PRODUCTION OF FATTY ACID METHYL ESTERS FROM SIMAROUBA OIL VIA ULTRASONIC IRRADIATION PROCESS, EFFECTIVE UTILIZATION OF BYPRODUCTS. TESTING AND EXTRACTION OF PHYTOCHEMICALS FROM SIMAROUBA OIL AND CAKE COLLEGE : SIDDAGANGA INSTITUTE OF TECHNOLOGY. TUMKUR DEPARTMENT : MECHANICAL ENGINEERING GUIDE : ARUN S.B. STUDENTS : SHARATH M HARSHA HEBBAR H R VARUN A NAVEEN KUMAR K J Keywords: Simarouba Glauca, Heterogeneous base catalyst, Ultrasonic Processor, Phytochemicals. Introduction: In biodiesel production, vigorous mixing is required to create sufficient contact between the vegetable oil/animal fat and alcohol, especially at the beginning of the reaction. Ultrasound is a useful tool to mix liquids that tend to separate. Ultrasonic waves cause intense mixing at micro-levels and improve mass transfer greatly, so that the reaction can proceed at a much faster rate. Although not currently in wide use, ultrasound is a promising technology for biodiesel production. Ultrasound processing results in similar yields of biodiesel with a much shortened reaction time compared to the conventional stirred-tank procedure. Ultrasonic reactors can process triglycerides into biodiesel within minutes. In addition, current users of the technology claim that much less catalyst and methanol are required. Ultrasonic processing can be used successfully with a wide variety of feedstock, including high free fatty acid feedstock. In addition, ethanol can be used instead of methanol. Catalysts can include potassium and sodium hydroxide and sulfuric acid. Researchers have also reported using enzyme catalysts with ultrasonic processing, and showed good results without much loss of enzymatic activity during the time of the study. Ultrasound refers to sound waves that are above the frequency for human hearing, which is approximately 2 kilohertz (khz), or 2, cycles per second. These kinds of rapidly vibrating sound waves transfer energy into the fluid and create violent vibrations, which form cavitation bubbles as the low pressure part of the sound passes through the liquid. After the wave passes, the bubbles collapse, causing a sudden contraction of the fluid. This collapse produces very intense mixing in the area of the bubbles. Such a high-energy action in the liquid can considerably increase the reactivity of the reactant mixture and shorten the reaction time without involving elevated temperatures. In fact, this reaction can be achieved at or slightly above ambient temperature. More research is needed to determine optimum levels of ultrasonication power input for biodiesel production. Using a higher frequency and intensity does not necessarily increase the speed or effectiveness of the biodiesel reaction. Most experiments have used 2-24 khz for biodiesel processing. Objectives: To obtain a pure sample of Bio-diesel with the help of an Ultrasonicator To Improve the yield of Bio-diesel Fuel property test Phytochemicals test Effective use of by-products Reducing the usage of Non-renewable resources Methodology:
Materials: Simarouba Glauca, KOH and Methanol were used in production of biodiesel. The extraction of oil from Simarouba Glauca kernel was done by Mechanical expeller. Simarouba cake was used to test Phytochemicals. Characterization of Oil: Table 1.a: Percentage yield of Simarouba oil Extraction Method Yield in % Mechanical Expeller 2 Soxhlet Apparatus 5-55 The fatty acid composition of the Simarouba oil was analyzed using gas chromatography (GC). The chromatography consists of AGILENT equipped with flame ionization detector. Hydrogen gas used as carrier gas at a flow rate of 23ml/min. Column was packed with DB wax of dimension 3mm x.25mm. Injector port and detector port temperatures were maintained at 27 C and 28 C respectively. Data is shown in table 1.b. Table 1.b: Chemical compositions of Simarouba oil. Sl. No. Fatty acids Carbons Fatty acid (%) 1 Palmitic Acid 16: 12.81 % 2 Stearic Acid 18: 23.23 % 3 Oleic Acid 18:1 57.17 % 4 Linoleic Acid 18:2 4.1 % 5 Arachidonic Acid 2:2 1.18 % Transesterification setup: Transesterification reaction mixture is taken in a 25ml glass beaker. Ultrasonic Processor SONOPROS PR-25M with the power supply of AC-25V is used for transesterification process. The Sonotrode or Probe is carefully placed inside the beaker. Figure 1: Ultrasonic Processor SONOPROS PR-25M Transesterification process: Reaction mixture is produced by adding 6:1 molar ratio of methanol to simarouba oil along with 1.5% (w/v) of KOH catalyst. The reaction mixture is taken in a 25ml of glass beaker and placed in an ultrasonic processor. The devices provide four different programs which control the vibration of
sonotrode. Each program has different pulse time and total reaction time. Pulse time is the time period during which sonotrode vibrates and static time is the time period during which sonotrode remains stationary. Total reaction time is the sum of pulse time and static time. Reaction is carried out by selecting any particular program out of four. High vibration of sonotrode causes vigorous mixing and converts triglycerides into methyl esters. Figure 2: Transesterification reaction setup Separation: The product obtained from the reaction is transferred into a separating funnel to settle down for 12 hours. After this, reaction product separates into two layers, low density Bio-diesel settle at the top and glycerin at the bottom. Phytochemicals test: Simarouba Glauca plant and seeds are known to have medicinal properties and phytochemicals. Phytochemical tests are used to study the presence of following constituents such as, alkaloids, carbohydrates, Flavonoids, Glycosides, proteins, Saponins, steroids and tannins. Results and Discussion: Table 2: Fuel properties of Methyl Ester (SOME) SI. NO PROPERTIES UNITS Biodiesel (SOME) EXPERIMENTAL VALUES Biodiesel Standards (ASTM) Conventional Diesel 1 Kinematic viscosity@4 c centistokes 4.9 1.9-6. 2.54 2 Density 3 kg/m 875 85-9 82 3 Flash point C 155 >13 * 54 4 Calorific value KJ/kg 3793 37 435 5 Cloud point C 15-3 to 12-28 to -7 6 Pour point C 12-15 to 1 5.6 to 11.1 7 Ash content %w/w Nil -----.2max 8 Carbon residue %w/w Nil -----.5max
2 18 16 Kinematic Viscosity (cst) 14 12 1 8 6 4 2 Graph 1: Comparison of kinematic viscosity among above test samples 8 Density (kgm -3 ) 6 4 2 Graph 2: Comparison of Density among above test samples 2 Flash Point ( C) 15 1 5 Graph 3: Comparison of Flash point among above test samples Table 3: Phytochemical compounds presents in simarouba seed cake Sl. no. Phytochemical test Seed cake 1) Flavonoids + a. Ferric chloride test + b. Alkaline reagent test +
2) Alkaloid - a. Mayer s test - b. Wagner s test - 3) Carbohydrates - a. Molish s test - b. Benedict test - 4) Proteins + a. Xanthoprotein test + b. Nanhydrin test + 5) Saponin + a. Foam test + 6) Glycosides - a. Killer klani test - b. Bromin wates test - 7) Steroids - a. Salkowaski s test - b. Lieberman s test - 8) Tannins + a. Ferric chloride test + Conclusion: Bio-diesel is a low emission, high lubricating and alternative fuel produced from renewable resources. The tree borne oil like Simarouba Glauca is the most potential species to produce biodiesel in India which could offer opportunity for generation of rural employment. The process is based on Homogeneous base catalyzed transesterification. Use of Ultrasonic processor reduces reaction time. By selecting the program-4 in Ultrasonic processor, simarouba oil methyl ester of yield 96% is achieved. Results indicate the presence of phytochemicals like Flavonoids, Proteins, Saponins and Tannins. Scope of future work: By using bigger Sonotrode it is possible to carry out reaction in larger quantity. By varying the reaction time and pulse time it may be possible to improve yield. Varying the quantity of methanol and catalyst concentration may improve conversion ratio.