Ijraset Journal For Research in Applied Science and Engineering Technology
Authors: J. Srinithi, M. Thirumarimurugan
DOI Link: https://doi.org/10.22214/ijraset.2023.53741
Certificate: View Certificate
Biodiesel can be easily used an alternative fuel. Using the Soxhlet apparatus, the oil waas extracted, and centrifuged to separate the oil. The physical characteristics of oil was determined. A number of >3 indicates an acid, while a value < 3 indicates a base. If the FFA content is >0.5, the substance is an acid, and if it’s less than 0.5, a base. Suitable solvent based on its physicochemical characteristics was selected. In this study two types of seeds were used. A mixed heterogeneous base catalyst containing CaO prepared from waste egg shells and cockle shells. The egg shells and cockle shells were dried in microwave oven for 24 hours at 120?C and placed in Muffle furnace at 900 ?C and mixed in 1:1 ratio. SEM, EDAX and FTIR were used to characterize the catalyst. The two feedstock used in this study was Solanum Torvum and Murraya Koenigii. Double Step Esterification was preferred. The oil was treated with the strong acid H2SO4 . Then oil along with methanol was treated with both acid and base catalyst separately to give Fatty Acid Methyl Ester. Finally optimum condition was found for maximum yield of FAME, was obtained using RSM.
I. INTRODUCTION
Automotive vehicles that rely on petroleum, diesel, gasoline, or petro-fuels as their combustion fuel are one of the main contributors to greenhouse gas emissions that result from the use of fossil fuels. However, there are relatively few fossilised matter deposits, and thus, there are very few fossilised matter-derived goods like petroleum and diesel, etc (Hannah Ritchie et al. 2020). Environmental pollution caused by fuel combustion's byproducts is severe (Barbir, F. et al. 1990). Investigating and learning about new, clean renewable energy sources is urgently needed.
In the past century, the transportation, industries have been developed in India and other parts of the world. Also, the change in lifestyle of people, population growth leads to more energy consumption. This has caused the depletion of fossil fuels. The use fossil fuels also lead to degradation of environment causing global warming, acidification, climate change etc…The excessive nitrogen oxides and carbon monoxide emission can lead impairment of health in human beings. Since the fossil fuels have many disadvantages, it is important to develop a fuel which is non-toxic, environmentally friendly, readily available, cost effective etc. Due to the increased transportation and industries in. past decade the energy demands have been increased several folds. It is apparent that the energy demands further increases in future due to the growing population and increased transportation facilities. However, the fossil fuel available currently may diminish within 100 years and also ‘the price of fossil fuels increases every day and their usage also cause adverse environmental and health effects. Due to this increased price, scarcity of diesel fuel and detrimental environmental effects, biofuels emerge as an ultimate solution to overcome this problem. They are environmentally friendly, cost effect and has similar energy content as petroleum fuels.
India is a diverse country that promotes the use of renewable energy sources and offers incentives for the creation of energy sources based on non-conventional green fuels, like gobar gas, biomass fuels, and biofuels. In order to create a B20 mixed blend (petroleum diesel oil is blended with 20% biodiesel), India also promotes the blending of biodiesel with petroleum diesel.
Bio-fuels cause lesser pollution, leading to lower chances of acid rain and reducing the greenhouse gases emission into the atmosphere. Biodiesel consists of monoalkyl methyl esters that are derived from animal or plant sources. Biodiesel causes very negligible pollution and is a promising alternative to petroleum and diesel. It exhibits greater heating value than coal but slightly lesser than that of diesel, petro-diesel, or gasoline and it can be directly used in automotive engines configured for diesel as the combustion fuel. (Biodiesel: A Realistic Fuel Alternative for Diesel Engines, 2008).
These biofuels are non-toxic because they emit less amount of greenhouse gases like carbon monoxide, hydrocarbons, particulate matter and smoke. Although the energy production has improved the economy, it has adversely affected the environment at local, regional and global level by the emission of greenhouse gases, acid rain, drought, ozone depletion etc. Hence now the focus is to produce fuels which is environmentally friendly and economical. These methods can help us to develop sustainable earth.
Rapeseed, palm, and soybean oils are the most often used oils for biodiesel synthesis, although they are less profitable as biofuels due to their high production costs as well as significant demand for their raw materials in the cosmetics and pharmaceutical industries. Vegetable sources are generally favoured because of their widespread availability and the ease of growing and harvesting them (Issariyakul et. al. 2014). Although edible oils can be used to produce biodiesel since they eventually put a strain on agricultural lands through repetitive cultivation. The fact that they may be produced easily without the aid of fertilisers to increase production is perhaps the most essential benefit of all. This lowers manufacturing costs overall and enables producers to use biodiesel.
Transesterification is the next step in the process of biodiesel synthesis once the triglycerides have been extracted from the oil. Alcohols including methanol, ethanol, and iso-propanol can be used in the transesterification process. Alkaline catalysts and methanol do not react poorly, making it simple to separate the substance (H. Sanli et al. 2008). An acidic or basic homogeneous or heterogeneous catalyst can be used to carry out the transesterification process (Meena, R. et al. 2014).
It is reasonable to choose homogeneous catalysts over heterogeneous catalysts since they have a faster rate of reaction. Additionally, homogeneous catalysts are exceedingly expensive and challenging to separate from the reaction mixture (Ma and Hanna, 1999; Du et al. 2004). The lipid FFA% is crucial for determining which acid and alkali catalyst to use (Free Fatty Acid). Acid esterification is followed by an alkaline transesterification process if the FFA content is greater than 3% and Base esterification is followed by an alkaline transesterification process if the FFA content is lesser than 3% (Lopez et.al 2006; Dossin et. al 2006; Sharma et. al. 2009). Contrarily, soap production is a significant obstacle to using base catalysts, particularly when that are derived from animal or plant sources. Biodiesel causes very negligible pollution and is a promising alternative to petroleum and diesel. It exhibits greater heating value than coal but slightly lesser than that of diesel, petro-diesel, or gasoline and it can be directly used in automotive engines configured for diesel as the combustion fuel. (Biodiesel: A Realistic Fuel Alternative for Diesel Engines, 2008). These biofuels are non-toxic because they emit less amount of greenhouse gases like carbon monoxide, hydrocarbons, particulate matter and smoke. Although the energy production has improved the economy, it has adversely affected the environment at local, regional and global level by the emission of greenhouse gases, acid rain, drought, ozone depletion etc. Hence now the focus is to produce fuels which are environmentally friendly and economical. These methods can help us to develop sustainable earth.
II. SINGLE STEP BASE TRANSESTERIFICATION
III.TWO STEP TRANSESTERIFICATION
IV. ADVANTAGES OF BIODIESEL
V. FEEDSTOCK FOR BIODIESEL PRODUCTION
The biodiesel can be produced from animal fats, vegetable oils and used cooking oils. The animal fats cannot be used directly for biodiesel because the distribution of fats is a major disadvantage. The biodiesel can be produced from waste cooking oils too. However, usually, vegetable oils are used in biodiesel production. There are different vegetable oils which are used for biodiesel production. Some of them are soyabean oil, sunflower oil, cotton seed oil, jojoba oil etc…
In the present study oil extracted from berries of Solanum torvum(turkey berry) is used for biodiesel production.
VI. EXTRACTION OF OIL
There are different methods involved in extraction of oil from seed. They are catalytic cracking, blending, solvent extraction, enzymatic extraction etc. In the mechanical pressing process the oil extracted requires further treatment of filtering and degumming. The enzymatic process uses enzyme to extract oil which increases the cost and is a long process. Thus, solvent extraction using Soxhlet extraction technique is the one with less disadvantages. Hence it is used in this study to extract oil.
VII. CATALYSTS FOR BIODIESEL PRODUCTION
The catalysts are used in biodiesel production process so as to initiate and speed up the formation of Fatty Acid Methyl Ester compounds. The catalysts can be homogeneous, heterogeneous catalyst.
A. Heterogeneous Catalysts
Heterogeneous catalysts are developed recently. Generally, calcium oxide derived from bio- based substance is used as catalyst. These are easy to separate from the reaction mixture after the reaction is over.
B. Homogeneous Catalyst
If the catalyst is soluble in one of the reactants or if the reactants and catalysts are in same phase then it is called homogeneous catalyst. These are generally used in commercial production of biodiesel owing to the faster reaction rates provided by them. The homogeneous catalysts can be further classified as base catalysts and acid catalysts.
C. Acid Catalysts
Sulfuric Acid
It is a strong corrosive acid with pungent smell. It is colourless to slight yellow in colour.so in this study sulphuric acid is used as acid catalyst.
D. Base Catalysts
Sodium Hydroxide Catalyst
Initially sodium hydroxide was produced by reaction between sodium carbonate and calcium hydroxide. However, with the arrival of chlor-alkali industry, nowadays sodium hydroxide is produced from brine using an electrolytic process. The formula for Sodium hydroxide is NaOH. This catalyst is used for biodiesel production from olden days.
In this study, sodium hydroxide is used as catalyst for biodiesel production.
VIII. INFLUENCE OF DIFFERENT PARAMETERS ON BIODIESEL PRODUCTION
IX. PROPERTIES OF BIODIESEL
A. Cetane Number
Cetane number indicates the combustion speed of diesel fuel. Higher cetane ratings lead to maximum engine power and efficiency. The cetane number is an indication of fuel readiness to auto-ignite when it has been injected into the diesel engine.
Diesel fuels are required to have a cetane number higher than 40 and most refineries produce diesel with cetane numbers between 40 and 45. Biodiesel has a higher cetane number between 46 and 60 (depending on the feedstock used) which shortens the ignition delay in the engine and improves the combustion characteristics.
B. Flash Point
The flashpoint of a fuel is the temperature at which the vapor above the fuel becomes flammable. Petroleum-based diesels have flashpoints of 50 ºC to 80 ºC which makes them intrinsically safe. Biodiesel has a flashpoint of over 160 ºC which means that the fire hazard associated with transportation, storage and usage of biodiesel is much less than with other commonly used.
C. Viscosity
Plants and waste oils have higher viscosities compared to diesel fuel; transesterification of these oils reduces the viscosity to a large extent in converting to biodiesels. Viscosity measurement is a basic parameter reflecting the extent of the reaction.
D. Melt Point Or Pour Point
Melt or pour point refers to the temperature at which the oil in solid form starts to melt or pour. In cases where the temperatures fall below the melt point, the entire fuel system including all fuel lines and fuel tank will need to be heated.
E. Cloud Point
The temperature at which an oil starts to solidify is known as the cloud point. While operating an engine at temperatures below an oil’s cloud point, heating will be necessary in order to avoid waxing of the fuel.
F. Density
It is the weight per unit volume. Oils that are denser contain more energy. For example, petrol and diesel fuels give comparable energy by weight, but diesel is denser and hence gives more energy per litre. (Fuel Density). The aspects listed above are the key aspects that determine the efficiency of a fuel for diesel engines. There are other aspects/characteristics which do not have a direct bearing on the performance, but are important for reasons such as environmental impact etc.
G. Calorific Value, Heat Of Combustion
Heating Value or Heat of Combustion, is the amount of heating energy released by the combustion of a unit value of fuels. One of the most important determinants of heating value is moisture content. Air-dried biomass typically has about 15-20% moisture, whereas the moisture content for oven-dried biomass is negligible.
Moisture content in coals vary in the range 2-30%. However, the bulk density of most biomass feedstocks is generally low, even after densification between about 10 and 40% of the bulk density of most fossil fuels. Liquid biofuels however have bulk densities comparable to those for fossil fuels.
H. Simulation Analysis
The simulation software used here was Design of expert version 13. Response surface methodology was performed using the software.
Effect of process parameters such as Temperatures , Reaction time, Methanol /oil ratio and catalyst loading on biodiesel production was analysed using Response surface methodology(RSM)
X. MATERIALS AND METHODS
A. Materials
Extraction thimble, hot air oven, magnetic stirrer with hot plate, measuring jar, conical flask, beakers, centrifuge, Sohxlet apparatus, Round bottom flask, condenser etc.
2. Reagents
Solanum torvum and Murraya koenigii seeds were purchased from world export Madurai. Methanol, petroleum ether, sulfuric acid.
3. Collection and Preparation of Weed Sample
a. Turkey Berry Seeds
Seeds of solanum torvum were collected from all over the world. The common name of solanum torvum is turkey berry. It is a bushy, erect and spiny perennial plant. The plant is usually 2 or 3 m in height and 2 cm in diameter. It is also an edible part and have lot of medicinal values. It seeds also used in extraction of biodiesel. The seeds were sundried to remove any external moisture and then dried in a hot air oven for 8 hours at 150 o c and weighed. The seeds were crushed using an electric grinder till a consistency similar to ground powder were obtained and sieved to 60 micrometre sieve. The seeds of solanum torvum is shown in figure.
Table 3.1. Classification of solanum torvum
Kingdom |
Plantae |
Order |
Solanales |
Family |
Solanaceae |
Genus |
Solanum |
Species |
Solanumtorvum |
Habitat |
Forests, plantation crops, waste areas. |
b. Curry Seeds
Curry berries are the fruits of Curry tree which grows in clusters. The clusters consists of 32- 85 small curry berries. The white bloom present in Curry tree produce tiny fruits which is initially green in colour and ripens to shiny black in colour. About 50% of the fruit constitutes of flesh and ethereal blue is with juicy texture. Each of this fruit consists of 1-2 seeds which are in deep green colour. These seeds are toxic and not for consumption. Curry berries are not a seasonal fruit, available in all the seasons. Large amount of vitamin C is present in curry berries .It also contains anthocyanins, minerals like calcium, phosphorous, magnesium and iron. The edible part of curry tree plays an important role in Indian cooking and also in Ayurvedic medicine. The curry tree is the native of Asia. The curry tree is small in size of 4 to 6m in height and 40cm diameter. The leaves are used in many dishes in Indian subcontinent.
Table 3.2. Classification of Murraya Koenigii
Kingdom |
Plantae |
Order |
Sapindales |
Family |
Rutaceae |
Genus |
Murraya |
Species |
Murraya Koenigii |
Habitat |
Grown throughout India |
B. Properites
Table 3.3. Properties of petroleum ether
Vapor pressure |
31 kPa at 20°C |
Molar mass |
82.2 g/mol |
Appearance |
Volatile, clear, colorless, non-fluorescent liquid |
Density |
0.653 g/ml |
Viscosity |
0.46 m Pa s |
Boiling point |
42-62°C |
Uses and safety measures: It is used as a solvent for dissolving fat, oil and it helps in the extraction of oil. It is used in the manufacture of pharmaceutical compounds. It is extremely volatile, since it has low flash point and it acts as an allergen to skin.
2. Sulphuric Acid
Table 3.4. Properties of Sulphuric acid
Molecular formula |
H2SO4 |
Molar mass |
98.097 g/mol |
Density |
1.83 g/ml |
Boiling point |
337°C |
Melting point |
10.31°C |
Uses and safety measures: It is used for fertilizer manufacturing and it is also used for manufacturing printing ink, enamels. It can cause severe burns and it can cause permanent blindness. When it is swallowed, internal organs are affected and cause death. So safety measures should be taken.
3. Methanol
Methanol also known as methyl alcohol among others, is a chemical with the formula CH3OH. Methanol acquired the name "wood alcohol" because it was once produced chiefly as a byproduct of the destructive distillation of wood. Today, industrial methanol is produced in a catalytic process directly from carbon monoxide, carbon dioxide, and hydrogen. Methanol is the simplest alcohol being only a methyl group linked to a hydroxyl group. It is a light, volatile, colorless, flammable liquid with a distinctive odor very similar to that of ethanol (drinking alcohol). However, unlike ethanol, methanol is highly toxic and unfit for consumption. At room temperature, it is a polar liquid, and is used as an antifreeze, solvent, fuel, and as a denaturant for ethanol. It is also used for producing biodiesel via transesterification process. Oils and fats are included in the ester family. When they react with methanol or ethanol, they make methyl or ethyl esters and a new alcohol called glycerol or, more commonly, glycerin. The vegetable oils and animal fats used to make biodiesel can come from virtually any source.
Table 3.5. Properties of methanol
Molecular formula |
CH3OH |
Density |
0.792 g/ml |
Boiling point |
64.7°C |
Solubility |
Miscible and soluble in water |
Appearance |
Colourless liquid |
4. Methyl Ester
Fatty acid methyl esters are a type of fatty acid ester that is derived by transesterification of fats with methanol. The molecules in biodiesel are primarily FAMEs, usually obtained from vegetable oils by transesterification.
Table 3.6. Properties of methyl ester
Molecular formula |
C14-C24 |
Density |
0.860-0.849 g/ml |
Boiling point |
>475 |
Solubility |
Insoluble in water |
Appearance |
Light to dark yellow, clear liquid |
Uses and safety measures: In leather chemical industry, it is used to produce the leather fat- liquoring agent and sulfonic-succinate acyclic acyl ether disodium, serving as a promising textile detergent.
Fatty acid methyl ester can also serve as a raw material of bio-diesel which is a new environment-friendly energy source. For safety measures avoid contact to the eyes because it may cause eyes irritation and skin irritation. Vapors or mist may be irritating to mucous membranes and cause irritation and dizziness.
5. Glycerol
Glycerol is a simple polyol compound. It is a Colorless, odorless, viscous liquid that is widely used in pharmaceutical formulations. Glycerol has three hydroxyl groups that are responsible for its solubility in water and its hygroscopic nature. IUPAC Name: propane- 1, 2, 3-triol. Other names: Glycerin, propanetriol, 1, 2, 3-trihydroxypropane.
Table 3.7. Properties of Glycerol
Molecular formula |
C3H8O3 |
Molecular mass |
92.09382 g/mol |
Density |
0.126 g/ml |
Boiling point |
290 ° C |
Melting Point |
17.8 ° C |
Appearance |
Colorless, liquid, hygroscopic |
C. Methods
The dry seeds of solanum torvum and Murraya koenigii were obtained from world life export. They were dried in the sunlight .Dried in a Hot air oven at 130 ° C for 8 hours and at 1050C for 2 hours respectively until it is dried well. The seeds are then crushed and stored in air-tight container.
2. Extraction of Oil
The crushed seeds were used for oil extraction by Soxhlet extraction. Petroleum ether and n- hexane were used as two different solvents for extraction. The ratio of solvent to dried seed powder was varied for process optimization. In brief the extraction apparatus was washed with particular solvent and a cotton plug was placed at bottom and ground. The crushed seed powder(feed) was placed above the cotton plug. Appropriate solvent was filled in the round bottom flask. The entire apparatus was placed on a heating mantle. The extraction was done for 3 – 4 hours. The contents from the round bottom flask were distilled to separate solvent and extract. The volume and weight of extract and solvent was noted.
The yield of oil was calculated using the following formula:
XI. CHARACTERIZATION OF EXTRACTED OIL
The physicochemical properties of extracted oil were estimated using standard methods (AOCS, 1998; Vicente et al., 2004). FTIR spectral analysis was done to identify the functional groups and chemical interactions using FTIR spectrophotometer (Bruker, USA). GCMS analysis of the oil was performed using Gas Chromatography Mass spectrophotometer CH- GCMSMS-02 and the obtained data was compared against the data available in the Mass spectra library of the National Institute of Standards and Technology and Wiley FTIR analysis handbook. From the GC-MS and FTIR analysis, the oil’s fatty acid composition and existing functional groups were analyzed. The FFA (%) of each end product from each trial was measured using toluene solvent (AS S ilitonga et al, 2013).
A. Catalyst Preparation
The waste eggshell was collected from the hotels near by and cockle shell was also collected. Both the eggshell and cockle shell were thoroughly cleaned with warm water to remove impurities make it free from any dirties. The eggshell and cockle shell were kept in daylight for 2-3 days separately. After this both the eggshell and cockle shells were heated in oven for 4-6-hours separately at a temperature 100?-150?. The eggshell and cockle shell were crushed using mortar machine and sieved separately for 100-150micron sieve tray. The product obtained were in fine powder form. These powders were filled in crucible and kept in muffle furnace for calcination. The eggshell powder were kept at 700-800 whereas cockle shell powder were kept at 800-900. After calcination the product was allowed to cool. The both the eggshell powder and cockle shell powder were in the ratio of 1:1 which served as a base catalyst in this project.
B. Esterification Process
The oil had a pretreatment step in the first esterification reaction of the double step esterification process in order to lower the acid value. Three parts oil to one part solvent made up the oil to solvent ratio. In accordance with the above technique, numerous experimental tests were carried out to optimise the process factors.
a. First step esterification process for Solanum torvum oil
Oil was measured, transferred to a 50 ml eppendorf tube, and then methanol and catalyst were added. Thermo-mixer settings for the tube's reaction time, temperature, and agitation speed were made. After the reaction was finished, the tube's contents were transferred to a separation funnel, where the mixture instantly split into two different layers. The top and bottom layers were tested. The top layer was found to have methanol predominantly and the bottom layer was found to have the treated oil. From this treated oil alone taken to find the optimum. Testing was done on the top and bottom layers. Methanol was discovered to be predominately present in the top layer, whereas treated oil was discovered to be present in the bottom layer. To obtain the best results, only use this prepared oil. The following criteria were taken into account during the initial trials: Methanol to oil ratios of 3:1, 6:1, 9:1, and 15:1 were used, as well as catalyst loadings of 0.1- 0.5. The reaction temperature was 45°C-55°C. A significant reduction was only seen for the methanol :oil ratios of 3:1 at a reaction temperature of 55°C for 0.1ml catalyst loading , for the reaction time of 3 hours. This oil was produced in bulk volume to carry out second step esterification.
Table 3.8. First step esterification process for Solanum torvum oil
Methanol / Oil |
Temperature |
Catalyst Loading |
Time |
Acid value |
FFA |
3:1 |
55 |
0.1 |
3 |
0.76 |
0.38 |
3:1 |
55 |
0.2 |
3 |
0.9 |
0.45 |
6:1 |
55 |
0.1 |
3 |
1.06 |
0.51 |
6:1 |
55 |
0.2 |
3 |
1.2 |
0.6 |
9:1 |
55 |
0.1 |
3 |
1.6 |
0.8 |
9:1 |
55 |
0.2 |
3 |
1.78 |
0.89 |
12:1 |
55 |
0.1 |
3 |
3.6 |
1.8 |
12:1 |
55 |
0.2 |
3 |
4.2 |
2.1 |
b. First step esterification process for Murraya koenigii oil
Oil was measured, transferred to a 100ml beaker, and then methanol and catalyst were added. The sample was placed in magnetic stirrer with varying time ,temperature, catalyst. After the reaction was finished, the beakers's contents were transferred and centrifuged and then transferred to separation funnel, where the mixture instantly split into two different layers. The top and bottom layers were tested. The bottom layer was found to have methanol predominantly and the top layer was found to have the treated oil. From this treated oil alone taken to find the optimum.
Testing was done on the top and bottom layers. Methanol was discovered to be predominately present in the bottom layer, whereas treated oil was discovered to be present in the top layer. To obtain the best results, only use this prepared oil. The following criteria were taken into account during the initial trials: Methanol to oil ratios of 3:1, 6:1, 9:1, and 15:1 were used, as well as catalyst loadings of 0.1- 0.5. The reaction temperature was 45°C-55°C. A significant reduction was only seen for the methanol :oil ratios of 3:1 at a reaction temperature of 50°C for 0.2ml catalyst loading , for the reaction time of 1.5 hours. This oil was produced in bulk volume to carry out second step esterification
Table 3.9. First step esterification process for Murraya Koenigii
Methanol / Oil |
Temperature |
Catalyst Loading |
Time |
Acid value |
FFA |
3:1 |
50 |
0.1 |
3 |
0.96 |
0.48 |
3:1 |
50 |
0.2 |
1.5 |
0.84 |
0.42 |
6:1 |
50 |
0.1 |
3 |
1.18 |
0.59 |
6:1 |
50 |
0.2 |
1.5 |
1.1 |
0.55 |
9:1 |
50 |
0.1 |
3 |
1.86 |
0.93 |
9:1 |
50 |
0.2 |
1.5 |
1.8 |
0.9 |
12:1 |
50 |
0.1 |
3 |
7.6 |
3.8 |
12:1 |
50 |
0.2 |
1.5 |
7 |
3.75 |
2. Second step acid esterification using CaO catalyst
The oil had a pretreatment step in the first esterification reaction of the double step esterification process in order to lower the acid value. The optimum oil was prepared in bulk to perform second step esterification. In accordance with the above technique, numerous experimental tests were carried out to optimise the process factors.
a. Second step acid esterification – Solanum torvum
The oil that produced in bulk volume from optimum of first step esterification is used for the second step esterification process. As the FFA (%) value fall down below 0.5, it was chosen to continue the esterification process using the base catalyst. Oil was measured, transferred to a 50 ml eppendorf tube, and then methanol and catalyst (CaO) were added. Thermo-mixer settings for the tube's reaction time, temperature, and agitation speed were made. After the reaction was finished, the tube's contents were transferred to a separation funnel, where the mixture instantly split into two different layers. The qualities of the top and bottom layers were examined. The testing revealed that the top layer primarily contained methanol, catalyst, and other contaminants, while the bottom layer had a dark, oil-like substance that was only slightly miscible in distilled water. The substance from the bottom layer was centrifuged and stored.
Methanol to oil ratios was maintained from 3:1, 6:1, 9:1, and 15:1 Catalyst loadings of 0.1-0.5 was maintained. The reaction temperature was 45°C-55°C. A significant reduction was only seen for the methanol :oil ratios of 3:1 at a reaction temperature of 55°C for 0.2grams catalyst loading , for the reaction time of 2 hours. The oil was given for biodiesel test
The yield was calculated by the formula,
Table 3.10. Second step esterification process for Solanum torvum oil
RUN |
OIL / METHANOL RATIO (mL) |
WEIGHT OF OIL TAKEN (grams) |
CATALYST LOADING (grams |
TEMP (°C) |
TIME (hours) |
WEIGHT OF PRODUCT OBTAINED (grams) |
ACID |
FFA |
YIELD (%) |
1 |
3 |
1.5 |
0.1 |
55 |
3 |
1.285 |
0.32 |
0.16 |
85.65 |
2 |
6 |
1.5 |
0.2 |
50 |
2 |
1.220 |
0.40 |
0.20 |
81.33 |
3 |
6 |
1.5 |
0.5 |
45 |
2 |
1.342 |
0.46 |
0.23 |
89.46 |
4 |
6 |
1.5 |
0.5 |
55 |
3 |
0.828 |
0.62 |
0.31 |
55.20 |
5 |
9 |
1.5 |
0.2 |
50 |
2 |
1.312 |
0.50 |
0.25 |
87.46 |
6 |
9 |
1.5 |
0.1 |
50 |
3 |
1.237 |
0.40 |
0.20 |
82.46 |
7 |
3 |
1.5 |
0.1 |
50 |
3 |
1.150 |
0.38 |
0.19 |
76.66 |
8 |
3 |
1.5 |
0.2 |
55 |
2 |
1.402 |
0.24 |
0.12 |
93.46 |
9 |
6 |
1.5 |
0.2 |
55 |
3 |
0.913 |
0.58 |
0.29 |
60.86 |
10 |
9 |
1.5 |
0.3 |
50 |
2 |
1.328 |
0.62 |
0.31 |
88.53 |
11 |
15 |
1.5 |
0.5 |
55 |
3 |
0.832 |
0.74 |
0.37 |
55.46 |
12 |
3 |
1.5 |
0.5 |
50 |
3 |
1.282 |
0.38 |
0.19 |
85.46 |
13 |
6 |
1.5 |
0.1 |
50 |
2 |
1.343 |
0.48 |
0.24 |
89.53 |
14 |
6 |
1.5 |
0.1 |
55 |
3 |
0.955 |
0.64 |
0.32 |
63.66 |
15 |
6 |
1.5 |
0.3 |
45 |
3 |
1.268 |
0.54 |
0.27 |
84.53 |
16 |
9 |
1.5 |
0.5 |
50 |
2 |
1.314 |
0.48 |
0.24 |
87.60 |
17 |
9 |
1.5 |
0.2 |
55 |
3 |
0.808 |
0.42 |
0.21 |
53.86 |
18 |
9 |
1.5 |
0.3 |
55 |
2 |
0.954 |
0.36 |
0.18 |
63.45 |
19 |
3 |
1.5 |
0.5 |
55 |
3 |
0.762 |
0.38 |
0.19 |
50.80 |
20 |
15 |
1.5 |
0.1 |
50 |
3 |
1.209 |
0.54 |
0.27 |
80.60 |
21 |
6 |
1.5 |
0.2 |
55 |
3 |
0.826 |
0.64 |
0.32 |
55.06 |
22 |
3 |
1.5 |
0.1 |
45 |
3 |
1.354 |
0.28 |
0.14 |
90.26 |
23 |
3 |
1.5 |
0.5 |
55 |
2 |
0.890 |
0.64 |
0.32 |
59.33 |
24 |
3 |
1.5 |
0.3 |
50 |
3 |
1.087 |
0.46 |
0.23 |
72.46 |
b. Second step acid esterification – Murraya Koenigii
The oil that produced in bulk volume from optimum of first step esterification is used for the second step esterification process. As the FFA (%) value fall down below 0.5, it was chosen to continue the esterification process using the base catalyst. Oil was measured, transferred to a 50 ml eppendorf tube, and then methanol and catalyst (CaO) were added. Magnetic stirrer settings for the tube's reaction time, temperature, and agitation speed were made. After the reaction was finished, the tube's contents were transferred to a separation funnel, where the mixture instantly split into two different layers. The qualities of the top and bottom layers were examined. The testing revealed that the bottom layer primarily contained methanol, catalyst, and other contaminants, while the top layer had a dark, oil-like substance that was only slightly miscible in distilled water. The substance from the bottom layer was centrifuged and stored.
Methanol to oil ratios was maintained from 3:1, 6:1, 9:1, and 15:1 Catalyst loadings of 0.1- 0.5 was maintained. The reaction temperature was 45°C-55°C. A significant reduction was only seen for the methanol :oil ratios of 6:1 at a reaction temperature of 50°C for 0.5grams catalyst loading , for the reaction time of 2 hours. The oil was given for biodiesel test
The yield was calculated by the formula,
Table 3.11. Second step esterification process for Murraya Koenigii
RUN |
OIL / METHANOL RATIO (mL) |
WEIGHT OF OIL TAKEN (grams) |
CATALYST LOADING (grams |
TEMP (°C) |
TIME (hours) |
WEIGHT OF PRODUCT OBTAINED (grams) |
ACID |
FFA |
YIELD (%) |
1 |
3 |
1.84 |
0.1 |
50 |
3 |
1.482 |
0.70 |
0.35 |
80.54 |
2 |
6 |
1.84 |
0.2 |
45 |
2 |
1.538 |
0.42 |
0.21 |
83.57 |
3 |
6 |
1.84 |
0.5 |
50 |
2 |
1.734 |
0.36 |
0.18 |
94.23 |
4 |
6 |
1.84 |
0.5 |
55 |
3 |
1.081 |
0.48 |
0.24 |
58.75 |
5 |
9 |
1.84 |
0.2 |
45 |
2 |
1.664 |
0.80 |
0.40 |
90.43 |
6 |
9 |
1.84 |
0.1 |
50 |
3 |
1.460 |
0.68 |
0.34 |
78.34 |
7 |
3 |
1.84 |
0.1 |
55 |
2 |
1.572 |
0.74 |
0.37 |
85.43 |
8 |
3 |
1.84 |
0.5 |
50 |
3 |
1.607 |
0.58 |
0.29 |
87.33 |
9 |
6 |
1.84 |
0.2 |
55 |
3 |
1.118 |
0.48 |
0.24 |
60.76 |
10 |
9 |
1.84 |
0.2 |
50 |
2 |
1.648 |
0.72 |
0.36 |
89.56 |
11 |
15 |
1.84 |
0.5 |
55 |
3 |
1.059 |
0.78 |
0.39 |
57.55 |
12 |
3 |
1.84 |
0.5 |
50 |
2 |
1.650 |
0.50 |
0.25 |
89.67 |
13 |
6 |
1.84 |
0.1 |
50 |
2 |
1.680 |
0.52 |
0.26 |
91.30 |
14 |
6 |
1.84 |
0.1 |
55 |
3 |
1.106 |
0.60 |
0.30 |
60.09 |
15 |
6 |
1.84 |
0.3 |
50 |
3 |
1.611 |
0.38 |
0.19 |
87.55 |
16 |
9 |
1.84 |
0.5 |
45 |
2 |
1.660 |
0.76 |
0.38 |
90.21 |
17 |
9 |
1.84 |
0.2 |
55 |
3 |
0.975 |
0.82 |
0.41 |
52.98 |
18 |
9 |
1.84 |
0.3 |
55 |
2 |
1.114 |
0.74 |
0.37 |
60.54 |
19 |
3 |
1.84 |
0.5 |
55 |
3 |
1.024 |
0.62 |
0.31 |
55.65 |
20 |
15 |
1.84 |
0.1 |
50 |
3 |
1.427 |
0.82 |
0.41 |
77.55 |
21 |
6 |
1.84 |
0.3 |
55 |
2 |
1.092 |
0.76 |
0.38 |
59.34 |
22 |
3 |
1.84 |
0.2 |
45 |
3 |
1.575 |
0.44 |
0.22 |
85.58 |
23 |
3 |
1.84 |
0.5 |
55 |
2 |
1.141 |
0.54 |
0.27 |
62.01 |
24 |
3 |
1.84 |
0.1 |
50 |
3 |
1.381 |
0.48 |
0.24 |
75.05 |
XII. RESULT AND DISCUSSION
A. Selection Of Solvent For Extraction Of Oil
The trials for oil extraction using the proven solvent method with petroleum ether and N- hexane yielded a higher amount of triglycerides . The crushed seed to solvent ratio was maintained as 1:4 and the extraction was carried out using three solvents. The extraction with this solvent was carried out for 3-4 hours It seen that yield of petroleum ether of 40% and using n-hexane an yield of 20% oil is obtained for Solanum torvum and it is seen that an yield of 43.25% was obtained by using petroleum ether and using n-hexane an yield of oil of about 12% is obtained for Murraya koenigii. Thus, the solvent petroleum ether shows the best result, as it provides higher yield, relatively lower cost and enables easier separation process than n- hexane. The extraction was carried for same ratio of 1:4 feed to petroleum ether at to petroleum ether at different time and the Table 4.1 shows the optimisation for the time of oil extraction for both feedstocks.
The findings revealed that utilising petroleum ether as the solvent seed ratio, the seed oil had a 40% yield. Esters and carboxylic acids were present, as determined by the FTIR analysis. The results of the GCMS analysis revealed a significant amount of linoleic acid (methyl ester) and a general fatty acid composition. The free fatty acid content of the oil was decreased to 1.2% at 55°C, a reaction period of 2 hours, a 3:1 Methanol Oil ratio, and a catalyst loading of 0.2grams of CaO for Solanum torvum. The free fatty acid content of the oil was decreased to 1.8% at 50°C, a reaction period of 2 hours, a 3:1 Methanol Oil ratio, and a catalyst loading of 0.5 grams of CaO for Murraya koenigii. The experimental values were simulated using Design of expert software version 13 following RSM. Linear model was suggested for set of both experimental values.
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Copyright © 2023 J. Srinithi, M. Thirumarimurugan. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Paper Id : IJRASET53741
Publish Date : 2023-06-05
ISSN : 2321-9653
Publisher Name : IJRASET
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