Optimization of the Temperature and Reaction Duration of One Step Transesterification

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1 Optimization of the Temperature and Reaction Duration of One Step Transesterification Ding.Z 1 and Das.P 2 Department of Environmental Science and Engineering, School of Engineering, National university of Singapore 21Lower Kent Ridge Road, Singapore ABSTRACT Acid catalysed direct transesterification of wet biomass is carried out in order to improve energy efficiency. A comparison of FAME conversion rate under variable temperature & duration is made between sulfuric acid and hydrochloric acid. It is found that sulfuric acid catalyses the reaction four times faster. Optimization of temperature and duration is found in order to achieve relatively high conversion rate at low consumption of heat energy. Higher FAME conversion yield was observed for both the catalysts, for increasing the temperature, within the temperature range studied. At C, minimum time requirement was 30 minute for 100% FAME conversion, when H 2 SO 4 was used; for HCl, it was almost 2 hours. It is concluded that direct transesterification of wet biomass is a viable approach in producing biodiesel from microalgae. INTRODUCTION Unsustainable burning of fossil fuel has resulted in irreversible consequences like global warming, depletion of non-renewable fossil fuel reserves which may hinder the human development in the near future. Thus finding a renewable source of energy to replace the fossil fuel remains as the main focus of many researchers in the energy field. The energy density of biodiesel is almost equal to the petroleum fuel. Microalgae have a high potential to become the source of energy supply in the future. However, the biodiesel production from microalgae still faces challenges; especially in the downstream processing.one step transesterification can avoid some of the energy intensive drying and lipid extraction process and can make the overall process more efficient. BIODIESEL FROM MICROALGAE Biofuel from agricultural crop versus microalgae Currently there are two types of biofuel that have been commercialized. One is from food crops that have high oil content like soybeans and the extracted oil is converted to biodiesel. The other one is from crops with high sugar content like sugarcane and the sugar extracted is converted to bioethanol. However these two types of biofuel only contributed 4/10ths of 1% of the total petroleum-based fuel production (Biofuel facts, 2008). Furthermore, the production of biofuel in large quantities from agricultural crops is not sustainable (Chisti, 2008). Biodiesel from microalgae has high oil to biomass ratio 1 Student 2 PhD Student/Supervisor

2 and the fast growth rate which makes it great alternative to the future oil source. The two main challengers of this technology are to maximize energy efficiency and minimize the cost in the production. Oil derived ester FAME (Fatty acid methyl esters) is the major product from the process (Posten& Schaub, 2009). In situ conversion of lipid into FAME was then developed to reduce the solvent requirement in a relatively shorter time. Direct conversion of wet algae biomass into biodiesel in one step was not studied earlier. Such technique will reduce the energy required for drying the biomass which contributes greatly to the overall energy consumption. Objectives of the experiments 1. Compare the FAME yield for different acid catalysts: Acids are commonly used to catalysts to speed up the transesterification of oils extracted from wet microalgae biomass. The rate of FAME conversion will be compared by using sulfuric acid and hydrochloric acid. 2. Optimize the temperature and duration for the transesterification reaction of wet algal biomass Experimental processes Microalgae species and cultivation processes In this study a locally isolated marine yellowish green microalgae, Nannochloropsis sp. was used. Under optimum conditions the strain can double its biomass in less than a day. Although the strain accumulates low level of neutral lipid in phototrophic growth mode, the lipid content and classes can be enhanced by adding appropriate organic substrate; which make the strain an ideal candidate for biodiesel feedstock production. Seawater used to grow the algae was first filtered through progressively lower pore size filters and finally sterilized using UV light by a TMI filtration system. 10 liter sterile culture of Nannochloropsis sp. was transferred into 200 liter plastic tubes. When the culture in the plastic tubes was sufficiently dense (optical 680nm wavelength was 1.2), 20 liter of culture was transferred into an outdoor raceway pond (20 cm depth and 250liter capacity). Sunlight was the only light source for the photosynthesis that occurred in the raceway ponds. The depth of the culture, as increased by rainfall, was not adjusted later. Guillard f/2-si was used as the nutrients medium for the culture. A submergible water pump was used to provide a 20cm/s liquid flow in the raceway pond. No organic substrate was supplemented throughout the entire culturing period. Once the culture reach in its stationery phase (after 12 days), it was kept for 3 additional days to accumulate more lipid. Finally the culture density reached about 0.52gm/liter as dry weight. Harvesting and biomass processing The algae biomass was harvested using ferric chloride as coagulant and air sparging device to assist coagulation flocculation (ASACF) process, a process developed in our lab, which is very simple and robust technique consuming less than 20 times energy of any reported value. Details of the process can be found elsewhere. After decanting the top layer of water (95% by volume), the bottom part was centrifuged to reduce water content further. At this stage the biomass was in paste form. The algae paste was then divided into three parts: (1) first part for FAME conversion with no modification applied to it (FP), (2) second part was kept in freeze dryer overnight (FF) and (3) the last part was dried in oven at 80 0 C for 12 hours (FO). In

3 order to study the effect of coagulant, a little volume of the culture was centrifuged and dried in freeze dryer (CF). Processing biomass for FAME synthesis 200 mg of wet biomass was taken into 20 ml glass vials. A transesterification reaction solution was prepared using 10:1 ratio of methanol and H 2 SO 4.4 ml of freshly prepared TRS was added into the vial and was immediately sealed with a septum and an aluminum cap. Next the vials were kept in ultrasonic bath (100 watt, 30 0 C) for 10 minutes to cause the burst of the cells and release to lipid. The vials were then transferred into oven and kept there at 40 0 C C. After a predetermined time interval (5, 10, 15, 30, 60, 90 and 120 minutes), the vials are removed from the oven and allowed to cool at room temperature. Next the entire solution was transferred into a centrifuge tube and immediately 1 ml of water was added. Next the 3ml solution mixture of hexane and chloroform (4:1) was added in the tube. The tube was kept in a vortex and later centrifuged at 4000 rpm for 5 minutes and the top layer was collected. The process was repeated one more time. Thus obtained extracted solution was analyzed for FAMEs using Agilent7900 Gas Chromatography fitted with Flame Ionization Detector (GC-FID). Results and discussion Figure 1: Relative FAME yield for catalyst HCl, at different time under different temperature

4 Figure 2: Relative FAME yield for catalyst H 2 SO 4, at different time under different temperature Compare the FAME yield for different acid catalysts Concentration o f catalysts were 1.01M and 0.97M for HCl and H 2 SO 4 respectively. For the two lower temperatures 40 C and 60 C, the rate of FAME conversion is almost the same for the two catalysts, i.e., 50 to 60% FAME conversion at 30 minutes. After 30 minutes, the graph flattens out as the rate of FAME conversion slowed down and reached a stop after 60 minutes for both of the catalyzed reactions. For the two higher temperatures, the rate of FAME conversion varies differently for the two catalyzed reactions. Although H 2 SO 4 concentration was lower than HCl concentration, faster and complete FAME conversion was observed when H 2 SO 4 was used as a catalyst. Under optimum temperature, i.e., C, 100% FAME conversion yield was observed after 30 minutes when H 2 SO 4 was used. However, the maximum FAME conversion yield was 94% after 2 hours at C when HCl was used as a catalyst. Hence using H 2 SO 4 as a catalyst is preferred when reaction is taking place under high temperature, i.e., 80 C the reaction time can be reduced by 90 minutes to reach high rate of FAME conversion. This will make the one step transesterification more efficient. Optimize the temperature and duration for the transesterification reaction of wet algal biomass As it is observed from Figure 1 and Figure 2, when temperature increased from 60 C to 80 C, there is a great increase in the rate of FAME conversion. However, a minimal increase in rate of FAME conversion is observed when temperature increased from 80 C to 100 C. Hence, the optimum temperature should be between 80 C to 100 C. Within this optimum temperature range, the optimum duration is 30 minutes and 60 minutes for transesterification catalyzed by sulfuric acid and hydrochloric acid respectively. Conclusion As demonstrated here, the direct transesterification of wet microalgae biomass is technically feasible. A comparison was made between the reactions catalyzed by sulfuric

5 acid and hydrochloric acid. It was proven that sulfuric acid gives greater rate of FAME conversion. Within the optimum temperature range 80 C to 100 C, the preferred catalyst sulfuric acid only takes 30 minutes to reach 100% FAME conversion. By operating transesterification under optimum condition, the energy efficiency is improved and the production of the biodiesel will be more cost effective. With the advancement in technology, the cost in production can be further reduced by increasing the lipid content of the microalgae through either genetic modification and improving the culturing technique. The biodiesel from microalgae will be part of our sustainable development in the near future. References Biofuel facts, BBC News. Last retrieved on 7 th August,2009 from shtml Chisti,Y.(2008) "Biodiesel from microalgae beats bioethanol." Trends in Biotechnology 26(3): Posten,C & Schaub,G.(2009) Microalgae and terrestrial biomass as source for fuels A process view. Journal of Biotechnology 142 (2009) 64 69

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