Keywords:
Biodiesel production
Edible oils
Algae oils
Heterogeneous catalysts
Glycerol
1. Introduction
Since its early commercialization as a substitute for petroleumdiesel for nearly a decade now, biodiesel have remained a good
global fuel for running automobile engines. Many interesting factors have been attributed to this success. Among others, biodiesel is
chemically non-toxic in nature, biodegradable and can simply be
prepared via transesterication under mild conditions [1]. In
addition to insignicant contribution to CO2 and other particulate
matter emissions, it could be employed directly in conventional
petroleum-diesel engines given optimal performance, particularly
due to very low sulfur and aromatic contents and compatible ash,
cloud and pour points [1e3]. However, although the global demand
for biodiesel has been projected to either doubled or tripled in
many regions by 2020 and beyond and relevant researches fully
intensied, a number of factors have not been critically addressed.
Conversion of the triglyceride esters in oils to the mono-alkyl esters
(biodiesel) requires a reaction of the former with monohydric
alcohol. Many researchers have recommended lower monohydricalcohols (i.e. methanol to propanol), with no clear justication of
which provides the best viscosity requirements in line with
http://dx.doi.org/10.1016/j.energy.2014.06.018
0360-5442/ 2014 Elsevier Ltd. All rights reserved.
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
Table 1
Short term projection of biofuels from algae.
Short term potentials, 2014
Billion gallons
Assumed 1 gallon
of oil $3.0
1500
41
26
15
2.73%
$123 billions
9.2%
$425 billions
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
Table 2
A summary of heterogeneous transesterication catalysts reported in the literature
[14e43].
Solid acids
Solid bases
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
Table 3
Role of calcination temperature on the activity of WO3 modied ZrO2 [49].
Sample
code
Calcination
temperature [ C]
Conversion (%),
5 wt.% WO3/ZrO2
Conversion (%),
15 wt.% WO3/ZrO2
A
B
C
D
E
400
500
600
700
900
93
95
10
5
5
78
81
20
25
17
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
Table 4
Data for biodiesel production over solid catalysts (including zeolites) from algae and
some common oils.
Feedstock
Catalysts
Soybean
Corn oil
Algae oil
Algae oil
Algae oil
Algae oil
Algae oil
Algae oil
Algae oil
Scheme 3. Mechanism of transesterication via acid catalysis.
[18,46]. The two fundamental methods available for algae today are
the mechanical and chemical methods. The mechanical method is
mainly expeller press or ultrasound-assisted whereas hexane solvent, soxhlet and supercritical uid extractions are the available
chemical methods. The mechanical method requires algae drying,
thus making it energy intensive whereas health and safety issues
are critical for the chemical option [18,46]. Adopting supercritical
extraction process involved the used of expensive high pressure
equipment that is also energy intensive. Industrially, a single step
process by OriginOil Company is used in wide application. The
method involved sequential steps of harvesting, concentration, and
extraction oil from algae. It separate oil, biomass and water in a
single step (mostly in less than 1 h). No chemicals or heavy
equipment is needed and the process requires no initial dewatering
of the fresh algae. Another novel method is that of Cavitation
Technologies Inc. The company's Nano-based reactor is employed
to generate cavity bubbles in the solvent [54]. Collapsing of the
bubbles close to the cell walls generates pulses that break the cell
walls to produce oils into the extraction solvent. The Catilin's
method, which is under research and development stage, would be
of great interest to the Nano-technologists. Specially developed
mesoporous nanoparticles would be employed to preferentially
extract and sequester specic fuel-based compounds in the algal
Algae oil
Microalgal's lipid
Fresh water microalgae oil
Fresh water microalgae lipids
Groundnut oil
Cotton seed oil
(fatty acid 4.34%)
Sunower oil
Yellow horn
Waste cooking oil
Palm oil
Jatropha curcas oil
Soybean oil
Chinese tallow seed oil
Croton megalocarpus oil
Waste cooking oil
Waste cooking oil
Waste cooking oil
Mutton fat
Sunower oil
ZrO2/La2O3 [16]
Cs2.5H0.5PW12O40 [16]
MgO/TiO2 [16]
CaO/Al2O3 [16]
CaO/Fe3O4 [30]
Li/MgO [30]
KF/CaO [30]
sulfated SnO2eZrO2
[30]
Zeolite Y (Y756) [31]
H3PW12O40.6H2O [31]
K3PO4 [31]
MgO/KOH [35]
NaeX zeolite [45]
Biodiesel yield/
Conversion (%)
88.10
88.30
90.20
99.00
83.00
98.00
94.70
94.27
99.50
>98
97.5
>95
>95
80
80
84.9
96.22
91.6
98.64
95
93.9
96.8
95
85
87
97.3
98
83.53
lipid feed. The free fatty acids and triglycerides rich balanced algal
oil would be transesteried into biodiesel using the T300 catalyst
developed by the company. A key important issue here is that, the
technology is potentially very efcient and involved heterogeneous
catalyst, thereby ensuring environmental sustainability, cost
reduction, catalyst reusability and high purity biodiesel and glycerol [54]. Other methods of oil extraction that are under investigation include enzymatic extraction and osmotic shock, with the
former being considered much more expensive than the hexane
extraction method. The process utilizes specic molecules of enzymes to break the cell walls with a common solvent, thereby
making fractionating the oil easier.
Demirbas and Demirbas [55] recently reported an estimate of up
to 80,000 liters per acre of algae oil. This gure exceeds 30 times the
quantity obtainable from other feedstocks like palm oil. They
showed common algae species such as Botryococcus brauni and
Schizochytrium sp. to yield up to 77% oil based on dry matter. A
model by the same authors revealed 100,000 L of oil per hectare for
algae species compared to only 446 and 952 L per hectare for soy
and sunower plants, respectively. Vazhappilly and Chen [56],
Volkman et al. [57] and Yaguchi et al. [58] have reported closer
trends. Algae oils are also known to be rich in fatty acids of the
unsaturated class. They include omega-3's, omega-6, docosahexanoic and ecosapentanoic acids. These compounds could be isolated and employed for other industrial applications, consequently
favoring economic exploitability [59,60].
After the successful oil extraction, the next step is the transesterication of the oil into biodiesel. Algae oils are basically
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
feedstocks (algae, corn, tall and soybean oils). The catalysts proved
very efcient, especially with the algae oil (Table 4). Percentage
biodiesel yields of 90.2, 88.3 and 88.1% were obtained from algae,
corn and soybean oils, respectively under constant conditions.
Similarly, the economics of the process indicated much more cost
effectiveness than with conventional homogeneous options.
Limited interference due to fatty acids was encountered. The
thermal stability of the catalysts is also very interesting for reusability purpose. Some authors [78], have recently developed a two
steps in situ process, with potentials to reduce the fatty acids
interference encountered with some heterogeneous base catalysts
and increase biodiesel yield. The method involved a preesterication of the algae oil before the base-catalyzed transesterication. It can allow biodiesel recovery up to 98%, greater
than values obtainable by a single-step catalytic in situ process.
Dong et al. [78] shows that, the heterogeneous material,
Amberlyst-15, was employed without activity decay for eight
repeated times. Catalyst loading causes increased in ester yield up
to 30 wt.%, beyond which its concentration has no any effect on the
transesterication activity. On the contrary, increasing methanol
to algae oil ratio shows the negative effect on biodiesel yield, with
optimal value obtained at a yield of 20%. The technology can
potentially play a good role as more environmentally sustainable
cost-reduced method due to the optimal biodiesel yield and
catalyst reusability. Recently, Sani et al. [79] have also reported a
range of heterogeneous solid acids such as NiOeMoO3/Al2O3, PtSAPO-11, NiOeMoO3/H-ZSM-5 and microporous titania to be
successfully employed for microalgae oil. The conversions were
generally between 83 and 99% (see Table 4), catalysts were very
stable, no corrosion or recycling problems encountered and the
materials showed potentials for reduced industrial production
costs in comparison to homogeneous systems. Generally, many
authors [25,46,80e98] have the great opinion that biodiesel production from algae or comparable non-edible feedstock via heterogeneous catalysis would be the best method for the future.
However, research should be intensied to identify what the
technical and economical feasibility by integrating economic aspects with science, technology and policy issues.
Another interesting issue is that, algae oil can similarly be
employed for production of gasoline and or diesel range hydrocarbons [99e102], animal feeds and ne chemicals [25] and even
HVO (Hydrogenated Vegetable Oil). Solid acid catalysts are the key
heterogeneous materials exploited in this respect. The general
conversion processes include cracking, hydrotreating and hydrodeoxygenation [99,103,104]. Among the solid catalysts Al2O3, AlCl3
and oxides of Ca and Mg, SAPO-5, SAPO-11 [99], HZSM5, HBEA and
USY [99,104] have been evaluated as good materials for the cracking
reactions. Heterogeneous systems such as NieMo/g-Al2O3, sulphides of NiMo and CoMo and their silica-alumina supports are
good candidates for hydrotreating of bio-oils even at low temperatures, with limited stability challenges. They have shown good
thermal stability with resistances to catalyst poisons in the reaction
feed. Alumina, zeolites and silica supported Ni and/or noble metal
catalysts are primary deoxygenation materials and could be used to
convert fatty acids in the algae oil to liquid hydrocarbons of mostly
diesel range.
Recently, Hu et al. [105] pyrolyzed oil obtained from oil-riched
blue-green algae (microcystis species) at temperatures ranging
between 300 and 700 C in a xed bed reactor. The liquid bio-oil
produced was found to be rich in gasoline and diesel range hydrocarbons, especially at the optimal temperature of 500 C. Benzene, phenols, methylphenols and heterocyclic amines like pyrrole,
indole, pyridine and substituted pyrazines were similarly detected
to signicant concentrations. Similar observations were reported
by other authors using different species [63,106e112].
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
Table 5
A summary of key industrial derivatives from glycerol [110e125].
Product
Uses
Production process
1,3-Propanediol
1,2-Propanediol
Dihydroxyacetone
Succinic Acid
Hydrogen
Polyglycerols
Polyesters
Fuels applications.
Polyhydroxyalkanoates
Syngas, methane
Polymer applications.
Fuel for energy.
Oleins
5. Glycerol conversion
Glycerol (propan-1,2,3-triol) is a simple trihydric-alcohol with
rine
, glicerol, glucerite, glycerin,
other names as alcohol glyce
rine, vegetable glycerin etc. It both occurs naturally
glycerine, glyce
and can be synthesized industrially or in the laboratories. The
compound forms the triester backbone of triglycerides (see Scheme
1) and phospholipids. Glycerol is colorless, odorless compound
widely employed as raw-material in some key industries. The three
hydroxyl groups account for considerable water solubility.
Glycerol is the key waste product produced (up to 1 kg per 10 kg
of algae oil) from biodiesel production, that has in the past been
considered a great challenge to industries [14e16,68e70,113].
However, there are progresses that the compound could be puried
and successfully converted to a number of useful industrial rawmaterials (Table 5). Initially, homogeneous catalysis was mainly
employed, but series of problems similar to those of biodiesel
synthesis have accounted for a shift to the heterogeneous method.
Hirai et al. [114] has carried out gaseous phase steam reforming
of glycerol with a range of transition metals using MgO, Y2O3, Al2O3,
ZrO2, SiO2, CeO2 and LaO3 as support materials, prepared by
employing the conventional impregnation method and reactions
monitored under atmospheric conditions. Best and promising
result was obtained with 3 wt.% Ru supported on Y2O3 at 500 C,
due to signicant resistance to deactivation by carbon deposition.
Tapah et al. [115] employed mixed Fe2O3 and Cr2O3 as catalyst and
glycerol concentrations of 2e30 wt.% at ow rates from [10e65 ml/
min] for a CSCWG (catalytic supercritical water gasication) conversion of glycerol. The results showed high temperature and low
glycerol concentrations to increased the yield and selectivity toward H2 production. Similarly, syngas of about 64 mol % was produced with minimum 4:1 mol ratio of H2:CO. Other volatile
hydrocarbons (methane and ethylene) were obtained to signicant
yields. This promotes the optional use of the technology for turbine
operations. Nearly 100% conversion of glycerol was successful at
high temperature of 550 C. Also a maximum of 11 wt.% of methanol, allyl alcohol and formaldehyde were obtained at 400 C
temperature. Catalyst stability was also studied and was found to
reach relative stability for up to 9 h of reactions. The choice of
Fig. 3. Conversion of glycerol to gaseous and intermediate liquid products via combined gasication and pyrolysis process.
Please cite this article in press as: Galadima A, Muraza O, Biodiesel production from algae by using heterogeneous catalysts: A critical review,
Energy (2014), http://dx.doi.org/10.1016/j.energy.2014.06.018
Fig. 4. Integrated routes for the conversion of glycerol, a byproduct in biodiesel plant, to fuels.
light naphtha production coupling low temperature catalytic conversion of glycerol with WGS (wateregas shift) technology and
FischereTropsch synthesis (Fig. 4). They have also reported a
number of authors have successfully converted glycerol into olens
using USY, ZSM-5, H-MOR, macroporous NieW system, Y-zeolite,
BETA and silica and alumina supports at temperatures between 300
and 650 C, yielding nearly 100% glycerol conversion and up to 60%
olens production. Zakaria et al. [121] showed the activity of Ca, Cu,
Li, Mg and Ni doped ZSM-5 zeolites characterized by FTIR, XRD and
NH3 desorption, to depends on the catalyst structureeacidity
properties during oleins and parafns production from glycerol.
Metal loadings improved HZSM-5 acidity and glycerol conversion.
Recently, Van de Vyver et al. [122], Possato et al. [123], Seran et al.
[124], Gonzalez et al. [125] and Kim et al. [126] showed the activity of
zeolites in glycerol conversion to diols and olens, to be dependent
on the structural, acidity and active metal properties. Zeolites with
low porosity produced light gaseous products, acidity enhances
conversion and metals loading promotes acidity and textural
properties thereby enhancing glycerol conversion. Table 6 presents
a further detail of various literature reports on the conversion of
Table 6
A literature report of glycerol conversions into various products over zeolites and some other solid acids.
Method/process
Catalyst system
Conversion (%)
CuZSM-5
H-ZSM-5 (29)
H-ZSM-5 (29)
Macropore NieW
USY
Cu/ZSM-5, Cr/ZSM-5, Ni/ZSM-5, Li/ZSM-5
100 [120]
35.70e80.20 [120]
91e95 [120]
100 [120]
100 [120]
100 [120]
Pt/NaY
18.1e18.4 [122]
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