AWERProcedia Advences in Applied Sciences

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1 AWERProcedia Advences in Applied Sciences Vol 1 (2013) st Global Conference on Environmental Studies 2013 Synthesis of Zeolites from Fly Ashes the Industrial Scale Lidia Bandura*, Department of Geotechnics, Lublin University of Technology, Nadbystrzycka 40, Lublin, Poland. Wojciech Franus, Department of Geotechnics, Lublin University of Technology, Nadbystrzycka 40, Lublin, Poland. Rafał Panek, Department of Geotechnics, Lublin University of Technology, Nadbystrzycka 40, Lublin, Poland. Magdalena Wdowin, Division of Geotechnology, Mineral and Energy Economy Research Institute of the Polish Academy of Sciences, Wybickiego 7, Krakow, Poland. Suggested Citation: Bandura, L., Franus, W., Panek, R. & Wdowin, M. Synthesis of Zeolites from Fly Ashes the Industrial Scale AWERProcedia Advances in Applied Sciences. [Online]. 2013, 1, pp Available from: Proceedings of Gobal Conference on Environmental Studies (CENVISU-2013), April 2013, Zeynep Sentito Hotel, Belek Antalya, Turkey Received December 14, 2012; revised January 17, 2013; accepted March 03, Selection and peer review under responsibility of Dr. Nehir Varol Academic World Education & Research Center. All rights reserved. Abstract This study presents a technological line prototype, on the basis of which it is possible to obtain the zeolite materials based on hydrothermal reaction of fly ashes with sodium hydroxide. This technological solution allows to obtain three types of zeolite products: Na-P1 type, mixture of Na-P1/Linde-A and mixture of Na-P1/Linde- A/Na-X. the final product is dependent on the parameters of the synthesis process. The resulting zeolite materials, in relation to the fly ash, had much better surface/sorption properties, which are crucial for the potential application in environmental engineering. These materials can be used in: Removal of hydrocarbon substances, Removal of heavy metal ions from waste water, Removal of radionuclides from mine water. * ADDRESS FOR CORRESPONDENCE: Lidia Bandura, Department of Geotechnics, Lublin University of Technology, Nadbystrzycka 40, Lublin, Poland, address: / Tel.:

2 Fly ashes, which are waste materials, can be applied in the synthesis of low cost zeolites, whose chemical, morphological and textural properties are promising from the environmental protection point of view. Keywords: zeolites, fly ash, industrial technology; 1. Introduction Zeolites are microporous, hydrated aluminosilicates of alkali elements, alkaline earth metals or other cations, which contain in their crystal structure a numerous of channels and chambers of different sizes (in the order of several angstroms), giving them a number of characteristic sorption properties, ion exchange, molecular-sieve and catalyst. Thanks to those properties, they are widely used mineral resources in many areas of industry, agriculture, medicine, chemical technology, environmental protection and engineering. Natural zeolites, represented by more than 100 minerals, are formed in different geological environments and often create various mineral forms. Some of them occur in the form of accumulations, which are viable for extraction and processing. Among the most important zeolites forming deposits can be distinguished clinoptilolite, philipsite, chabazite and mordenite. At the end of the last century manufacturing technologies of synthetic zeolites began to develop intensively. They allow to obtain zeolites with specific structure parameters which qualifies them for particular industrial applications (e.g., selective molecular sieves). Synthetic zeolites in comparison to the natural zeolites are better mineral resources in industrial technologies, because the natural zeolites generally require costly modifications (of the structure) to the applications in the industry. Although the synthesis process is also associated with specific costs incurred. Thus, a substrate for the synthesis reaction should be a cheap mineral material or waste. Synthetic zeolite materials can be obtained from chemical reagents in a chemical reaction of sodium silicate and sodium aluminate, mineral resources (clay minerals, minerals from the group of silica), and specific waste materials, which are circumstantial combustion products (such as fly ash). Works on this type of chemical reactions are carried out in many research centers. Their particular development is observed at the turn of the twentieth and twenty-first century. The possibilities of using the hard coal fly ash (conventional and fluid bed combustion), as well as the brown coal to synthesis of zeolite materials are shown in a number of papers [1-4]. It is described that for each type of fly ash, using appropriate methodology of laboratory work, it is possible to obtain different zeolite structures as among others: analcime, chabazite, cancrinite, gmelinite, NaP1, ZSM-5, ZSM-28, Na-X, Na-Y, philipsite and sodalite [5, 6]. Despite the widely described process of converting fly ash into zeolites in the laboratory conditions, there is almost no works concerning a method of zeolites synthesis on a ¼ technical scale, which gives the possibility to turn this process on an industrial scale. 2. Methods The test arrangement for synthesis on a ¼ technical scale is shown in Figure 1. On the scheme of the device for manufacturing zeolites 4 processing blocks are shown: The reactor loading block, Reaction block, Separation of the reaction products block, 575

3 The final processing block. The reactor-loading block consists of two storage tanks where granular sodium hydroxide pellets and fly ash are stored. These tanks are connected by two worm gears with a weight tank. The purpose of the two worm gears is the transportation of fly ash and sodium hydroxide pellets from the storage tanks to the weight tank. The tank is made of stainless steel with the symbol l316l. It has the shape of a converse cone head ended by a roller. In order to avoid an excessive dustiness of the room the tank is closed by cap. Figure 1. The prototype line for the synthesis of zeolites from fly ash To provide suitable amount of substrates for the synthesis reaction, the tank is mounted on threeweight stain gauges sensor. In order to improve the dump of substrates (NaOH, fly ash) to the synthesis reaction tank, the worm gears and the weight tank are equipped with pneumatic piston vibrators. The main component of the described line is a reaction tank, where the conversion process of fly ash into zeolites is carried out. Total volume of the tank is 130 dm 3 (working volume is 100 dm 3 ). The tank is equipped with a system of three heaters (2 kw of each), a probe for controlling the reaction temperature, and the level of tank filling probe, and a stirrer, which is sequentially switched on, and is responsible for the homogenization of the material and prevents the aggregation of the material during the reaction process. At the tank outlet a pneumatic membrane is installed that pumps the zeolite material during and after reaction. The separation of the products block consists of a filter press, and the two tanks in which the postreaction aqueous solution of NaOH as well materials rinsing solution from press are stored. The aqueous solution from the first rinsing of the reaction products is directed to the storage tank and then pumped back to the reactor for further synthesis. A solution from rinsing is modified to its original composition, and is directed to the next reaction cycle. 576

4 The volume of water during loading and the volume of solution after modification process and recycling is controlled by flow meters. The final processing block consists of a ribbon feeder and the rotary furnace. The drying step of the zeolite material obtained by filtration of the solution and the calcination is carried out in a rotary furnace. 3. Results and Discussion 3.1.Properties of the obtained zeolite materials On the basis of the above-described prototype of production line, a series of chemical reactions were made in which the final product depends on the following parameters of the process: the type of fly ash, the ratio of ash to the volume of NaOH aqueous solution, NaOH concentration, temperature of process and duration of the reaction. The following synthesis conditions were applied: kg fly ash, kg NaOH, 90 dm 3 technological water, Reaction temperature C, The duration of the synthesis process h. As a result of the process of converting fly ash into zeolite materials based on a proposed technological solution three types of zeolite materials can be obtained from the fly ash (from Kozienice Power Plant). They are as follow: Na-P1, Na-P1/Linde-A and Na-P1/ Na- X/Linde-A. The mineral composition of the zeolite material obtained from the synthesis reaction is shown in Figure 1. The textural properties are presented in Table 1. Using 20 kg fly ash and 12 kg NaOH, 90 dm 3 water, the reaction temperature 80 C and time 36 h the Na-P1 type of zeolite material were obtained. The content of the zeolite phase in this material was 72%. Ion-exchange capacity was 0.54 meqg -1, and a surface area of 77 m 2 g -1. Using 20 kg fly ash and 12 kg NaOH, 90 dm 3 water, the reaction temperature 70 C and time 24 h the mixture of zeolitic material were obtained as the reaction product, which is dominated by Na-P1, with a few percent of weight content of zeolite type Linde-A. The quantitative zeolites content calculated from XRD was 64%. The additional presence of zeolite Linde-A has resulted in increase of ion exchange capacity to 0.63 meqg -1 and a surface area to 82 m 2 g -1, despite a decrease in the content of the zeolite phases in the reaction product. Table 1. Textural properties of zeolite materials received on a technological scale Material S BET [m 2 g -1 ] V mic [cm³ g -1 ] S mic [m 2 g -1 ] V mes [cm³ g -1 ] S mes [m 2 g -1 ] Average pore diameter [nm] Ads. Des. Ads. Des. Ads. Des. Na-P Na-P1/ Linde-A

5 Na-P1/ Linde-A/ Na-X Using 15 kg fly ash and 12 kg NaOH, 90 dm 3 water, the reaction temperature 80 C and time 24 h, were obtained a mixture of zeolite material as the reaction product, in which besides the zeolite Na- P1, Linde-A and Na-X were present. A total weight content of three zeolites was 63% of the mass of the products. The presence of zeolite Linde-A and Na-X has resulted in increase of ion exchange capacity of 0.73 meqg -1 and a specific surface area of 116 m 2 g -1, despite a decrease in the content of the zeolite phase in the obtained reaction product. In the composition of the residue of the reaction products were the remains of unreacted aluminosilicate glass, mullite and quartz Possible directions of use The derived zeolite materials can be widely used in environmental engineering as a multi-pollutant sorbents [7, 8]. Taking into account the textural properties and ion exchange capacity of the zeolites derived on the basis of the technological line, there are few possible directions of use: Removal of hydrocarbon substances, Removal of heavy metal ions from waste waters, Removal of radionuclides from mine water. Laboratory tests of regeneration possibilities of the worked transformer oil (TRAFO) and turbine oil (TU) by the contact refining method showed, that the efficiency in reducing the acid number in comparison with commercial sorbents used to remove such contaminants (i. a., attapulgite, Al 2 O 3, silica gel). The effect of refining on the basis of the acid number [W], for TRAFO oil was about 60% and for TU oil reached almost 80%. The zeolite material in relation to the commercial products, has removed slightly worse the compounds which worsen the colour [R] of the tested oil (e. g., resins, polymers). For the TRAFO oil R varied in the range from 47% to 58%, whilst for TU oil R was significantly lower and ranged from 9% to 18%. Much better bleaching parameters exhibited the commercial sorbents, where R ranged from 27% to 38% for TRAFO oil and from 78% to 85% for TU oil. Obtained zeolites were also tested in the direction of their use as sorbents for petroleum compounds. Sorption capacity study was investigated using Westinghouse method. The experimental data showed, that zeolite sorbents obtained by converting the fly ash has sorption capacity in the range from 1.12 to 1.48 gg -1 for Ecodiesel and from 0.88 to 1.33 gg -1 for biodiesel B100 respectively. Commercial sorbents based on diatomite have sorption capacity at level of 0.65 gg -1. The new direction of application the zeolite minerals can be use them as sorbents for removal of radionuclides present in numerous mine waters, especially in the case of hard coal mining, oil or gas exploration. Large salinitization and reducing conditions cause, that in this type of water the main occurring radionuclides are 226 Ra from uranium series and 228 Ra from thorium series. Water treatment experiments showed that zeolite materials have very high ion selectivity for the radium isotopes. The research for the salt pits water from the coal mine Piast revealed that after passing through the column 120 dm 3 of water in which the concentration of radium isotopes was for 226 Ra and for 228 Ra 7.81 kbqm -3, the elimination level for 226 Ra and 228 Ra was kbqm -3 and 0.10 kbqm -3 respectively, which is the removal of 99%. 578

6 Removal of heavy metal ions from water and wastewater by zeolites is also widely described in literature. Good removal effects are obtained due to a number of physical and chemical properties such as: high cation exchange capacity and the properties of molecular-sieve. In order to determine the efficiency of synthetic zeolites derived on the basis of fly ash, the static and dynamic sorption experiment was investigated. This research involved removal of Zn(II) from the washings derived from galvanizing PZL Swidnik. This study shows, that the zeolite material is a highly effective sorbent for these ions. Zeolite Na-P1 purified to the breakthrough point 429 bed volumes of wastewater and removed meq of Zn(II) in 30 minutes. This allows to drain the treated wastewater into water and soil. 4. Conclusion The proposed method of conversion of fly ash into zeolite material can be a new and very promising development direction of this type of waste, because storage of them has a significant and costly effect on the environment, due to their high dust fractions and sometimes elevated levels of heavy metals and radioactive elements. The developed technology allows to obtain several types of zeolite materials with different physical and chemical properties, which can be used as sorbents for removal of impurities from the water and wastewater treatment. This researches are financed within Project no WND-POIG /09 and PSB1/A2/7/2012. References Querol X., Moreno N., Umaña J. C., Juan R., Hernández S., Fernandez-Pereira C., Ayora C., Janssen M., García- Martínez J., Linares-Solano A., Cazorla-Amoros D. Application of zeolitic material synthesized from fly ash to the decontamination of waste water and flue gas, Journal of Chemical Technology and Biotechnology, 2002, 77, pp Purnomo C. W., Salim C., Hinode H. Synthesis of pure Na X and Na A zeolite from bagasse fly ash, Microporous Mesoporous Materials, 2012, 162 (1), pp Derkowski A., Franus W., Beran E., Czímerová A. Properties and potential applications of zeolitic materials produced from fly ash using simple method of synthesis, Powder Technology, 2006, 166 (1), pp Derkowski A., Franus W., Waniak-Nowicka H., Czímerová A. Textural properties vs. CEC and EGME retention of Na-X zeolite prepared from fly ash at room temperature, International Journal of Mineral Processing, 2007, 82 (2), pp Adamczyk Z., Białecka B. Hydrothermal synthesis of zeolites from Polish coal fly ash, Polish Journal of Environmental Studies, 2005, 14 (6), pp Franus W. Characterization of X-type zeolite prepared from coal fly ash, Polish Journal of Environmental Studies, 2012, 21 (2), pp Franus W., Wdowin M. Removal of ammonium ions by selected natural and synthetic zeolites, Mineral Resources Management, 2010, 26 (4), pp Wdowin M., Franus W., Panek R. Preliminary results of usage possibilities of carbonate and zeolitic sorbents in CO 2 capture, Fresenius Environmental Bulletin, 2012, 21 (12), pp

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