Catalytic Hydrocracking of Jatropha Oil for Bio-jetfuel Production using natural clay

doi:10.21203/rs.3.rs-2956399/v1

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Catalytic Hydrocracking of Jatropha Oil for Bio-jetfuel Production using natural clay

https://doi.org/10.21203/rs.3.rs-2956399/v1

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published 17 Aug, 2023

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Biofuels such as biodiesel and bio-jet fuel are‏ important sources of renewable energy, which has to be added to petroleum fuels in different ratios for environmental purposes. Biofuels in general, can be produced from several raw agriculture materials. Currently, the most important biofuel is the bio-jet fuel, used for partial replacement of jet fuel from petroleum origin. The most promising method for bio-jet fuel manufacture is the catalytic hydrocracking of a low-cost raw vegetable oil such as non-edible Jatropha oil. The type of product and its quality and quantity depend on the process conditions such as reaction time, temperature, and catalyst type, form, and amount. Heterogeneous catalysts play an important role in this process. The present study aims to the production of bio-jet fuel by hydrocracking of Jatropha oil conforming to ASTM specifications by the selection and preparation of an economic inorganic catalyst. The 4% catalyst was used in the production of biojet fuel under the obtained optimum operating conditions of 350˚C, 4 bar H₂, 18 min, and followed by fractionation tower. The products were tested and their specifications conformed to the ASTM specifications, viz the freezing point (-56˚C), the flash point (53˚C), and existent gum content (5.9 mg/100 ml).

Physical sciences/Engineering/Chemical engineering

Earth and environmental sciences/Environmental social sciences/Climate change mitigation

Bio-jet fuel

catalytic hydrocracking

inorganic catalyst

nonedible oils

Jatropha oil

natural clay.

Several challenges face the demand and supply of energy in the world. The increase in petroleum fuel consumption worldwide affects fossil fuel reserves. The daily global total consumption of petroleum reached 99.56 million barrels in 2022. The estimated petroleum oil reserves will be drained in less than fifty years, at the current consumption rate of 2.7% annually [1, 2]. Also, the emissions that are exhausted from fossil fuels combustion are large contributors to global warming and environmental pollution[3–5]. Environmental awareness, depletion of fossil fuels and the increase in energy consumption and price‏ are the main factors leading to the search for alternative energy resources to substitute fossil‏ fuels[4, 6–8].

Renewable energy sources decrease the effect of greenhouse gases and are superior to fossil fuels with respect to their lower SO_x, CO, and CO₂ emissions[9]. Representative renewable energy source technologies include fuel‏ cells, hydropower, solar power, geothermal energy, wind power, biofuel, and hydrogen production[10, 11].

Biojetfuel is‏ one of the most important sources of renewable and green energy expected to gradually replace fossil fuels in the near future with increased blending ratios. It is anticipated to reach 25% in 2020, 30% in 2030, and 50% in 2050[12–15]. Biofuels can be produced from several agricultural raw materials, through different production methods depending on the required final products and feedstock[16]. These are mainly vegetable oil based and biomass. Vegetable oil-based feedstock includes edible and non-edible oils, waste cooking oil, jatropha, jojoba, rapeseed, castor and microalgal oil. Biomass feedstock includes waste materials, aquatic biomass, energy crops, and forest products [9, 10, 14, 17].

Biofuel production processes range between catalytic cracking, pyrolysis, transesterification, and fermentation[18]. Using the proper catalyst, hydrocracking is one of the best routes to produce biofuels from oils. This is due to many reasons firstly, the catalytic hydrocracking operating temperature range of (350–450˚C) is lower than pyrolysis temperatures of (500–850˚C), also the choice of feedstock used in pyrolysis plays a significant role in the quality of the final product. Secondly, the reaction time of the catalytic hydrocracking process is much shorter than that required in the fermentation process. Production of ethanol via fermentation necessitates pretreatment processes such saccharification and hydrolysis. Finally, catalytic hydrocracking can produce several fractions of petroleum cuts such as gasoline, kerosene, diesel, and mazot compared to the transesterification method that produces only biodiesel[19–21].

Bio-kerosene or bio-jet fuel, used mainly in air transportation, is one type of biofuel having the same characteristics of jet-fuel according to ASTM and contains the same components. There are two types of jet-fuel: civil aviation (Jet A, Jet A-1, Jet B) and military jet fuels "(JP.1- JP.10, JPTS, Zip fuel, Syntroleum)[9, 13, 14]. These are produced by different processes based on the feedstock which could either be a gas, sugar, alcohol, or oil[22]. The catalytic hydrocracking process is considered the best choice to convert vegetable oil to bio-jet fuel in one step[15].

The catalytic hydrocracking of "non-edible and edible oils" demands the development of the appropriate cracking catalysts and the selection of the proper reactors for the production of bio-jet fuel[23–25]. The aim of this work is the production of bio-jet fuel through hydrocracking of Jatropha oil by using prepared inorganic catalysts from natural clay. Catalyst characterization will be undertaken and the reaction products will be evaluated for each catalyst type. Comparison between the conventional jet fuel and the produced bio-jet fuel will be undertaken by chemical and physical analyses to verify the bio-jet fuel conformity to ASTM specifications.

2.1. Materials

The used catalyst The Egyptian Bentonite B is obtained from Borg El Arab, Alexandria, Egypt. It comes from Egyptian quarries and it is used in the manufacture of ceramics, pottery and handicrafts. Jatropha Curcas seeds were obtained from the Ministry of Agriculture and from Jatropha which is growing successfully in Egypt and can be cultivated arid land and using municipal waste water primary treated, in many places in Egypt. Hydrochloric acid HCl was purchased from Sigma – Aldrich laborchemikalien GmbH Company, Germany. The acid has a concentration of 37% and molecular weight of 36.5.

2.2. Methods

2.2.1. Extraction of Jatropha oil

Jatropha oil is extracted using hexane from crushed Jatropha seeds. The extraction was carried out in a soxhlet apparatus at 60°C -70°C. The volume ratio of hexane to Jatropha seeds was 5:1. Hexane is separated from Jatropha oil by vacuum distillation of hexane at 40°C. The extracted oil yield is about 25% weight of feeds. Table 1 summarizes the physical properties of Jatropha oil while Table 2 represents its fatty acids profile.

Table 1

Physical properties of Jatropha oil.
Viscosity 40^°C (m.Pa.s)	Density (kg m^-3)	Specific Gravity	Iodine value g I₂/100 g oil	Peroxide value m Mol kg^-1	Molecular Weight (g/mol)
28.8	825	0.825	23.6296	297.62	900

Table 2

Chemical analysis of Jatropha oil.
Fatty acid composition	% weight
Palmitic acid	18.22
Stearic acid	5.14
Oleic acid	28.46
Linoleic acid	48.18
Phorbol esters	0.0018

2.2.2. Catalyst preparation and Characterization

The catalyst preparation and modifications that are produced and used in the catalytic hydrocracking of oil depend on many previous surveys and research to add value to the mineral earth clays use in a wide range of industrial applications[19, 26, 27]. The Catalyst is prepared by adding 50 gm of Bentonite clays (B) to a prepared 500 ml of 0.1M HCl and the mixture is heated to110°C in a round flask connected to a condenser, for 4h. The resulting Bentonite clays suspension is then rapidly quenched by 500ml ice-cold distilled water. After quenching, the suspension medium was filtered and washed several times using distilled water until chloride ions Cl^− 1 are removed by the washing water. The modified Clay is then dried in an oven at 110°C and then calcinated at 550°C for 4h. The pastel is ground to the powder form. The produced catalyst specifications are shown in Tables 3 and 4, which illustrate XRF analysis and surface area properties. XRD pattern, Fourier transforms infrared spectroscopy; FTIR and adsorption-desorption isotherm of raw and treated catalyst are shown in Figs. 1–3 respectively.

It is obvious from XRF that SiO₂ and Al₂O₃ are the major components of all raw materials and prepared catalysts, with trace amounts of other metal oxides. The hydrochloric acid effect on raw materials is to increase the silica content and to decrease the abundance of metal oxides such as CaO, Na₂O, Fe₂O₃, MnO, Ca²⁺, Na⁺ cations. It is seen that in XRD, modifications exist in the clays peaks on treatment with HCl. The peaks illustrate the intensity and width of catalyst which are nearly the same as the pure raw materials. This indicates structural preservation. The peak severity is an index of the degree of laminar structure retained by the clay[26, 28].

The Egyptian clays contain bands as seen in FTIR figure which indicate H-O-H stretching of absorbed water, C-H stretching, and OH stretching, and hydration of clay minerals respectively. The prepared catalyst MB shows band due to H-O-H stretching of absorbed water, C-H stretching, OH stretching hydration, Si-O stretching, and Si-O-Si bending[26, 28]. It is observed that the prepared catalysts have increased pore size and a wide range of distribution. This indicates good reactant distribution during the catalytic process. The adsorption-desorption isotherm curves of the prepared catalysts are shown in Figure (3). It is seen that the modified catalysts have a higher capability of adsorbing the reactants on their surface and a higher products desorption from the catalyst surface.

Table 3

XRF analysis of raw (B) and prepared catalyst (MB).
Main Constituents (wt%)	B	MB
SiO₂	48.7	67.2
TiO₂	1.2	1.6
Al₂O₃	19.19	19.75
Fe₂O₃tot.	9.55	5.4
MnO	0.1	0.01
MgO	2.06	0.87
CaO	4.5	0.35
Na₂O	1.37	0.57
K₂O	1.19	1.53
P₂O₅	0.25	0.10
SO₃	1.28	0.09
Cl	0.44	0.02
LOI	10.17	2.50

Table 4

Specifications of raw material (B) and prepared Catalyst (MB).
Sample property	Molecular Weight (g/mol)	Cross section area (°A²/mol)	“Total Pore volume (cm³/g)”	“S_BET (m²/g)”	“Average Pore diameter (nm)”
B	28.013	16.2	0.048352	52.2959	3.6984
MB	28.013	16.2	0.10388	96.2112	4.3186

2.2.3. Biojet fuel preparation

Catalytic hydrocracking was implemented as follows: 100 gm of filtered Jatropha oil is charged in a stainless-steel bench scale high pressure high temperature batch reactor (450ml). The prepared catalyst was added in different ratios by weight to the Jatropha oil. Hydrogen gas is compressed into the reactor to maintain a pressure of 4 bars. The mixture was heated to reach the required temperature of 350°C – 450°C for a time interval of 10 to30 minutes. The collected product was then centrifuged to separate any suspended particles from the produced bio fuel mixture. The biofuel mixture was fractionated in a laboratory distillation unit to obtain biogasoline at a temperature range of (60°C -170°C), biojet fuel at a temperature range of (170°C-270°C) and biodiesel at a temperature range of (270°C-330°C), this process is presented in a simplified flow sheet and illustrated in Fig. 4. The produced biojet fuel after fractional distillation is presented in Fig. 5.

2.2.4. Produced biojet fuel characterization

The produced biojet fuel is characterized according to ASTM specifications. The following properties are measured.

Freezing point

The freezing point of biojet fuel samples is measured according to ASTM specifications. 15 ml from every sample are placed in a glass tube and placed in liquid nitrogen until the sample is totally freeze. The freezing point was measured by reading the thermometer indicator point. This occurs when temperature reading stabilizes at the last thin crystal layer in the solid-liquid mixture.

Flash point

The flash point of biojet fuel or any volatile material is the lowest temperature at which fumes of the liquid will ignite in presence of a source of ignition. The flash point is a descriptive property used to distinguish flammable fuels, Petrol and combustible fuels, such as diesel. A fuel with a flash point less than 37.8°C is called flammable, whereas fuels are called combustible when the flash point temperature is above 37.8°C.

According to the ASTM specification, the PENSKY MARTENS FLASH POINT TESTER is used to estimate the flash point of biojet fuel. The sample is contained in an open / closed cup which is heated at different rates. A flame is brought over the liquid surface at sufficient height and the cup is opened with every degree increase in temperature up to the moment of vapors ignition.

Viscosity

Viscosity is a property used to measure the resistance of a specific fluid to flow. The sample is measured by a laboratory "DV-II + Pro" Viscometer which determines the viscosity of a specific fluid by a given shear stress and shear rates depending on the specific liquid temperature and a drive motor rpm.

Density

The density of fluids is measured using Hydrometers. It is a laboratory floating body made from a glass material which contains a cylindrical stem and a bulb loaded with a metal weight. Depending on the depth that plunges within the sample, the density value is determined directly from the reading scale at the top part of the glass body with its measuring units.

Existent gum content

According to ASTM D-381, the existent gum content of jet fuel must not exceed 7 mg/100 ml[12]. The test was carried out in the laboratory of Misr Petroleum Company. The gum values are estimated for the blend of 5% vol. biojet fuel with Jet A-1.

3.1. Bio-jet fuel production

The biojet fuel process is affected by many operating conditions such as temperature, reaction time, catalyst types, the catalyst to oil ratio, etc. Table (5) shows that at the reaction temperature of the hydrocatalytic cracking of 350˚C, the reaction is exothermic. The reaction mixture temperature is elevated to about (100 ˚C ± 10 ˚C), the highest temperature reached was 452˚C when using 4% MB catalyst and the lowest temperature reached was 445˚C when using 2% MB catalyst.

The constant hydrogen inlet pressure of 4 bars is used during the reaction to saturate double bonds and helps all cracking reactions to occur. The highest constant pressure reached in the batch reactor was 80 bar when using 4%MB at 18 min, 2%MB at 20, 30 min and the lowest pressure of 40 bar was reached when using 2% MB at a reaction time of 10 min. The pressure during the reaction system is an indicator of product quality and a good achievement of cracking reaction. The non-condensable gases, after cooling, that are produced from the reaction, result in an increase from 4 bars to 20 bars. These are carbon dioxide, carbon mono oxides, and C₁-C₄ aliphatic compounds.

Table 5

Operating conditions of catalytic hydrocracking of jatropha oil.
% Catalyst MB	Reaction Pressure (bar)	Time (min)
No-Catalyst	65	18
4%	80	18
3%	70	18
2%	70	18
1%	70	18
2%	40	10
2%	80	20
2%	80	30

Under the same conditions of 350˚C, 4 bar H₂, MB catalyst was used in the hydro-catalytic cracking of Jatropha oil at different percentage: 1%, 2%, 3%, 4% and different time (10 min − 30 min) to produce biojet fuel, the specifications of which are shown in Table (6) and Figs. 6 and 7. It is seen from Fig. 6. that the reaction time has a pronounced effect on the product yield, especially in the bio-jet fuel cut. Three laboratory experiments were performed using 2% MB catalyst, at 350 ˚C, and for three different times 10, 20, and 30 min, it was observed that the yield of bio-jet fuel increased with the reaction time. This is attributed to the completion of cracking reaction of long and heavy carbon chains to smaller chains to the produce the jet-fuel cut. The highest yield of 38% was at 30 min and the lowest yield of 18.3% was at 10 min.

For the same reaction conditions of 18 min, 350˚C, and 4 bar H₂, different percentages of MB catalyst: 1%, 2%, 3%, 4% were added to produce bio-jet fuel. The results of these experiments are shown in Figure (7). It is seen that the bio-jet fuel production yield increased with the increase of MB percentage. The 4% MB gave the best yield followed by 3% MB (40% & 39.74% bio-jet fuel) and the lowest yield was observed when using 1% MB and 2% MB (33% & 33.76% bio-jet fuel) respectively. When no catalyst was used, a bio-jet fuel yield of 33.8% was obtained. The optimum yield (40%) was obtained using MB at 18min and 4% catalyst.

Table 6

Biofuel specification and the yield of 1st three fractionations from ASTM distillation.
Catalyst Type	Feed (ml)	Feed (gm)	Density (gm/ml)	Viscosity (m.pa.s), 40°C, 60 r.p.m	Biogasoline 170°C		Biojet 270°C		Biodiesel 340°C
Catalyst Type	Feed (ml)	Feed (gm)	Density (gm/ml)	Viscosity (m.pa.s), 40°C, 60 r.p.m	Ml	% Vol	Ml	% vol	ml	% vol
No-Catalyst 18 min	68	59.8	0.879	3.75	31	45.5	23	33.8	-	-
4% MB, 18 min	75	65.9	0.878	5.15	15	20	30	40	14	18.7
3% MB, 18 min	78	69.3	0.8878	5.3	19	24.35	31	39.7	-	-
2% MB, 18 min	77	68.26	0.8864	4.9	24	31.16	26	33.76	-	-
1% MB, 18 min	76	65.9	0.867	4.6	23	30.3	25	33	-	-
2% MB, 10 min	87	78.68	0.904	10.8	19.5	22.5	16	18.3	-	-
2% MB, 20 min	87	76	0.8735	5	30	34.5	27	31	-	-
2% MB, 30 min	79	68.79	0.87	4.5	26	33	30	38	-	-

3.2. Bio-jet fuel specifications

The density of the obtained bio-jet fuel after distillation is given in Table (7) and was in the range 0.8241–0.8345 g/ml at 15°C. This conforms to the ASTM specifications of range of 0.775–0.84 g/ml. Freezing point is one of the most important methods of testing aviation fuel products. As the plane ascends, temperatures in the fuel tank and lines can drop. If the temperature of the tanks and lines drops below the freezing point of the fuel, this will impede the flow of the fuel and close the filter. This will starve the engine and shut down. Table (7) also gives the freezing point values of the produced bio-jet fuel. It ranges between − 52°C and − 56°C and are comparable with the ASTM maximum value of -47°C. Transportation regulations distinguish fuel as flammable or combustible, depending on the point of ignition by measuring of fuel flash point. The produced bio-jet fuels flash point of 53°C is well above the ASTM value of 38°C. The maximum gum content as specified by ASTM is 7 mg/100 ml, the high gum content can cause induction-system deposits and sticking of intake valves. Table (7) also presents the gum content of a blend of 5% of the produced bio-jet fuel with 95% jet A-1. The gum content is below the range specified by ASTM. The results were obtained using the catalyst (MB) and without using a catalyst. Both of them produced the lowest gum content of 5.9 mg/100ml and 6.4 mg/100ml respectively.

Table 7

Fuel specifications for the blend (5% bio-jet with 95% jet A-1).
Catalyst type	Density (g/ml)	Freezing Point (°C)	Flash Point (°C)	Existent Gum mg/100 ml	Final boiling point (°C)	Sulphur, mercaptan, wt.%
No – Catalyst	0.8241	-52	50	6.4	270	0
4% MB	0.8345	-56	53	5.9	270	0
Jet A-1[15]	0.775–0.84	-47 max	38 min	7 max	300 max	0.003 max

The catalyst (MB) was characterized physically and chemically by XRF, XRD, FTIR, and BET. The catalyst was used in the production of bio-jet fuel by catalytic hydrocracking of Jatropha oil under the obtained optimum operating conditions of 350°C, 4 bar H₂, 18 min reaction time, and 4% catalyst.

The biofuel mixture obtained from the reaction was separated according to their boiling point by distillation into four fractions: biogasoline, bio-jet, biodiesel, and mazot. The obtained bio-jet fuel yield was 40% from the total product.

The bio-jet fuel produced using the catalyst (MB) was tested and its specifications conform to the ASTM specifications with respect to freezing point (-56°C), the flash point (53°C), and existent gum content (5.9 mg/100 ml).

H₂; Hydrogen gas.

B; the Egyptian Bentonite clay

MB; modified Bentonite clay

ASTM; American Society for Testing and Materials

XRF; X-ray fluorescence

XRD; X-ray Powder Diffraction

FTIR; Fourier-transform infrared spectroscopy

BET; Brunauer, Emmett and Teller surface area

Ethics approval and consent to participate

Not applicable in this section.

Consent for publication

Not applicable in this section.

Data Availability

The datasets used and/or analyzed during the current study available from the corresponding author on reasonable request.

Competing interests

"The authors declare that they have no competing interests" in this section.

Funding

National Research Centre, award number (6/3/18), grant recipient master degree of Sarah Hisham Hassan.

Authors' contributions

S.H; Writing the paper and doing the experimental work in catalyst preparation and production of biofuel, catalyst characterizations and biofuel specification.

G.I; Review the paper, interprets biofuel results and develop the working plan.

N.K; Participating in the experimental work of the biojet fuel, analyzing data results, and Writing and Review the paper.

S.K; Interpretation of catalyst results, Review the paper.

M.R and R.S; Review the paper.

“All authors have read and approved the manuscript”, and ensure that this is the case.

Experimental research and field studies on plants

" The present study complies with the international, national or institutional guidelines"

Acknowledgements

Authors would like to express their sincere gratitude to National Research Center in Egypt for its invaluable support throughout experimental work and chemical analysis. Funded by the National Research Centre award number (6/3/18).

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Catalytic Hydrocracking of Jatropha Oil for Bio-jetfuel Production using natural clay

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Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Materials and Methods

2.1. Materials

2.2. Methods

2.2.1. Extraction of Jatropha oil

2.2.2. Catalyst preparation and Characterization

2.2.3. Biojet fuel preparation

2.2.4. Produced biojet fuel characterization

3. Results and discussion

3.1. Bio-jet fuel production

3.2. Bio-jet fuel specifications

4. Conclusions

Abbreviations

Declarations

Ethics approval and consent to participate

Data Availability

The datasets used and/or analyzed during the current study available from the corresponding author on reasonable request.

Competing interests

Funding

Authors' contributions

Experimental research and field studies on plants

" The present study complies with the international, national or institutional guidelines"

Acknowledgements

References

Additional Declarations

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Journal Publication

Version 1