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Frontiers of Environmental Science & Engineering

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Front. Environ. Sci. Eng.    2021, Vol. 15 Issue (5) : 97    https://doi.org/10.1007/s11783-020-1343-9
REVIEW ARTICLE
Application of heterogeneous catalysis to biodiesel synthesis using microalgae oil
Violeta Makareviciene(), Egle Sendzikiene, Ieva Gaide
Vytautas Magnus University, Agriculture Academy, K. Donelaicio str. 58, LT-44248 Kaunas, Lithuania
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Abstract

• Microalgae oil application for biodiesel synthesis is discussed.

• Catalytic effectiveness of ferment preparations and chemical catalyst is disputed.

• Application of heterogeneous catalysts for biodiesel synthesis is reviewed.

• Possibilities of catalyst regeneration is shown.

Recently, there is a growing interest in the use of microalga in various fields. Microalgae have properties such as rapid reproduction and high biomass accumulation, and under certain conditions, some are able to accumulate a large amount of oil. However, microalgae oil often contains more free fatty acids than the vegetable oil and is therefore unsuitable for biodiesel synthesis using alkaline catalysts. For this reason, some authors suggest the application of heterogeneous catalysis. A particular interest in the use of immobilized enzymes has developed. Other solid substances can also be used as heterogeneous catalysts are usually metal oxides, carbonates or zeolites. The use of these catalysts results in simpler biodiesel synthesis, especially purification processes, a cleaner end product and a less polluted environment. The molar ratio of alcohol to oil is lower during enzymatic transesterification, and more than 90% ester yield is obtained using a molar ratio of alcohol to oil of 3:1 to 4.5:1. The alcohols do not have a negative effect on the effectiveness of chemical catalysts, so it is possible to use alcohols in molar ratio from 4:1 to 12:1. The optimal temperature of enzymatic process is 30℃‒50℃. An ester yield of more than 95% was obtained in 12‒48 h. Using chemical catalysts, greater than a 95% yield of esters was obtained at higher temperatures in a shorter time. Material costs of enzymatic catalysis can be reduced by reusing the catalysts directly or after regeneration.
Keywords Biodiesel      Heterogeneous catalysis      Transesterification      Microalgae oil     
Corresponding Author(s): Violeta Makareviciene   
Issue Date: 24 December 2020
 Cite this article:   
Violeta Makareviciene,Egle Sendzikiene,Ieva Gaide. Application of heterogeneous catalysis to biodiesel synthesis using microalgae oil[J]. Front. Environ. Sci. Eng., 2021, 15(5): 97.
 URL:  
https://academic.hep.com.cn/fese/EN/10.1007/s11783-020-1343-9
https://academic.hep.com.cn/fese/EN/Y2021/V15/I5/97
Algae Microalgae biomass Acid value
Lipid content % Ref. Acid value
mg KOH/g		 Ref.
B. braunii FACHB 357 51.6 Cheng et al., 2013
B. braunii IPE 001 64.3 Xu et al., 2012
B. braunii Showa 30-39 Yoshimura et al., 2013
B. braunii UK 807-2 65-70 Li and Qin, 2005
Botryococcus sp. 28.6 Lee et al., 2010
C. vulgaris FACHB1068 42 Feng et al., 2011a
Chlorella vulgaris 10 Lee et al., 2010
Chlorella vulgaris 16.41 Converti et al., 2009
Chlorella vulgaris C7 56.6 Liu et al., 2008a
Chlorella vulgaris ESP-31 55.9 Yeh and Chang, 2011
Chlorella vulgaris P12 11 Anjos et al., 2013
Dunaliella tertiolecta ATCC 30929 70.6-71.4 Takagi et al., 2006 167.25 Krohn et al., 2011
Isochrysis zhangjiangensis 53 Feng et al., 2011b
Monoraphidium sp. FXY-10 51.72 Zhao et al., 2014
N. oleoabundans 40 Li et al., 2008
Nannochloris sp. UTEX LB1999 50.9 Takagi et al., 2000
Nannochloropsis oculata 15.31 Converti et al., 2009 83.4 Krohn et al., 2011
Nannochloropsis sp. 59.9 Jiang et al., 2011 6.5 Chen et al., 2012
Neochloris oleabundans UTEX 1185 56 Gouveia et al., 2009a
Pond water algae 0.4 Nautiyal et al., 2014
Porphyridium cruentum 8 Biller and Ross, 2011
Scenedesmus obliquus CNW-N 22.4 Ho et al., 2012
Scenedesmus sp. 10 Lee et al., 2010 8.7 Chen et al., 2012
Scenedesmus sp. LX1 53 Xin et al., 2010
Spirulina 0.45 Nautiyal et al., 2014
Tetraselmis subcordiformis 29.77 Huang et al., 2013
Tab.1  Lipid content of microalgae biomass and acid value of microalgae oil
Fatty
acid		 Content %
Rapeseed1 Ankistrodesmus fusiformis2 Butyrococcus braunii2 Chlorella sp.1 Chlorella vulgaris2 Chlamidomonas sp.2 Haematococcus sp.1 Nanochloropsos sp.3 Nannochloris sp.1 Scenedesmus sp.1 Spirulina maxima3 Micractinium sp. IC-764
Saturated: 5.40 37.33 9.85 36.91 49.46 78.61 18.78 30.96 14.27 22.81 41.68 32,5
C14:0 Myristic ? 2.02 0.73 0.31 0.63 1.61 0.23 7.16 ? 0.73 0.34 2.2
C16:0 Palmitic 3.22 26.95 7.17 31.09 40.31 50.7 9.78 23.35 8.62 17.17 40.16 28.1
C17:0 Margaric 0.47 0.51 1.55 0.93 0.51
C18:0 Stearic 2.18 2.01 1.59 4.11 8.01 11.54 3.99 0.45 2.81 2.87 1.18 2.2
C20:0 Arachidic 0.57 1.37 0.73 0.44 0.06
C22:0 Behenic 0.24 1.81 1.09 0.92
C24:0 Lignoceric 2.22 0.06 0.1 3.17
Unsaturated: 94.60 52.63 90.15 63.09 45.02 21.39 81.24 59.20 85.74 77.19 51.9 67.5
C16:1 Palmitoleic 0.25 2.28 3.16 0.28 1.66 26.87 1.00 12.05 9.19 3.5
C18:1 Oleic 16.92 19.61 77.22 43.01 29.8 7.82 49.43 13.20 62.35 41.95 5.43 12.4
C18:2 Linoleic 66.32 12.23 5.16 10.95 8.54 3.93 13.67 1.21 12.72 13.02 17.89 29.2
C18:3 Linolenic 11.14 26.50 1.57 6.03 1.57 0.82 10.94 5.44 17.97 4.9
C 20:1 Gadoleic 0.51 1.95 4.59 2.12 1.11
C22:1 Erucic 0.22 0.24 0.83 0.62 0.20
C24:1 Nervonic 0.02 0.12 1.49 0.89
Tab.2  Composition of fatty acids for the given types of microalgae oil compared to rape oil
Fig.1  Principal technological scheme of biodiesel production from microalgae biomass.
Fig.2  Transesterification reaction of triglycerides (a) and esterification reaction of free fatty acids (b).
Solvent Conversion efficiency (%)
Acetone 53.05
1-butanol 11.36
t-butanol 79.69
Dichlormethane 19.78
Ether 71.25
Ethyl acetate 20.66
Hexane 51.81
Isopropanol 39.19
MTBE 77.66
Pyridine 6.98
Tab.3  Efficiency of solvent use in enzymatic catalysis
Catalyst Solvent Acyl receptor Optimal conditions Yield (%) Ref.
Lipolase 100L ? Ethanol Ethanol to oil molar ratio 3:1, 30°C, 26 h, 10% of enzyme 96.9 Makareviciene et al., 2017
Lipozyme TL IM Diesel fuel Ethanol Ethanol to oil molar ratio 4.5:1, 30°C, 13 h, 13.3% of enzyme 98 Gumbyte et al., 2018
Candida antarctica t-butanol Methanol Methanol to oil molar ratio 12:1; oil and t-butanol ratio 1:1 (w/v), oil and lipase mass ratio 20:1; 40°C, 12 h, 250 r/min >97 Wu et al., 2017
Candida sp. 99?125 and immobilized
by physical absorption onto macroporous resins		 Methanol Methanol 30% of lipase, 10% of water, methanol to oil molar ratio 3:1, 38°C, pH 7, 12 h 98.15 Xiong et al., 2008
Candida sp. Hexane Methanol (stepwise) Methanol to oil molar ratio 3:1, 38°C, 12 h., 75% of enzyme 98.2 Li, et al., 2007
Penicillium expansum lipase [BMIm][PF6] Methanol Methanol to oil molar ratio 4:1, 50°C, 48 h., 20% of enzyme 90.7 Lai et al., 2012a
Candida sp.
Novozyme 435		 Dimethyl carbonate Dimethyl carbonate 50% of lipase, 60°C, 6 h 75.5 Lee et al., 2013
Tab.4  Optimal conditions of enzymatic microalgae oil transesterification (Makareviciene and Skorupskaite, 2019)
Fig.3  Possible chemical heterogeneous catalysts for biodiesel synthesis.
Catalyst Amount (%) Temperature (°C) Yield (%) Ref.
CaOAl2O3 1.56 50 88.9 Narula et al., 2017
Mg–Zr solid base catalyst 10 65 28 Li et al., 2011
KF/CaO catalysts with different KF loadings 12 60 93.07 Ma et al., 2015
Cr2O3/Na2Cr2O3/Al2O3 20 80 98.28 Guldhe et al.,2017a
Tungstated zirconium oxide (WO3/ZrO2) 15 100 94.58 Guldhe et al., 2017b
Amberlyst-15 30 90 >98 Dong et al., 2013
Acid resins:
CT-269
CT-275
Amberlite 15
KSF klay
Silica-alumina		 0.8 (M) 100 >90
67
18.2		 Carrero et al., 2015
Tab.5  Heterogeneous catalysts used for microalgae oil transesterification and process conditions (Makareviciene and Skorupskaite, 2019)
Catalyst Amount (%) Temperature (°C) Pressure (kPa) Yield (%) Ref.
NiO, MoO3/Al2O3 4 370 5000 99 Verma et al., 2011
18
NiO, MoO3/H-ZSM-5 5 375 1000 83 Verma et al., 2011
18
Microporous titania Continues 340 15513.78 31 Krohn et al., 2011
(HY-340) niobium oxide 10 200 20684.27 94.27 Reyes et al., 2012
Tab.6  Findings from studies on biodiesel synthesis from microalgae oil under supercritical conditions using heterocatalysts
Catalyst Fatty raw material Transesterification agent Preparation of catalyst for reuse No of cycles Ref.
Novozym 435 Soybean oil Methanol ? 1 Du et al., 2004
Novozym 435 Insect fat Methanol Recovered Novozym 435 was immersed in tert-butanol for its regeneration, followed by washing with insect fat for the removal of tert-butanol on the catalyst 20 Nguyen et al., 2017
Novozym 435 Soybean oil Three-step methanolysis 25 Watanabe et al., 2002
Novozym 435 Vegetable oil Two-step methanolysis 70 Shimada et al., 2002
Novozym 435 Vegetable oil Three-step methanolysis 50-52 Shimada et al., 2002, Shimada et al., 1999
Novozym 435 Fish oil Ethanol 10 Suárez et al. 2019
Novozym 435 Tuna oil Two-step ethanolysis 37 Shimada et al., 2002
Novozym 435 Tuna oil Three-step ethanolysis 54 Shimada et al., 2002
Novozym 435 Soybean oil Methyl acetate 100 Du et al., 2004
Rhodotorula mucilaginosa MTCC8737 Chlorella salina oil Methyl acetate 10 Surendhiran, et al., 2014
Novozym 435 Insect fat Methyl acetate 20 Nguyen et al., 2018
Novozym-435 Crude jatropha oil Ethyl acetate 12 Modi et al., 2007
Novozym 435 Soybean oil Methanol ultrasonic waves 5 Yu et al., 2010
Tab.7  Multiple reuse of biocatalysts in biodiesel synthesis
Catalyst Fatty raw material Preparation of catalyst for reuse No of cycles Ref.
Nanocrystalline CaO Soyabean oil ? 8 Reddy et. al., 2006
Nanocrystalline CaO Poultry fat ? 3 Reddy et. al., 2006
CaO Sunflower oil ? 8 Granados et. al., 2007
CaO Palm olein ? 5 Yoosuk et. al., 2010
CaO Soyabean oil 20 Liu et al., 2008 b
Ca(OCH3)2 Soyabean oil ? 20 Liu et. al., 2008 b
KOH/NaX Soyabean oil Washing with cyclohexane and heating at 398 K for 2h 1 Xie et. al., 2007
KOH/NaX Soyabean oil Washing with cyclohexane and heating at 398 K for 2h, impregnation with 5% KOH 1 Xie et. al., 2007
Mg2CoAl Canola oil Filtration and drying at 100°C 7 Li, et al., 2009
Na/SiO2 Jatropha curcus oil Washing with methanol and drying at 100°C for 2 h 5 Kumar, et al., 2010
Dolomite Canola oil ? 3 Ilgen, 2011
Dolomite Sanflower oil ? 2 Sendzikiene et al., 2018
Dolomite Palm kernel oil Centrifugation and washing with methanol 7 Ngamcharussrivichai et al., 2010
waste eggshell Soyabean oil ? 13 Wei et al., 2009
Starch-derived solid acid catalyst Waste cooking oils ? 50 Lou et al., 2008
Tab.8  Multiple uses of chemical/natural catalysts in biodiesel synthesis
Homogeneous catalysis Heterogeneous catalysis
Chemical Enzymatic
Advantages Disadvantages Advantages Disadvantages Advantages Disadvantages
High process rate and yield Sensitivity to moisture and a larger amount of free fatty acids in raw materials Possibility to regenerate or reuse the catalyst Average process speed Water and free fatty acids contained in raw materials have no negative impact on process efficiency Average process speed, long duration
Ability to use excess of alcohol Corrosive environment Easy separation of esters, clean glycerol non-contaminated with salts Possibility to regenerate or reuse the catalyst Inactivation of ferment preparations by alcohols
Low cost of catalysts Impossibility to regenerate or reuse the catalyst Stability of catalysts effectiveness Easy separation of esters, clean glycerol non-contaminated with salts Require high amount of catalysts
Difficult cleaning and purification of the product or alcohol regeneration Low cost of catalysts Low process temperature High material costs associated with the high cost of enzymatic catalysts
Difficulty of application of an continues process Ability to use excess of alcohol
Quite high energy consumption and material expenses Quite low energy consumption and material expenses
Tab.9  Comparison of homogeneous and heterogeneous catalysis
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