Химия и химические технологии/ 5.Фундаментальные проблемы создания новых материалов и технологий

Ph.d. Student, Sadeq Muneer Shawkat

National technical university "Kharkov polytechnic institute", Ukraine

Technical aspects of biodiesel production by using a heterogeneous catalyst

 

The reactions for direct transformation of vegetable oils into ethyl esters and glycerol have been known for more than a century. The reactions of interest today, mainly those producing ethyl esters from rapeseed, soybean and sunflower oils, have been studied and optimized in order to manufacture the high quality diesel fuel known as biodiesel.  With over ten years of development and commercial use in

Europe, biodiesel has now proved its value as a fuel for diesel engines [1-2]. The product is free of sulfur and aromatics, and, as it is obtained from renewable sources, it reduces the lifecycle of carbon dioxide emissions higher compared to conventional diesel fuel. Moreover, recent European regulations in year 2005 have restricted sulfur content in diesel fuel to no more than 50 ppm [3].

Several commercial processes to produce fatty acid methyl esters from vegetable oils have been developed and are available today. These processes consume basic catalysts such as caustic soda or sodium methylate which form unrecyclable waste products. This work provides a general description of a new process using a heterogeneous catalytic system.

 

Biodiesel production principles and processes

The transesterification of triglycerides to ethyl esters with ethanol is a balanced and catalyzed reaction as illustrated in Figure 1. An excess of ethanol is required to obtain a high degree of conversion.  Rapeseed and soybean oils are among the main vegetable oil candidates for biodiesel uses.

Figure 1. Overall reactions for vegetable oil alcoholysis.

 

The conventional catalysts in natural oil transesterification processes are selected among bases such as alkaline hydroxides [4]. However, transesterification could also be performed using acid catalysts, such as sulfuric, or using metallic base catalysts such as oxides of calcium, magnesium, or zinc. All these catalysts act as homogeneous catalysts and need to be removed from the products after the ethanolysis step. 

 

Heterogeneous catalyzed

To avoid catalyst removal operations and soap formation, much effort has been expended on the search for solid acid or basic catalysts that could be used in a heterogeneous catalyzed process [5-6]. Some solid metal oxides such as those of calcium, magnesium, and zinc are known catalysts but they actually act according to a homogeneous mechanism and end up as metal soaps or metal glycerates.  This work a new continuous process is described, where the transesterfication reaction is promoted by a completely heterogeneous catalyst. This catalyst consists of a mixed oxide of zinc and aluminum which promotes the transesterification reaction without catalyst loss.

The reaction is performed at a higher temperature than homogeneous catalysis processes, with an excess of ethanol. This excess is removed by vaporization and recycled to the process with fresh ethanol. The desired chemical conversion is reached with two successive stages of reaction and glycerol separation to displace the equilibrium reaction. The flow sheet for this process appears in Figure 2. 

Figure 2. General scheme for a continuous heterogeneous catalyzed process.

 

The catalyst section includes two fixed bed reactors that are fed by oil and ethanol at agiven ratio. Excess ethanol is removed after each of the two reactors by a partial flash. Esters and glycerol are then separated in a settler. Glycerol phases are joined and the last traces of ethanol are removed by vaporization. Biodiesel is recovered after final recovery of ethanol by vaporization under vacuum and then purified to remove the last traces of glycerol.  In this heterogeneous process, the catalyst is very stable with no metal leaching. There is no formation of either glycerate salts or metal soaps which affords the following advantages: no neutralization step is required, there is no introduction of water, and there is no salt formation; these accounts for exceptional glycerol purity. In addition, there is no waste production of low-value fatty acids. 

The purity of ethyl esters exceeds 98% with yields close to 100% of the theoretical. Glycerol treatment is much easier than in homogeneous catalyzed processes. A simple elimination of ethanol by vaporization suffices and no chemicals are required. The glycerol produced is neutral, clear and exempt from any salt, with purities above 98%. This valuable product could be used in many chemical applications without further treatment. If required, pharmaceutical grade can easily be reached.

The process feeds are limited to vegetable oils and ethanol and the only products are biodiesel and a high-purity glycerol that is free of water and salt. With all its features, the process can be considered as a green process. Experiments on ethanolysis with acid-containing vegetable oils have also been conducted with no special acid removal treatment of the raw material. ethanolysis of a blend of 5% oleic acid in rapeseed oil leads to an ester  product composition compatible with biodiesel requirements. In that case, esterification and transesterification reactions occur simultaneously.

 

References:

1.      Canakci, M., (2007). The potential of restaurant waste lipids as biodiesel feedstocks. Bioresour.  Tech., 98 (1), 183-190 (8 pages).

2.      Biodiesel - A Success Story, Report of the International Energy Agency, February 2002.

3.      Montagne, X.,  2nd European Motor Biofuels Forum, Graz, September 1996.

      4.  Kreutzer, U., J. Am. Oil. Chem. Soc., 1984, 61 , pp.343.

      5.  Stern, R.; Hillion, G.; Rouxel,  J. J.; Leporq, S. US Patent 5,908,946 (1999)

      6.  Gelbard, G.; Brès, O.; Vielfaure-Joly, F.  J. Am. Oil. Chem. Soc.,1995, 72, pp1.