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Selective Cracking of Natural Gasoline Over HZSM-5 Zeolite

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Selective Cracking of Natural Gasoline Over HZSM-5 Zeolite FUEL PROCESSING TECHNOLOGY 89 (2008) 819– 827 www.elsevier.com/locate/fuproc Selective cracking of natural gasoline over HZSM-5 zeolite Marcelo J.B. Souzaa, Fabiano A.N. Fernandesb,⁎, Anne M.G. Pedrosac, Antonio S. Araujoc aUniversidade Federal de Sergipe, Departamento de Engenharia Química, Cidade Universitária Prof. José Aloísio de Campos, CEP 49100-000, Aracaju/SE, Brazil bUniversidade Federal do Ceará, Departamento de Engenharia Química, Campus do Pici, Bloco 709, 60455-760, Fortaleza/CE, Brazil cUniversidade Federal do Rio Grande do Norte, Departamento de Química, Campus Universitário, 59078-970, Natal/RN, Brazil ARTICLE INFO ABSTRACT Article history: This work presents a study on the catalytic cracking of natural gasoline (extracted from Received 29 October 2007 natural gas) over HZSM-5 zeolite. A factorial planning was carried out to evaluate the effect Received in revised form of temperature and W/F ratio on the cracking of natural gasoline, analyzing their effects on 13 December 2007 conversion and product distribution using an analysis based on surface response Accepted 31 December 2007 methodology. The process was optimized focusing on the maximization of the mass fractions and the production of specific products such as ethene, propene and butanes. The Keywords: results have shown that the maximum selectivity and hourly mass production of ethene is Natural gasoline obtained at high temperature (450 °C) and low catalyst weight to flow rate ratio (W/F) (7.2 to Cracking 8.2 gcat h/mol). Maximum selectivity of propene is obtained at 350 °C and 7.0 gcat h/mol, while Zeolite HZSM-5 the best condition for maximum mass production is found at 421 °C and 5.7 gcat h/mol. The Optimization highest mass production of butanes is favored by high temperature (450 °C) and mid range Neural network W/F ratios (12.1 gcat h/mol), while the highest selectivity is found at low temperature (350 °C). © 2008 Elsevier B.V. All rights reserved. 1. Introduction in yield and selectivity will have a very significant economical and ecological impact. These improvements can be obtained Natural gas is a mixture of hydrocarbons such as methane at many levels, from the design of new and improved catalysts (main component), ethane, propane, butane and nature gaso- to the optimization of reaction conditions [2]. In this work a line (pentane, hexane and heptane). During the processing of new zeolite-based catalyst was developed and the best natural gas, natural gasoline cut is condensed and separated operating condition for the reaction was investigated. from the gaseous products. It can be sold as such or can be Zeolites are used in catalytic and separation technologies, cracked selectively to produce other hydrocarbons such as especially, in processing of hydrocarbons; therefore, their ethene and propene to the plastic industry or as propane and adsorptive properties are considered important. Adsorption of butane to LPG (liquefied petroleum gas) production. n-pentane, n-hexane and n-heptane on MFI-type molecular Hydrocracking is an important process in the petroleum sieves (HZSM-5 zeolites) has attracted attention of many refining industry to produce feedstocks. Current hydrocrack- researchers because of the complex adsorption profiles ing processes are based on commercial catalysts that are observed in this system [3–8]. The adsorption isotherms of effective above 450 °C. The development of new catalysts that n-pentane and n-hexane on MFI show a step at the loading can present high activity under lower temperatures may corresponding to four molecules per unit cell [3–5].The increase the operational and economical benefits of hydro- adsorption of n-hexane observed on MFI molecular sieves cracking processes [1]. follows a two-step adsorption pathway due to two different Hydrocracking is also the industrial process with the adsorption sites in the micropore system, fact supported by largest consumption of catalyst and even small achievements satisfactory fitting of adsorption profiles with functions ⁎ Corresponding author. Tel.: +55 85 33669611; fax: +55 85 33669610. E-mail addresses: [email protected] (M.J.B. Souza), [email protected] (F.A.N. Fernandes). 0378-3820/$ – see front matter © 2008 Elsevier B.V. All rights reserved. doi:10.1016/j.fuproc.2007.12.014 820 FUEL PROCESSING TECHNOLOGY 89 (2008) 819– 827 Fig. 1 – Scheme of the catalytic reactor. Where: G1 = nitrogen; G2 = helium; V1, V2, = 4 way valves; CF1, CF2, CF3 = flux valves; B = saturator; P = 10 way pneumatic valve; CT1, CT2 = temperature controllers; T1, T2 = thermocouples; S = vent; C = chromatogram; CG = gas chromatograph; F = oven e R = reactor with catalyst. derived from the dual-site Langmuir adsorption model. It is 2.2. Natural gasoline hydrocracking reaction assumed that the molecules are adsorbed either in the straight or in the zigzag channels, since they have smaller diameter The experiments were carried out in a catalytic fixed-bed reactor than the intersections, ensuring stronger interaction of the operating at continuous flow rate and atmospheric pressure. A reactor made of quartz with 0.15 m in length and 0.015 m in diameter adsorbed molecules with the zeolite lattice [8,9]. The stronger was used. A scheme of the reaction apparatus is shown in Fig. 1. interaction of adsorbed n-hexane and also of n-pentane with Prior to the reaction, the catalyst (HZSM-5 zeolite) was the zeolite lattice can be an advantage for cracking reactions, activated in situ at 450 oC for 2 hours under a flow of dry nitrogen reason for which this zeolite was selected as a catalyst the (20 mL/min). The fine powder catalyst sample (0.4 g) was loaded cracking of natural gasoline. into the micro-flow reactor and a thermocouple was placed on the Catalytic cracking involves a very complex reaction scheme center of the catalyst bed to monitor the reaction temperature. operating on the solid catalyst. The complexity of real feeds Fine powder catalyst was used to avoid any mass transfer effects. The reaction was performed diluting C5+ vapor (natural and the number of reactions involved requires a large volume gasoline) with nitrogen under constant flow rate. Liquid natural of calculations in addition to the problem of the number gasoline was fed into the saturator and was totally gasified of unknown kinetic parameters that requires estimation. previous to reaction to ensure constant composition of the feed To overcome the difficulties in dealing with such detailed stream. The C5+ vapor to nitrogen ratio was maintained at 1.6 in models, the optimization of the reaction condition was carried all runs. An experimental planning was designed to study the out using stacked neural networks. effects of temperature and catalyst weight to flow rate ratio (W/F) over the cracking selectivity and the conversion. Temperatures between 350 and 450 °C and W/F ranging from 5 to 17 gcat h/mol were applied in the experiments. The operating conditions used 2. Materials and methods in the experimental planning are presented in Table 1. The composition of the natural gasoline used in the experiments is 2.1. Catalyst Preparation Table 1 – Experimental planning The NaZSM-5 Zeolite was prepared by hydrothermal crystal- Run Experimental condition lization [10] in a steel autoclave at 423 K by 7 days, under autogenous pressure. The gel of synthesis was prepared from a Temperature (°C) W/F (gcat h/mol) mixture containing sodium hydroxide (Merck), aluminum sul- 1 350 16.56 phate (Inlab), silica gel (Riedel de Häen AG), sulfuric acid (Merck) 2 350 9.74 and tetrapropylamoniun bromide (Jansen Chimica), to direct the 3 350 6.90 structure of the ZSM-5 zeolite [11,12]. The gel molar composition 4 350 5.18 was 48.8 SiO2. 1.0 Al2O3: 14.3 Na2O: 2.4 (TPA)2O: 180 H2O. The 5 400 16.56 synthesis product was filtered, washed with distilled water and 6 400 9.74 dried for 10 h at 393 K. The sample was calcined at 773 K in 7 400 6.90 nitrogen flow by 15 h, and in dry air by 10 h, at the same 8 400 5.18 temperature. The HZSM-5 was obtained by ion exchange of a 9 450 16.56 NaZSM-5 zeolite, with 0.6 M ammonium chloride solution, and 10 450 9.74 subsequently calcined [12]. The HZSM-5 zeolite was characterized 11 450 6.90 by atomic absorption (Varian AA-175), X-ray diffraction (Rigaku) 12 450 5.18 and Scanning Electron Microscopy (SEM, Zeiss). FUEL PROCESSING TECHNOLOGY 89 (2008) 819– 827 821 Table 2 – Chemical composition of natural gasoline, data and the domain used for training purposes [13–15]. The provided by Petrobras-UPGN Guamaré (components optimization procedure is summarized in Figs. 2 and 3. Fig. 2 mass fractions) shows schematically the procedure to select the neural networks and Fig. 3 shows the procedure used to find the best operating n-Hexane 0.124 conditions with the trained set of neural networks. n-Pentane 0.404 In this work, the back propagation algorithm was used, as it is 2-methyl-pentane 0.094 the most extensively adopted algorithm for neural networks and 2-methyl-butane 0.305 performs well. The available data were split in two sets. One set Cyclopentane 0.028 was used to train the network and the other to test its prediction Cyclobutane 0.036 capability. The activation sigmoid function used in the neural network is given by Eq. (1). A random selected bias was used, and weights were updated by a Hessian approach. shown in Table 2 and were provided by Petrobras (UPGN Guamaré, RN, Brazil). 1 Under the given conditions, C5+ underwent cracking to C2, C3 y ¼ P ð1Þ 1 þ expðÞÀ x and C4 paraffins and C2 and C3 olefins.
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