Biyomotorin üretiminde rafinasyon aşamasının incelenmesi
An Investigation of the refining step of the bio diesel production
- Tez No: 46593
- Danışmanlar: DOÇ.DR. FİLİZ KARAOSMANOĞLU
- Tez Türü: Yüksek Lisans
- Konular: Kimya Mühendisliği, Chemical Engineering
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 1995
- Dil: Türkçe
- Üniversite: İstanbul Teknik Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Belirtilmemiş.
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 45
Özet
ÖZET Kolza yağı-metanol transesterifikasyon reaksiyonu ürünü ester (Biyomotorin); mevcut, yenilenebilir enerji kaynaklı, çevre dostu, uygulama aşamasına geçmiş en önemli ve tek motorin alternatifidir. Biyomotorin üretiminde belirgin sorunlar bulunmamakta, reaksiyon ürün karışımından saf biyomotorinin eldesi ise, çeşitli teknik zorluklara neden olarak yakıt maliyetini artırabilmektedir. Bu nedenle, transesterifikasyon reaksiyonu ürün karışımının rafinasyon aşaması ayn bir öneme sahiptir. Bu çalışma, kolza yağı-metanol transesterifikasyon reaksiyonu (katalizör: NaOH) ürün karışımının rafinasyonunun incelenmesi amacıyla gerçekleştirilmiştir. Yapılan teorik çalışma ile kolza yağı, biyomotorin üretimi ve özellikle rafinasyon aşaması ile yakıtın uygulamaları irdelenmiştir. Deneysel çalışmada ise, ham ve nötralize kolza yağı tanımlanmış, nötralize kolza yağı-metanol transesterifikasyon reaksiyonu %97.32 ester verimi ile gerçekleştirilmiştir. Bu reaksiyonun ürün karışımından saf biyomotorin eldesi için; sıcak su ile yıkama, petrol eteri ve suyla yıkama, sülfiirik asitle nötralleştirme rafinasyon yöntemleri denenmiştir ve en uygun rafinasyon yöntemi olarak 50°C'de sıcak suyla yıkama yöntemi seçilmiştir. iv
Özet (Çeviri)
SUMMARY AN INVESTIGATION OF THE REFINING STEP OF THE BIO-DIESEL PRODUCTION Supply-demand imbalances in the energy sector owing to constantly expanding populations and industrial growth, unreliable oil price policies that result in oil shortages, and energy crisis together with the predicted depletion of conventional fossil-derived fuels stimulated interest and research in the field of new renewable fuel alternatives. Among the new energy sources, biomass potential is particularly attractive compared to fossil resources, since it has the advantage of being renewable. Liquid fuels are a vital necessity particularly for agricultural production, which largely depends on diesel fuel. Timing of the field operations, such as planting, cultivating, and harvesting, within a seasonal cycle is especially critical. To keep all of these energy-intensive operations on track, a dependable and readily available source of liquid fuel is essential; therefore, agriculture and farming sectors throughout the world are looking for ways of controlling their own liquid fuel supplies. In the developing countries whose agriculture-based economics are particularly vulnerable to fuel shortages, the. need to become less dependent on oil imports and to ensure the continuation of agriculture activities with their own resources is even more important. A biomass-based technology is an alternative path to the energy development process in these countries and will eventually help to ease the burden of oil importation on their economics. As a source of biomass for producing liquid fuel, the majority of investigations have concentrated on vegetable oils and their derivarives since they seem to have the potential to be used as fuel alternatives for Diesel engines. There are more than 350 oil-bearing crops identified, among which only sunflower, safflower, soybean, cottonseed, rapeseed, and peanut oils are condsidered as porential alternative fuels for diesel engines. The major problems associated with the use of vegetable oils in the compression ignition engines are caused by their high fuel viscosity, which is approximately 10 times of that of Grade No.2-D diesel fuel. Dilution, microemulsification, pyrolysis, and transesterificarion are the four techniques applied to solve the problems encountered with the high fuel viscosity. Among these techniques developed for reducing the high viscosity of vegetable oils, chemical conversion of the oil through transesterification with short-chain alcohols, such as methanol and ethanol, to its corresponding fatty ester appears to be the most promising solution. The product of transesterification reaction is named as Diesel-Bi, Bio-Diesel, Biqftiel, Di-ester, Green ester. These names are used for the methyl ester products of rape, soybean, and sunflower oil. In our study ester fuels will be named as Bio-Diesel.The aim of the conversion of vegetable oils in their methyl esters can be classified as follows: 1. The complete removal of the glycerids, 2. Lowering the boiling point of the oil, 3. Lowering the flash point of the oil, 4. Lowering the pour point of the oil, 5. Lowering the viscosity of the oil, 6. The usage of glycerin in chemical industry, 7. The usage of the byproducts in soap and detergent industry. The purity level of the Bio-Diesel has strong effects on its fuel properties. Especially the amount of glycerids and triglycerids present in the fuel can cause serious problems. Another factor that must be taken in account is that the fuel must almost be free of water, alcohol, glycerin, and catalyst. Intensive studies have been performing in European countries aiming the control of the purity level of the Bio-Diesel through chromatographic and analytical ways. In European countries the properties of alternative fuels are restricted. According to these restrictions the free fatty acids, methanol, glycerin, and water content of the Bio-Diesel must have a minimum value and the fuel must be 99% pure. Therefore the refinement step of the products obtained by the transesterification reaction is extremely important. There aren't any significant problems in performing its reaction, but when it cpmes to obtain the Bio-Diesel from the product mixture several technical problems must be overcomed and therefore the operation cost can be increased. The target of this study was to investigate the refinement of the product mixture obtained by the transesterification reaction of rapeseed oil ( extracted from the seeds of the rape plant cultivated in the Thrace region of Turkey ) with methanol. In the theoretical study the properties of rapeseed and its oil, the production, refinement and the properties of the Bio-Diesel, and the application of this alternative fuel in European countries was investigated. In experimental study the characteristics of the crude and refined rapeseed oils were determined and three refinement methods were applied to the product mixture. The technological characteristics of the crude and refined rapeseed oil are given in Table 1. As can be seen from this Table the crude oil contains 2.2% by weight free fatty acids. Due to this free fatty acid content the catalyst (NaOH) had saponified during the transesterification reaction and lost its activity that resulted in a poor ester yield. Taking this fact into account it is decided to remove the free fatty acids prior to the transesterification reaction The reaction conditions are cited below: Vegetable oil/ Alcohol molar ratio : 1 :6 Temperature : 65 ± 1 °C Time : 38 minutes Catalyst : 1.8% NaOH by the weight of oil viTable 1. The technological characteristics od crude and refined rapeesed oil. VIIThe removal of free fatty acids of crude rapeseed oil was realized by the neutralization method by which a neutralization. yield of 97% and a refinement factor of 1.5 were obtained. The reaction of neutralized oil with methanol was performed with ester yield of 97%. The reaction conditions are as follows: Vegetable oil/ Alcohol molar ratio : 1:6 Temperature : 65 ± 1 °C Time : 38 minutes Catalyst : 1.7%NaOHby the weight of oil. The product mixture obtained by the transesterification reaction contains fatty acid methyl esters, glycerin, free fatty acids, mono- and diglycerids, soap, excess amount of the used methanol, and NaOH. First of all, the ester product and then the glycerine and the other byproducts must be obtained from this mixture. Taking the previous transesterification applications and our laboratory possibilities into consideration, 3 different refinement methods have been performed in order to obtain the ester product from the mixture: 1. Washing the mixture with hot water, 2. Washing with petroleum ether and water, and 3. Neutralizing the mixture with sulfuric acid. Table 2 shows the refinement yields, water contents and acid values of the Bio-Diesel's obtained through these three methods. A comparison between refinement yields shows us that the highest refinement yield is obtained in the first method in which the mixture is washed with water at 50 °C. The application of the second method gives the possibility of getting a refinement yield of 82.6% but this method requires petroleum ether usage beside the water. In the third method in which the mixture was neutralized with sulfuric acid and the catalyst was in solid state a refinement yield of 81.2% was obtained. This third method has given a refinement yield of 80.9% if the was first dissolved in methanol and then used in the reaction. In the last cited method the acid value and water content of the Bio-Diesel are found to be 6.08 and 0.22% respectively which are not coherent with Bio-Diesel properties according to the European restrictions. In the third method the catalyst has reobtained in the form of the Na2S04 powder. The purity level of the Bio- Diesel is effecting its fuel properties. The water content must be below 0. 1% (wt%) and the acid value must be smaller than 1. As can be seen from Table 2 the best refinement method is that of the washing the product mixture with water that is heated up 50 °C. In this method, beside the usage of hot distilled water also heated Na2S04 has been used, in order to remove the water present in the ester product. The amount of the Na2S04 was 25% by weight of the ester product. To see the effect of diminishing the amount of Na2SC«4 vmOT o B S I (D O 3 t/î 0) u, 4) H Csİ IXon the ester products water content, some other tests were performed. The ester product had let one night along with Na2S04 (20% by weight of the ester product) and then filtrated. In this case, the acid value was decreased to 0.10, the water content and the refinement yield were found to be 0.095% and 86.3% respectively. Since the gap between the 0.095% and the restriction value 1% was too close, the experiments realized with the diminution of Na2S04 were ceased. It's been concluded that the usage of heated Na2S04 20% by weight of the ester product was sufficient for the removal of the water. In our experimental study the glycerin purification and the evaluation of the economical aspects of the refinement processes have not been done. The realization of these studies would certainly give an idea about the application possibility of the refinement with hot water.
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