Biodiesel Abstract The purpose of this lab was to synthesize biodiesel by transesterification of triglycerides Fresh County Market vegetable oil and methanol into a mixture of fatty acids and glycerin This was done by heating a methoxide solution with vegetable oil KOH was used as a catalyst After this tests were performed to show the quality of the biodiesel A wash test showed how well it separated with water a methanol test showed how well the biodiesel dissolved and an FFA content test would have been done to show the biodiesel breaks down These tests concluded that the biodiesel was a decent quality proving the lab to be a success Introduction The purpose of this experiment is to convert vegetable oil into biodiesel The process used is transesterfication of triglycerides with methoxides Preparing a methoxide solution synthesizing biodiesel separating products and gas chromatography are all used in this lab Also The determination of free fatty acid FFA is also determined in this lab Studies in biodiesel range in many different areas and the science used in this lab also ranges to many different areas A specific study in china used gas chromatography as in this procedure to characterize a biodiesel compound Transesterfication was used to synthesize the oil as in this lab and a KF Sm2O3 catalyst was used1 In another biodiesel study a catalyst is in development that is very eco friendly made from crab shell waste and sunflower oil The process to synthesize the diesel is transesterfication They also used a gas chromogram along with X ray and NMR studies to characterize this biodiesel2 Finally in another study synthesized calcium methoxides from quick lime in a refined palm oil biodiesel production3 Biodiesel is a vegetable oil or animal fat based diesel fuel with long chains of esters One of the main chemistry concepts used in this lab is a transesterification reaction This is the main process used in the synthesis in this procedure and the basic premise of this concept is that an alcohol reacts with an ester group to yield another ester and a different alcohal4 Typically animal fats and vegetable oils are used due to long carboxylic acid chains attached to glycerol chains Specifically a triglyceride reacts with a methanol to form fatty acid methyl esters and glycerol Methanol and ethanol are typically used in this process due to the steric hindrances that larger alcohol have Steric hindrances are slower reaction rates due to larger atoms or groups6 These larger alcohols also have a higher volatility of the produced biodiesel This means they are easily evaporated or have low boiling points A catalyst is used to drive this reaction in this lab Catalysts lower the activation energy of reaction to make them more thermodynamically favorable Methoxides are synthesized in order to use transesterification to switch ester groups with triglycerides Methoxides are organic salts Gas chromatography is used in this lab to test the produced biodiesel and determined the FFA content Gas chromatography is separating the components of a solution by using the different boiling points and analyzing the different components FFA s or free fatty acids are unesterfied fatty acids that need to be neutralized because they did no convert in the transesterification process This can be done by acid catalyzed esterification A small amount of base can be used to neutralize this which turns FFA s into a soap solution This process is known as saponification The soap will then separate out with the glycerol Starting materials if the contain water will hydrolyze with triglycerides to form carboxylic acid salts or soaps This is a more favorable reaction than the transesterification Density separation is when different types of reagents will separate over time du to different densities They can then be easily extracted Also this means reagents that are polar will separate from non polar ones making it easy to separate these too Biodiesel titration is another concept used in this lab This can be used in the process of saponification to neutralize FFA s and form soap This titration is done in a slight excess in order for the reaction to proceed correctly Materials and Methods This lab was very limited in what was done due to the lack of some materials Biodiesel was created but many aspects were left out A complete list of the procedure can be seen in the lab manual3 The first time the methoxide solution was prepared it was over heated and the solution was disgarded along with the test The heat went above 65 which is the boiling point of methanol The second trial was not heated above 60 C and kept The temperature of 55 C was maintained for 55 minutes rather than an hour The FFA content was not determined due to the lack of waste oil This whole test was not done After the transesterification the biodiesel was allowed to separate for a week rather than a day and after washing the biodiesel was not allowed to dry rather than letting dry for a week None of the gas chromatography tests were done in this lab due to the lack of readiness of the machines For the methanol test the solution was put on heat of 55 C to dissolve the solution It did not exceed 65 C to ensure the methanol did not boil Other than these very large deviations no other deviations were necessary Results Table 1 Qualitative Observations of Wash Test Layer Color Bottom Foggy clear Top Yellow translucent Table 2 Observations of Methanol Test Color Of Biodiesel prior to Methanol After addition of Methanol Initial amount Methanol added Amount of extra Methanol Temperature added until dissolved Yellow translucent Clear with layer 225mL 37mL 52 mL 55 C Table 3 Color Observations Compound Fresh County Market Vegetable oil KOH Methanol Methoxide Biodiesel Glycine Wash Test Water Color Description Yellow White Solid Clear Solution Clear solution White Yellow viscous liquid Clear Cloudy then Clear Discussion The purpose of this lab was to synthesize biodiesel from the transesterification of triglycerides This triglyceride solution was methoxide This can be done and was done from Fresh County Market Vegetable oil This Fresh County Market vegetable oil contains long chains of carboxylic acids that are attached to a glycerol In the lab a methoxide solution was made from methanol and KOH The fresh unused County Markey vegetable was heated to fifty five degrees Celsius It was heated up no hotter than sixty degrees because methanol boils at sixty five degrees This was
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