Biodiesel synthesis from Hevea brasiliensis oil employing carbon supported heterogeneous catalyst: Optimization by Taguchi method

The present work illustrates the parametric effects on biodiesel production from Hevea brasiliensis oil (HBO) using flamboyant pods derived carbonaceous heterogeneous catalyst. Activated carbon (AC) was prepared maintaining 500 °C for 1 h and steam activated at optimised values of activation time 1.5 h and temperature 350 °C. Carbonaceous support was impregnated with KOH at different AC/KOH ratios. The transesterification process was optimized and significant parameters affecting the biodiesel yield was identified by Taguchi method considering four parameters viz. reaction time, reaction temperature, methanol to oil ratio and catalyst loading. The physicochemical properties of Hevea brasiliensis methyl ester (HBME) were examined experimentally at optimised condition and found to meet the global American standards for testing and materials (ASTM). The optimum condition observed to yield 89.81% of biodiesel were: reaction time 60 min, reaction temperature 55 °C, catalyst loading 3.5wt% and methanol to oil ratio 15:1. Contribution factor revealed that among four parameters considered, catalyst loading and methanol to oil ratio have more prominent effect on biodiesel yield. The cost for preparing carbonaceous catalyst support was estimated and observed to be fairly impressive. Thus, Hevea brasiliensis oil (HBO) could be considered as suitable feedstock and flamboyant pods derived carbon as effective catalyst for production of biodiesel.     

Waste capiz (Amusium cristatum) shell as a new heterogeneous catalyst for biodiesel production

The waste Capiz shell was utilized as raw material for catalyst production for biodiesel preparation. During calcination process, the calcium carbonate content in the waste capiz shell was converted to CaO. This calcium oxide was used as catalyst for transesterification reaction between palm oil and methanol to produce biodiesel. The biodiesel preparation was conducted under the following conditions: the mole ration between methanol and palm oil was 8:1, stirring speed was 700 rpm, and reaction temperature was 60 °C for 4, 5, and 6 h reaction time. The amount of catalyst was varied at 1, 2, 3, 4, and 5 wt %. The maximum yield of biodiesel was 93 ± 2.2%, obtained at 6 h of reaction time and 3 wt % of amount of catalyst. In order to examine the reusability of catalyst developed from waste of capiz (Amusium cristatum) shell, three transesterification reaction cycles were also performed.     

Synthesis and characterisation of rubber seed oil trans-esterified biodiesel using cement clinker catalysts

The synthesis of biodiesel using rubber seed oil by a transesterification reaction using cement clinker catalysts was studied. The mineral composition and morphology of both the catalysts were analysed using X-ray diffraction and scanning electron microscopy. The gas chromatography–mass spectrometry, Fourier transform infrared spectroscopy and nuclear magnetic resonance studies were used to find the Fatty acid methyl ester content and various compounds of esters in the synthesised biodiesel, which showed an efficient conversion of rubber seed oil to biodiesel. The highest yield of 80% was obtained from calcium oxide catalyst (1.5?g) activated at 50°C with a methanol-to-oil ratio of 6:1. The highest yield of 70% biodiesel was obtained using a cement clinker catalyst (0.5?g) activated at 50°C with a methanol-to-oil ratio of 6:1. The significant physical properties of biodiesel flash point, acid value and saponification value were found, and the results are within the American standard test method (ASTM D6751) limits.     

Biodiesel fuel production with solid amorphous-zirconia catalysis in fixed bed reactor

Amorphous zirconia catalysts, titanium-, aluminum-, and potassium-doped zirconias, were prepared and evaluated in the transesterification of soybean oil with methanol at 250 °C, and the esterification of n-octanoic acid with methanol at 175–200 °C. Titanium- and aluminum-doped zirconias are promising solid catalysts for the production of biodiesel fuels from soybean oil because of their high performance, with over 95% conversion in both of the esterifications.     

Manufacturing of zeolite based catalyst from zeolite tuft for biodiesel production from waste sunflower oil

In the present work, zeolite based catalyst was prepared from zeolite tuft by impregnation methods. The zeolite tuft was initially treated with hydrochloric acid (16%) and then several KOH/zeolite catalysts were prepared by impregnation in KOH solutions. Various solutions of KOH with different molarities (1–6 M) were used. Further modification for the catalyst was performed by a 2nd step impregnation treatment by heating and stirring the KOH/zeolite to 80 °C for 4 h. The zeolite tuft and the prepared catalysts were characterized by several analytical techniques in order to explore their physicochemical properties. These tests include: X-Ray Fluorescence (XRF), Scanning Electron Microscopy (SEM), Zero point of Charge (PHzpc), Fourier Transform Infrared (FT-IR), Energy-dispersive X-Ray analysis (EDX) and X-Ray Diffraction (XRD). The catalysts were then used for transesterification of waste sunflower vegetable oil in order to produce biodiesel. Among the different catalysts prepared, the 1–4M KOH/TZT catalyst provided the maximum biodiesel yield of 96.7% at 50 °C reaction temperature, methanol to oil molar ratio of 11.5:1, agitation speed of 800 rpm, 335 μm catalyst particle size and 2 h reaction time. The physicochemical properties of the produced biodiesel comply with the EN and ASTM standard specifications.     

Alkaline-catalyzed transesterification of Silurus triostegus Heckel fish oil: Optimization of transesterification parameters

The present work reports the production of biodiesel from Silurus triostegus Heckel fish oil (STFO) through alkaline-catalyzed transesterification by using potassium hydroxide (KOH) as an alkaline catalyst with methanol. Chemical and physical properties of the extracted oil were determined. It was found that STFO has a low acid value (1.90 mg KOH/g oil); hence no pre-treatment such as acid esterification is required to produce the biodiesel. The influence of the experimental parameters such as KOH concentration (0.25–1.0% w/w of oil), methanol to oil molar ratio (3:1, 6:1, 9:1 and 12:1), reaction temperature (32, 45 and 60 °C), reaction duration (30, 60, 90 and 120 min), type of the catalyst (potassium or sodium hydroxide) and step multiplicity (single- and two-step transesterification) on the yield of the biodiesel were investigated. The maximum biodiesel yield (96%) was obtained under the optimized parameters of the transesterification (KOH 0.50% w/w, 6:1 methanol to oil, at 32 °C for 60 min). The properties of the produced biodiesel were found to conform with the ASTM standard, indicating its suitability for internal combustion engines. Blending of the produced biodiesel with petro diesel with various volume percentages was investigated as well.     

Comparison and effect of Cinder supported with Manganese and Lanthanum oxide for biodiesel production

In this study, comparison and effect of Cinder supported with Lanthanum and Manganese oxide as catalyst for transesterification of triglyceride to methyl ester is proposed. The reaction mechanism along with the effects of methanol to oil molar ratio, amount of catalyst to oil, reaction temperature were also discussed. Moreover reusability of catalyst, catalyst resistance toward Free Fatty Acid and water were also discussed. The results show that yield of biodiesel produced with Mn:La:Cinder catalyst was 99% at ≥150 °C in 6 h. Cinder supported with Mn shows conversion of triglycerides from soybean oil in reaction with methanol after 6 h was over 99% at 150 °C. For both catalyst 3wt% of catalyst based on oil, 24:1 methanol/oil molar ratio was reused for 7 times with regeneration. The catalysts displayed great resistance toward 2.5% water and 1% wt fatty acids.     

Biodiesel production from refined sunflower vegetable oil over KOH/ZSM5 catalysts

ZSM5 zeolite was impregnated with different KOH loadings (15 wt.%, 25 wt.% and 35 wt.%) to prepare a series of KOH/ZSM5 catalysts. The catalysts were calcined at 500 °C for 3 h and then characterized by N₂ adsorption–desorption and X-ray diffraction (XRD) techniques. The catalysts were tested in the transesterification reaction in a batch reactor at 60 °C and under atmospheric pressure. It was found that KOH/ZSM5 with 35 wt.% loading showed the best catalytic performance. The best reaction conditions in the presence of KOH/ZSM5 (35 wt.%) were determined while modifying the catalyst to oil ratio and the reaction time. The highest methyl ester yield (>95%) was obtained for a reaction time of 24 h, a catalyst to oil ratio of 18 wt.%, and a methanol to oil molar ratio of 12:1. The properties of produced biodiesel complied with the ASTM specifications. The catalytic stability test showed that 35KOH/ZSM5 was stable for 3 consecutive runs. Characterization of the spent catalyst indicated that a slight deactivation might be due to the leaching of potassium oxides active sites.     

A bronsted basic ionic liquid as an efficient and environmentally benign catalyst for biodiesel synthesis from soybean oil and methanol

Morpholine basic ionic liquid was synthesized with N-methyl morpholine, N-butyl bromide, and KOH by two-step method and was used to catalyze the transesterification of soybean oil with methanol to biodiesel. The structure of the catalyst were examined by ¹H nuclear magnetic resonance. The effects of the molar ratio of methanol to oil, reaction temperature, and amount of catalyst on the biodiesel yield were investigated. Optimized biodiesel yield of 94.5% was achieved with catalyst amount of 3.0 wt%, and methanol to soybean oil molar ratio of 14:1 at reaction temperature of 60 °C for 6 h. The catalyst has maintained sustained activity after being employed to six cycles. The prepared biodiesel component was analyzed by gas chromatography-mass spectrometry (GC-MS) and the results showed that the biodiesel comprised of hexadecanoic acid methyl ester, 10, 13-octadecadienoic acid methyl ester, 9-octadecenoic acid methyl ester, and octadecanoic acid methyl ester, illustrating that fatty acids of soybean oil were converted completely.     

Biodiesel production from soybean and Jatropha oils using cesium impregnated sodium zirconate as a heterogeneous base catalyst

Cesium modified sodium zirconate (Cs-Na₂ZrO₃) was prepared by ionic exchange from sodium zirconate (Na₂ZrO₃), which was synthesized via a solid state reaction. Both ceramics, i.e., pristine Na₂ZrO₃ and the Cs-Na₂ZrO₃, were used as basic heterogeneous catalysts in biodiesel production. Soybean and Jatropha oils were used as triglyceride sources for transesterification reactions. Parameters, such as catalyst concentration (between 0.5 and 3 wt%), reaction time, different methanol/vegetable oil molar ratios, and temperature of the reaction, were evaluated. The cesium cation influence was evaluated from the basic transesterification reactivity. The results showed that the introduction of cesium significantly modified the catalytic activity in biodiesel production. Cs enhanced the reaction kinetics in obtaining biodiesel and reduced the reaction time in comparison with pristine Na₂ZrO₃. The results showed that Cs-Na₂ZrO₃ as a basic heterogeneous catalyst exhibited the best fatty acid methyl esters (FAME) conversion for soybean oil (98.8%) at 1 wt%, 30:1 methanol/oil ratio, 65 °C, and 15 min. The best conditions for Jatropha oil (90.8%) were 3 wt%, 15:1 methanol/oil ratio, 65 °C, and 1 h. The impregnation of Na₂ZrO₃ with cesium represents a very exciting alternative heterogeneous base catalyst for biodiesel production.     

Optimization of biodiesel production from waste fish oil

The present study deals with the production of biodiesel using waste fish oil. The research assesses the effect of the transesterification parameters on the biodiesel yield and its properties, including temperature (40–60 °C), molar ratio methanol to oil (3:1–9:1) and reaction time (30–90 min). The experimental results were fitted to complete quadratic models and optimized by response surface methodology. All the biodiesel samples presented a FAME content higher than 93 wt.% with a maximum, 95.39 wt.%, at 60 °C, 9:1 of methanol to oil ratio and 90 min. On the other hand, a maximum biodiesel yield was found at the same methanol to oil ratio and reaction time conditions but at lower temperature, 40 °C, which reduced the saponification of triglycerides by the alkaline catalyst employed. Adequate values of kinematic viscosity (measured at 30 °C) were obtained, with a minimum of 6.30 mm²/s obtained at 60 °C, 5.15:1 of methanol to oil ratio and 55.52 min. However, the oxidative stability of the biodiesels produced must be further improved by adding antioxidants because low values of IP, below 2.22 h, were obtained. Finally, satisfactory values of completion of melt onset temperature, ranging from 3.31 °C to 3.83 °C, were measured.     

Production of biodiesel from castor oil using iron (II) doped zinc oxide nanocatalyst

The depletion of fossil fuels has caused the price of petroleum to rise remarkably and created need for alternative energy such as biodiesel. In the present study, the biodiesel was produced from castor oil using ferromagnetic zinc oxide nanocomposite as heterogeneous catalyst for transesterification reaction. Single phase of nanocatalyst were confirmed by X-Ray Diffraction analysis. The spherical shape of the aggregated nanocatalyst was observed in Scanning Electron Microscopy. Magnetic properties were analysed using vibrating sample magnetometer. Atomic Force Microscopic analysis revealed the larger surface area and roughness of nanocatalyst. The biodiesel yield of 91% (w/w) was obtained in 50 min at 55 °C with 14 wt % catalyst loading and 12:1 methanol/oil ratio and was confirmed by Gas chromatograph with Mass Spectrometer. The result showed that the iron (II) doped ZnO nanocatalyst is a promising catalyst for the production of biodiesel via heterogeneous catalytic transesterification under milder reaction conditions.     

A comparative study of KOH/Al2O3 and KOH/NaY catalysts for biodiesel production via transesterification from palm oil

The transesterification of palm oil to methyl esters (biodiesel) was studied using KOH loaded on Al₂O₃ and NaY zeolite supports as heterogeneous catalysts. Reaction parameters such as reaction time, wt% KOH loading, molar ratio of oil to methanol, and amount of catalyst were optimized for the production of biodiesel. The 25 wt% KOH/Al₂O₃ and 10 wt% KOH/NaY catalysts are suggested here to be the best formula due to their biodiesel yield of 91.07% at temperatures below 70 °C within 2–3 h at a 1:15 molar ratio of palm oil to methanol and a catalyst amount of 3–6 wt%. The leaching of potassium species in both spent catalysts was observed. The amount of leached potassium species of the KOH/Al₂O₃ was somewhat higher compared to that of the KOH/NaY catalyst. The prepared catalysts were characterized by using several techniques such as XRD, BET, TPD, and XRF.     

A bone-based catalyst for biodiesel production from waste cooking oil

Biodiesel production via transesterification of waste cooking oil (WCO) with methanol using waste chicken bone-derived catalyst was investigated. The calcium carbonate content in the waste chicken bone was converted to calcium oxide (CaO) at a calcinations temperature of 800°C. The catalysts were prepared by calcination at 300–800°C for 5 h and catalyst characterization was carried out by X-ray diffraction (XRD) and Brunauer–Emmett–Teller (BET) surface area measurement. CaO was used as catalyst for biodiesel production. The results of the optimization imply that the catalyst concentration of 3.0 wt%, methanol to oil ratio of 3:1, and reaction temperature of 80°C for 3 h provide the maximum values of yield in methyl ester production. Reusability of the catalyst from calcined waste chicken bone was studied for four times, with a good yield.     

A novel one-pot synthesis of tetragonal sulfated zirconia catalyst with high activity for biodiesel production from the transesterification of soybean oil

A sulfated zirconia catalyst has been prepared by a novel one-pot vapor-controlled synthesis route using ammonium persulphate as sulfate agent. A possible formation mechanism of the catalyst is proposed. The effect of calcination temperature and S/Zr molar ratio on the structural, textural and catalytic properties of the prepared catalyst were investigated in detail using X-ray diffraction (XRD), N₂ adsorption–desorption, ammonia temperature programmed desorption (NH₃-TPD), Fourier transform infrared spectroscopy (FTIR) and a scanning electron microscope (SEM) which was equipped with an energy dispersive spectroscope (EDS). The results indicated that the samples calcined at 500 °C possessed zirconia of pure tetragonal structure, more content of sulfur and better distribution of acid sites on the surface of zirconia compared with the samples calcined at 600  °C at fixed S/Zr molar ratio. Moreover, they showed excellent catalytic activity with 100% yields of biodiesel for the transesterification of soybean oil with methanol.     

Catalytic performance of a novel amphiphilic alkaline ionic liquid for biodiesel production: Influence of basicity and conductivity

Three novel alkaline guanidine ionic liquids as amphiphilic catalysts have been successfully synthesized for two-phase transesterification, which can efficiently improve the catalytic activity for the synthesis of biodiesel. They were characterized by a series of techniques including ¹H NMR, thermal stability, electronegativity (DFT calculation), basicity and conductivity. It was demonstrated that 1,1,3,3-trimethyl-2-octyl-guanidine hydroxide(IL3) exhibited better catalytic activity compared with other base guanidine ionic liquid catalysts, which was related to the better basicity and electronegativity of the ILs. The experimental results indicated that catalytic performance was relative to both enough alkaline center and conductivity of ionic liquid catalysts, but the former was a main factor in the catalytic system. The catalytic performance also revealed that optimum catalyst dosage was about 6 wt.%, the appropriate reaction temperature was about 55 °C, the optimum n(Methanol)/n(Soybean Oil) for the biodiesel synthesis was about 15:1 and the suitable reaction time was 4 h on the basis of biodiesel yield of 97%. In addition, the reaction mechanism of the amphiphilic catalyst was illuminated by the interaction between the methoxyl group and the carbonyl group of the triglyceride after activating for two-phase transesterification.     

Preparation, characterization and application of heterogeneous solid base catalyst for biodiesel production from soybean oil

A solid base catalyst was prepared by neodymium oxide loaded with potassium hydroxide and investigated for transesterification of soybean oil with methanol to biodiesel. After loading KOH of 30 wt.% on neodymium oxide followed by calcination at 600 °C, the catalyst gave the highest basicity and the best catalytic activity for this reaction. The obtained catalyst was characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning electron microscopy (SEM), Thermogravimetric analysis (TGA), N₂ adsorption-desorption measurements and the Hammett indicator method. The catalyst has longer lifetime and maintained sustained activity after being used for five times, and were noncorrosive and environmentally benign. The separate effects of the molar ratio of methanol to oil, reaction temperature, mass ratio of catalyst to oil and reaction time were investigated. The experimental results showed that a 14:1 M ratio of methanol to oil, addition of 6.0% catalyst, 60 °C reaction temperature and 1.5 h reaction time gave the best results and the biodiesel yield of 92.41% was achieved. The properties of obtained biodiesel are close to commercial diesel fuel and is rated as a realistic fuel as an alternative to diesel.     

Analysis and evaluation of operating variables for the yield of Karanja and neem oil-based biodiesel production

The aim of this research is to present the possibilities of the use of non-edible oils in biodiesel production, to consider the various methods for treatment of non-edible oils and to emphasise the influence of the operating and reaction conditions on the process rate and the ester yield. Because of biodegradability and non-toxicity biodiesel has become more attractive as alternative fuel. Biodiesel is produced mainly from vegetable oils by transesterification. For economic and social reasons, edible oils should be replaced by lower-cost and reliable feedstock for biodiesel production, such as non-edible plant oils. In this work biodiesel is produced from neem and Karanja by using butanol, propanol, ethanol and methanol as alcohols and KOH and NaOH as alkali catalysts by the transesterification process. The aim of this research is to analyse the different reaction parameters such as catalyst concentration, type of catalyst, types of alcohol, alcohol to oil molar ratio, reaction time and reaction temperature on the yield of biodiesel from non-edible oils. The maximum yield obtained was 95% with Karanja as oil with methanol and KOH as alkali catalyst at oil to alcohol molar ratio of 6:1 in 1 h at 60°C. Special attention is paid to the possibilities of producing biodiesel from non-edible oils.     

Ethanolysis of waste cottonseed oil over lithium impregnated calcium oxide: Kinetics and reusability studies

A series of Li/CaO catalysts has been prepared by impregnating 0.5–5.0 wt% Li in CaO by wet chemical method. Prepared Li/CaO catalysts have been characterized by powder X-ray diffraction, scanning electron and transmission electron microscopy and Brunauer–Emmett–Teller (BET) surface area studies, in order to establish the structure and surface morphology of the catalyst. Hammett indicator test study was performed to determine the basic strength of the Li/CaO catalysts. The prepared Li/CaO catalysts have been employed as a heterogeneous catalyst for the transesterification of waste cottonseed oil (having 2.8 wt% free fatty acid contents) with ethanol. Under optimal reaction conditions viz., ethanol/oil molar ratio of 12:1, catalyst to oil weight fraction of 5% and 65 °C reaction temperature, 98% fatty acid ethyl ester yield was obtained in 2.5 h of reaction duration. Under the optimized reaction conditions, the pseudo first order constant and Arrhenius activation energy were found to be 0.03 min⁻¹ and 70.0 kJ mol⁻¹, respectively. Further Li/CaO catalyst was also found to be effective for the ethanolysis and methanolysis of vegetable oils having up to 3.4 wt% free fatty acids. The use of 3-Li/CaO catalyst is advantageous considering that it not only utilizes waste cottonseed oil as a feedstock, but also renewable and nontoxic alcohol, ethanol, for the biodiesel production.     

Improved transesterification of waste cooking oil into biodiesel using calcined goat bone as a catalyst

In this study, potassium hydroxide-treated animal bones were employed? as a solid heterogeneous catalyst in transesterification of waste cooking oil. This catalyst was characterized by the Fourier-transform infrared spectroscopy (FTIR), and it displayed high-catalytic activity for biodiesel production. Optimum conditions for biodiesel production were catalyst loading 6.0% (w/w) of oil, methanol/oil molar ratio 9:1, calcination temperature 800°C, reaction temperature 65°C, and reaction time of 5 h, which gave maximum biodiesel yield of 84%. Reusability of the catalyst was also confirmed by repeated use of the same catalyst three times without losing much of its activity. Hence, calcined goat bones were found to be a potentially applicable catalyst for biodiesel production at industrial scale.