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MATERIALS AND METHODS Materials All materials used in this experiment were analytical grade and used without further purification i.e. sodium aluminate, TPAOH 1M, TEOS 98%, triethylenetetramine, ethylenediamine, PDD-AM 35%, and deionized water. All materials were purchased from Sigma Aldrich. Deionized water was provided from MilliQ devices. Synthesis of ZSM-5 Zeolite Sodium aluminate, deionized water, TPAOH, and TEOS were mixed at 373 K under vigorous stirring and aged for 3 hours. Molar ratio of the materials were 1Al2O3 : 64.35SiO2 : 10.08(TPA)2O : 3571.66 deionized water [8]. For two other materials, (TPA)2O was replaced with 10.08TETA or 100en [7]. Then, PDD-AM solution was added into the mixture at room temperature and stirred for 48 hours [8]. The mixture was transferred into Teflon-line stainless steel autoclave for further crystallization at 443 K for 144 hours. The product was collected by filtration, washed, and dried. ZSM-5 zeolite was calcined until 823 K and characterized using XRD, FTIR, Surface Area Analyzer, and SEM-EDS. The ZSM-5 zeolites then denoted as ZSM-5_h/t, ZSM-5_h/teta, ZSM-5_h/en. As comparison, microporous ZSM-5 zeolite (ZSM-5_m) was synthesized at the same condition without PDD-AM solution as secondary template. Preparation of H/ZSM-5 H/ZSM-5 zeolites were prepared through ion exchange-treatment using 1 M ammonium nitrate solution with ratio 1:50. The mixture was heated at 333 K for 6 hours. The products were filtered, dried, and calcined at 823 K to remove all ammonia and produced H/ZSM-5. Catalytic Cracking Test The catalytic activity of H/ZSM-5 zeolites was tested using micro activity test (MAT) reactor at 773 K using n- hexadecane as feed. The catalyst was weighed for about 0.5 g and put into silica reactor. Catalyst was purged with N2 gas to remove all impurities at temperature of 573 K for 30 min. Then, feed n-hexadecane was weighed about 1.35 grams and injected into reactor for 80 s. Liquid and gas products were collected in a liquid receiver and in Teddlar bag for gases. After injected feed, nitrogen gas was purged into reactor to pull out all feed in syringe pump. RESULTS AND DISCUSSION Catalyst Characterization Figure 1 and Fig. 2 showed the XRD pattern of the as-synthesized ZSM-5 zeolites and their modification into H/ZSM-5. Figure 1 showed that the as-synthesized ZSM-5_h/en and ZSM-5_h/teta showed weak intensity at those position 2θ indicating that ZSM-5 zeolites did not well formed. Therefore, further characterization were not employed on both materials. The XRD powder pattern of ZSM-5_h/t and ZSM-5_m showed the strong intensity of ZSM-5 characteristic peak in position 2θ of 7-9° and 22-25° [9]. According to Fig. 1, ZSM-5_h/t had lower intensity than ZSM-5_m indicating that the presence of secondary template can decrease the crystallinity of ZSM-5. Therefore, only those last materials that subjected to ammonium ion exchange treatment to obtain H/ZSM-5. For H/ZSM-5_m and H/ZSM-5_h/t zeolites showed the same powder pattern to ZSM-5_m and ZSM-5_h/t, indicating that the modification did not destroy their primary structure. The result of surface area analysis was showed in Table 1. The surface area and the average of pore diameter for ZSM-5_h/t were larger than ZSM-5_m. This data was supported by isotherm adsorption – desorption curve that for ZSM-5_h/t showed in Fig. 3. The broad hysterical loop at 0.7 to 0.9 P/P ̊ only appeared in ZSM-5_h/t, indicating the presence of mesoporous in this sample. Furthermore, according to Table 1, ZSM-5_h/t has lower surface area than ZSM-5_m. This result indicated that the adding of secondary template could cause more amorphous ZSM-5 zeolite, as match as XRD result. 020088-2PDF Image | ZSM-5 zeolite using various templates as cracking catalysts
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