1.

0 ABSTRACT This experiment requires the researching and learning of a method to produce biodiesel from palm oil on a laboratory scale. Palm oil is reacted with methanol, catalysed by sodium hydroxide (NaOH) lye through a process called transesterification. This process involves the breaking up of the triglyceride chain in palm oil and combination of each chain with methanol, isolating out glycerine. When mixing and reaction are finally complete, the ester (biodiesel) and glycerine will isolate themselves away as two separate liquid phases.

2.0 OBJECTIVE OF EXPERIMENT To investigate and learn the methods to produce biodiesel from palm oil and methanol with sodium hydroxide as the catalyst.

3.0 SCOPE OF EXPERIMENT To produce biodiesel via transesterification process of palm oil with methanol, catalysed by sodium hydroxide on a laboratory scale.

4.0 THEORY Biodiesel is a biodegradable fuel and the fact that engines running on biodiesel do not emit black smoke can help to alleviate current environmental pollution problems caused by fossil fuels, especially greenhouse effects. Biodiesel produced from palm oil, or palm diesel, produced using patented PORIM (Palm Oil Research Institute of Malaysia)/PETRONAS (Petroliam Nasional) production technology has been widely tested as a substitute in a wide range of diesel engines. In fact, biodiesel possesses fuel properties comparable to those of petroleum diesel. The effort and initiative to utilize palm oil as an alternative energy source are also in accord with the Malaysian Governments five-fuel diversification policy to include renewable energy as the fifth fuel.

Palm oil belongs to a chemical group called triglycerides, containing glycerine. The biodiesel process turns the oil into ester, separating out the glycerine, which sinks to the bottom while the biodiesel floats on top. This process is called transesterification, which substitutes alcohol for the glycerine in a chemical reaction, using a catalyst. A variety of catalysts can be

used, for instance basic ones such as sodium or potassium hydroxides, acids such as sulphuric acid, ion exchange resins, lipases and supercritical fluids. In this experiment, a basic catalyst, namely sodium hydroxide (NaOH) is required.

Figure 1: Transesterification process

NaOH is used with methanol. In this process it is better to produce the alcoxy before the reaction to obtain a better global efficiency. The alcoxy reaction is R CH2OH + NaOH H2O + R CH2ONa The alcohol oil molar ratio that should be used varies from N = 1:1 6:1. However N = 6:1 is commonly used giving an important conversion for the catalyst without using too much alcohol. The standard temperature for the reaction to occur is 60C, but depending on the type of catalyst different temperatures will give different degrees of conversion. Therefore, the temperature range should be from 25 to 120C. Base-catalyzed processes are generally more efficient and less corrosive than using acid. Examples of other catalysts are tabulated in Table 1 on the next page.

Table 1: Experimental conversions to methyl ester for different catalysts

CATALYST NaOH Amberlyst A26 Amberlyst A27 Amberlyst 15 MELCat XZO682:01 MELCat XZO645:01 TIS TILCOM STC SnCl2 MgO USY-292 Novozym 435

CATALYST TYPE Strongly basic Anion-exchange resin Anion-exchange resin Cation-exchange resin Sulphate doped zirconium hydroxide Silica doped zirconium hydroxide Titanium silicate Titanium chelate Lewis acid Metallic oxide Zeolite Immobilized lipase

CONVERSION (%) 100.0 0.1 0.4 0.7 0.0 0.0 0.6 0.5 3.0 11.0 0.2 0.0

Temperature = 60C; reaction time = 8 hours

5.0 APPARATUS AND CHEMICALS 5.1 Apparatus : Handy-sized lightweight plastic bag, scales (accurate to 0.1 g)

measuring cylinder, thermometer, heater, blender, translucent white HDPE (#2 plastic) container with stopper and screw-on cap (0.5 L), funnel to fit HDPE container, PET bottles (water or soft-drinks bottle, 2 L), duct tape

5.2 Chemicals

: Palm oil (1 L), methanol (99% pure), sodium hydroxide lye (NaOH,

at least 96% pure)

6.0 METHODOLOGY

1. Measure 3.5 g of NaOH pellets (96% pure) into the plastic bag on the scales and close it quickly. NOTE : NaOH absorbs water from the atmosphere rapidly and water can interfere with biodiesel reaction NOTE : If 96% NaOH is not provided, use 4.9 g (99%) OR 5.3 g (92%) OR 5.8 g (85%). 2. Measure 200 mL methanol and pour it into the cone using the funnel. 3. Add NaOH to the methanol using a second funnel. The mixture is now methoxide. 4. Swirl the mixture in the cone for a minute or so five or six times until the mixture inside is clear with no undissolved particles. 5. Weigh an empty beaker and weigh it again containing 1 L palm oil. RECORD PALM OIL NET WEIGHT IN TABLE 1. 6. Preheat the palm oil to 55C. DO NOT PUT THE MAGNETIC BAR YET. 7. Pour the methoxide carefully into the oil. 8. Put in the magnetic bar and set the stirring mode at lower speed for at least 20 minutes. 9. Stop the stirring process and transfer the mixture into the separatory funnel (with stopcock tap closed). Close it with the stopper. 10. Let the mixture settle for 1 2 hours. 11. Open the stopcock tap to drain off the bottom glycerine layer. 12. Weigh another empty beaker and collect the biodiesel layer. RECORD BIODIESEL NET WEIGHT IN TABLE 2.

7.0 RESULT OF ANALYSIS

Table 1: Weight of 1 L Palm Oil Weight of beaker + 1 L palm oil Weight of empty beaker Net weight of 1 L palm oil 1328.15g 573.32g 754.83g

Table 2: Weight of Biodiesel Weight of beaker + biodiesel Weight of empty beaker Net weight of biodiesel 1006.09g 304.46g 701.63g

Percentage of biodiesel produced:

8.0 DISCUSSION

From the experiment, the percentage of biodiesel produced is 92.95 %. This shows that 80 90% of palm oil will produce biodiesel from the methanol and palm oil with sodium hydroxide, NaOH catalyst. The 10 20% of palm oil will produce glyceride from this reaction. A fatty acid ester is produced by the transesterification of triglycerides, which is one of the main constituents of vegetable oils, and alcohol. This ester has received much attention as a biodiesel with the advantages of non-toxicity and low emissions.

While adding the base, a slight excess is factored in to provide the catalyst for the transesterification. The calculated quantity of base (usually sodium hydroxide) is added slowly to the alcohol and it is stirred until it dissolves. Sufficient alcohol is added to make up three full equivalents of the triglyceride, and an excess of usually six parts alcohol to one part triglyceride is added to drive the reaction to completion. The alcohol is deprotonated with a base to make it a stronger nucleophile. Commonly, ethanol or methanol is used. As can be seen, the reaction has no other inputs than the triglyceride and the alcohol. The three most important parameters affecting triglyceride transesterification are the molar ratio of the methanol to the triglyceride, the nature and the amount of catalyst, and the reaction temperature. After settling, dark-coloured glyceride will collect as a layer at the bottom of the bottle, with a clear line of separation from the pale liquid above which is going to be decanted, namely the biodiesel. Both the biodiesel and by-product layers can exist in a variety of colours according to the oil used. Usually its pale and yellowish. The biodiesel might be clear or it might still be cloudy, which is however not a problem, as it will clear eventually after a long time period.

9.0 PRECAUTION

There are some precautions that need to consider such as: a) Make sure the methanol and sodium hydroxide powder, NaOH dissolve until no particle powder at bottom of beaker b) Mix the palm oil with the methanol and sodium hydroxide, NaOH homogenize c) The temperature during the mixing the palm oil must below 60 to get maximum yield during reaction with methanol and sodium hydroxide catalyst, NaOH

10.0

CONCLUSION

Biodiesel can be produced from palm oil by transesterification with methanol, catalyzed by sodium hydroxide. Through transesterification, palm oil reacts with methanol to form biodiesel and glycerine, which are separable liquid phases.

11.0

REFERENCES

Marchetti, J.M., Miguel, V.U., and Errazu, A.F., 2007, Possible methods for biodiesel production: Renewable and Sustainable Energy Reviews, v. 11, p. 1300 1311.

Crabbe, E., Nolasco-Hipolito, C., Kobayashi, G., Sonomoto, K., and Ishizaki, A., 2001, Biodiesel production from crude palm oil and evaluation of butanol extraction and fuel properties: Process Biochemistry, v. 37, p. 65 71.

Kim, H.J., Kang, B.S., Kim, M.J., Park, Y.M., Kim, D.K., Lee, J.S., and Lee, K.Y., 2004, Transesterification of vegetable oil to biodiesel using heterogeneous base catalyst: Catalysis Today, v. 9395, p. 315320