Hydrodesulfurization of Thiophene over Platinum Supported on Metal Oxide Catalysts
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1 Muroran-IT Academic Resources Title Hydrodesulfurization of Thiophene o on Metal Oxide Catalysts Author(s) 神 田, 康 晴 ; 小 林, 隆 夫 ; 上 道, 芳 夫 ; 杉 岡, 正 敏 Citation 室 蘭 工 業 大 学 紀 要 No.55, pp.33-38, 25 Issue Date URL Rights Type Journal Article See also Muroran-IT Academic Resources Archiv Muroran Institute of Technology
2 Mem. Muroran Inst. Tech., 55 (25) 33~38 Hydrodesulfurization of Thiophene over Platinum Supported on Metal Oxide Catalysts Yasuharu KANDA*, Takao KOBAYASHI*, Yoshio UEMICHI* and Masatoshi SUGIOKA* (Received 23 May 25, Accepted 2 September 25) Abstract The catalytic activities of platinum (Pt) supported on various metal oxides (MO X ; Al 2 O 3, SiO 2, TiO 2, MgO and ZnO) for hydrodesulfurization (HDS) of thiophene were investigated. HDS activities of supported Pt catalysts were examined at 35 o C by using conventional fixed bed flow reactor under atmospheric pressure. The order of HDS activities of Pt/MO X was as follows; Pt/Al 2 O 3 > Pt/SiO 2 > Pt/TiO 2 > Pt/MgO > Pt/ZnO. Catalytic properties of MO X supports and Pt/MO X were evaluated by nitrogen adsorption, decomposition of 2-propanol (2-PA), XRD and hydrogen adsorption. It was revealed that HDS activities of Pt/MO X catalysts were not correlated to BET surface area and acid-base properties of MO X but these were strongly correlated to the dispersion of Pt on MO X. Keywords: Hydrodesulfurization, Metal oxides, Noble metal, Supported platinum catalyst 1 INTRODUCTION Hydrodesulfurization (HDS) of petroleum feedstocks is one of the most important processes to produce clean fuels in the petroleum industry (1)(2). The CoMo/Al 2 O 3 catalyst is widely used in the HDS process of petroleum. Recently, the development of highly active HDS catalysts, which are more active than commercial CoMo/Al 2 O 3 HDS catalyst, has been claimed in the petroleum industry to produce much lower sulfur content fuels against the serious problems of environmental pollution on a global scale by acid rain caused by burning petroleum (3)(4). Supported noble metal catalysts have been proposed as new HDS catalysts (5)(6)(7). We reported that noble metals, especially platinum, supported on zeolites (8)(1)(12) and related materials (9)(11)(13)(14) exhibit high activity for the HDS of organic sulfur compounds and these catalysts have high potential as second generation HDS catalysts. In the present work, we investigated the catalytic *Department of Applied Chemistry, Muroran Institute of Technology performance of Pt supported on various metal oxides (MO X ) such as Al 2 O 3, SiO 2, TiO 2, MgO and ZnO for the HDS of thiophene as a model reaction of HDS of petroleum feedstocks. 2 EXPERIMENTAL Pt/MO X catalysts were prepared by an impregnation method using hydrogen hexachloroplatinate hexahydrate (H 2 PtCl 6 6H 2 O) aqueous solution and the amount of Pt loading was 5 wt%. After impregnation, the catalysts were calcined at 5 o C for 4 hrs in air and were reduced at 45 o C for 1 hr. Presulfiding treatment of the catalyst was performed by 5 vo1% H 2 S-H 2 mixture at 4 o C for 1 hr. Hydrodesulfurization of thiophene over Pt/MO X was carried out at 35 o C in a conventional fixed bed flow reactor under 1 atm. Thiophene was introduced into the reactor by passing hydrogen (3ml/min) through a thiophene trap cooled at o C in the HDS of thiophene. The HB2B/thiophene molar ratio (mol/mol) was 3. Reaction products in the HDS of thiophene were analyzed by gas chromatography (FID). BET surface area was measured by nitrogen 33
3 Yasuharu KANDA, Takao KOBAYASHI, Yoshio UEMICHI and Masatoshi SUGIOKA adsorption at liquid nitrogen temperature (-196 o C). Acidic and basic properties of MO X were evaluated by decomposition of 2-propanol (2-PA) using pulse reactor at 2 o C. Helium was employed as a carrier gas. Dispersion of Pt on MO X was measured by hydrogen adsorption method at 25 o C. Catalysts were pretreated by evacuation at 5 o C for 1 hr, and then reduced by hydrogen (2 Torr) at 45 o C for 1 hr and evacuation at the same temperature for 1 hr. XRD patterns of supported Pt catalysts were measured by using Rigaku diffractmeter with Cu K α radiation. 3 RESULTS AND DISCUSSION 3. 1 Catalytic Activities of Pt Supported on MO X for HDS of Thiophene The catalytic activities of Pt supported on various MO X such as Al 2 O 3, SiO 2, TiO 2, MgO and ZnO for the HDS of thiophene were examined at 35 o C. It was found that Pt/Al 2 O 3 catalyst showed the highest initial activity among Pt/MO X catalysts, but this activity was decreased with reaction time as shown in Fig. 1, probably due to the poisoning by hydrogen sulfide and/or carbon deposit. The order of the HDS activities of Pt/MO X catalysts after reaction for 2 hrs was as follows: Pt/Al 2 O 3 > Pt/SiO 2 > Pt/TiO 2 > Pt/MgO >> Pt/ZnO. The reaction products in the HDS of thiophene over reduced Pt/Al 2 O 3 were mainly C 4 hydrocarbons (butanes 93%, butenes 6%) and trace amount of C 1 -C 3 hydrocarbons as shown in Table 1. These results indicate that high catalytic activity of Pt/Al 2 O 3 for thiophene HDS was attributed to high hydrogenating ability for unsaturated C 4 hydrocarbons formed in the HDS of thiophene in the presence of hydrogen sulfide Al 2 O 3 SiO 2 TiO 2 MgO Time on stream (hr) W/F = 37.9 g hr/mol, H 2 /Tiophene = 3 Fig. 1 Hydrodesulfurization of thiophene over Pt/MO X catalysts at 35 o C. We reported in the previous paper (15) that HDS activities of Rh/Al 2 O 3 and Rh/SiO 2 catalysts were considerably enhanced by presulfiding treatment. Thus, we examined the catalytic activities of presulfided Pt/MO X for HDS of thiophene at 35 o C. The catalytic activity of Pt/SiO 2 was enhanced by the presulfiding treatment and this activity was the almost same as that of Pt/Al 2 O 3 catalyst as shown in Fig. 2. However, HDS activities of other Pt/MO X were decreased (Pt/Al 2 O 3, Pt/TiO 2 ) or hardly changed (Pt/MgO, Pt/ZnO) by presulfiding treatment. Al 2 O 3 SiO 2 TiO 2 MgO ZnO Reduced Sulfided W/F = 37.9 g hr/mol, H 2 /Tiophene = 3 Fig. 2 Catalytic activities of Pt supported on MO X for the HDS of thiophene at 35 o C Characterization of MO X Supports and Pt/MO X Catalysts BET Surface Area of MO X We also carried out the characterization of MO X and Pt/MO X in order to clarify the cause of high activity of Pt/Al 2 O 3 catalyst in the HDS of thiophene. Figure 3 shows the BET surface area of MO X and HDS activity of Pt/MO X catalyst. Al 2 O 3 and SiO 2 have high surface area (ca. 3 m 2 /g). However, surface area of MgO and ZnO were lower than these of Al 2 O 3 and SiO 2. Figure 4 shows the relationship between BET surface area of MO X and HDS activities of Pt/MO X catalysts. These results indicate that HDS activity of Pt/MO X was independent of BET surface area of MO X as supports Acidic and Basic Properties of MO X Since propylene and water are formed on acidic sites of solid acid catalysts and acetone and hydrogen are formed on basic sites of solid base catalysts in the decomposition of 2-propanol (2-PA), the acidic and basic properties of various MO X can be evaluated by the decomposition of 2-PA. We examined the catalytic 34
4 Hydrodesulfurization of Thiophene over Platinum Supported on Metal Oxide Catalysts activity and selectivity of various MO X in the decomposition of 2-PA at 2 o C. We found that Al 2 O 3 showed high activity for the dehydration of 2-PA, but other MO X showed very low activity for the decomposition of 2-PA as show in Fig. 5. These results indicate that Al 2 O 3 has high acidity and other MO X have very low acidity and basicity. Figure 6 shows the relationship between catalytic activities of MO X for 2-PA dehydration and HDS activities of Pt/MO X catalysts. It was revealed that HDS activity of Pt/MO X catalyst was not correlated to the acidic and basic properties of MO X. Table 1 Product distribution over Pt/MO X catalysts in HDS of thiophene at 35ºC. Catalyst HDS (%) < C 3 (%) a) C 4 (%) b) C = 4 (%) c) 1,3-C = 4 (%) d) Pt/Al 2 O 3 (reduced) Pt/Al 2 O 3 (presulfided) Pt/SiO 2 (reduced) Pt/SiO 2 (presulfided) Pt/TiO 2 (reduced) Pt/TiO 2 (presulfided) Pt/MgO (reduced) Pt/MgO (presulfided) Pt/ZnO (reduced) Pt/ZnO (presulfided) a) C 1 -C 3 hydrocarbons, b) butanes, c) butenes, d) 1,3-butadiene BET surface area (m 2 /g) BET surface area 8 HDS activity Al 2 O 3 SiO 2 TiO 2 MgO ZnO Fig. 3 BET surface area of MO X and HDS activities of Pt/MO X catalysts Conversion of thiophene HDS (%) Al 2 O 3 SiO 2 TiO 2 MgO BET surface area (m 2 /g) Fig. 4 Relationship between BET surface area of MO X and HDS activities of Pt/MO X catalysts Dispersion of Pt on Metal Oxides Figure 7 shows the XRD patterns of Pt/MO X catalysts before reduction. The peaks of Pt were not observed on Al 2 O 3, but these on SiO 2 were observed as shown in Fig. 7 (a). This indicates that the dispersion of Pt on Al 2 O 3 was higher than that on SiO 2. The peak height of Pt on TiO 2 and MgO was larger than that on SiO 2 as shown in Fig. 7 (b) and Fig. 7 (c). In the Pt/ZnO, the peaks of Pt were not observed, but peaks of Zn 2 PtO 4 were observed as shown in Fig. 7 (d). This result indicates that dispersion of Pt on ZnO was remarkably lower than these on other MO X. Furthermore, we examined the dispersion of Pt on MO X. Figure 8 shows the dispersion of Pt on MO X measured by hydrogen adsorption method at 25 o C. It was found that dispersion of Pt on MO X was changed by the kind of MO X. The order of the Pt dispersion on MO X was as follows; Pt/Al 2 O 3 > Pt/SiO 2 > Pt/TiO 2 > Pt/MgO >> Pt/ZnO. This order was the same as that of the HDS activities of Pt/MO X catalysts. The catalytic activities of Pt/MO X were strongly correlated to the dispersion of Pt on MO X as shown in Fig. 9. This means that HDS activity of Pt/MO X catalyst was remarkably controlled by the dispersion of Pt on MO X supports. 35
5 Yasuharu KANDA, Takao KOBAYASHI, Yoshio UEMICHI and Masatoshi SUGIOKA PA to propylene 2-PA to acetone HDS activity Al 2 O 3 SiO 2 TiO 2 MgO ZnO Conversion of thiophene HDS (%) Al 2 O 3 SiO 2 TiO 2 MgO Conversion of 2-PA dehydration (%) Fig. 5 Catalytic activities of MO X for decomposition of 2-propanol (2-PA) and HDS activities of Pt/MO X catalysts. Fig. 6 Relationship between catalytic activities of MO X for 2-propanol (2-PA) dehydration and HDS activities of Pt/MO X catalysts. (a) Pt/Al 2 O 3 and Pt/SiO 2 (d) Pt/TiO 2 Pt/SiO 2 Pt/Al 2O 3 Pt γ-al 2 O 3 Pt TiO 2 (Anatase) (c) Pt/MgO (d) Pt/ZnO Pt MgO ZnO Zn 2PtO Fig. 7 XRD patterns of Pt supported on MO X (a) Pt/Al 2 O 3 and Pt/SiO 2, (b) Pt/TiO 2, (c) Pt/MgO and (d) Pt/ZnO before reduction. 36
6 Hydrodesulfurization of Thiophene over Platinum Supported on Metal Oxide Catalysts Dispersion (H mol/pt mol) Dispersion of Pt 8 HDS activity 6 Al 2 O 3 SiO 2 TiO 2 MgO ZnO 4 2 Conversion of thiophene HDS (%) Al 2 O 3 SiO 2 TiO 2 MgO Dispersion of Pt (H mol/pt mol) Fig. 8 Dispersion of Pt on MO X and HDS activities of Pt/MO X catalysts. Fig. 9 Relationship between dispersion of Pt on MO X and HDS activities of Pt/MO X catalysts. 4 CONCLUSION It was found that HDS activities of Pt/MO X catalysts were not correlated to BET surface area and acid-base properties of MO X. However, the activities of Pt/MO X catalysts were strongly correlated to the dispersion of Pt on MO X. It is concluded that high dispersion of Pt on MO X supports is essential to prepare highly active MO X -supported Pt catalysts for the HDS of petroleum feedstocks. REFERENCES (1) Topsøe, H., Clausen, B. S. and Massoth, F. E., Catal.- Sci. Tech., 11, (1996), p1-31. (2) Whitehurst, D. D., Isoda T. and Mochida, I., Adv. Catal., 4, (1998), p (3) Sugioka, M., PETROTECH (in Japanese), 19, (1996), p (4) Okamoto, Y., PETROTECH (in Japanese), 27, (24), p (5) Nagai, M., Koizumi, K. and Omi, S., Sekiyu Gakkaishi, 4, (1997), p (6) Reddy, K. M., Wei, B. and Song, C., Catal. Today, 43, (1998), p (7) Wang, A., Wang, Y., Kabe, T., Chen, Y., Ishihara, A. and Qian, W., J. Catal., 199, (21), p (8) Sugioka, M., Erdöl & Kohle, Erdgas, Petrochemie, 48, (1995), p (9) Sugioka, M., Andalaluna, L., Morishita, S. and Kurosaka, T., Catal. Today, 39, (l997), p6l-67 (1) Sugioka, M., Sado, F., Kurosaka, T. and Wang, X., Catal. Today, 45, (1998), p (11) Sugioka, M., Morishita, S., Kurosaka, T., Seino, A., Nakagawa, M. and Namba, S., Stud. Surf. Sci. Catal., 125, (1999), p (12) Kurosaka, T., Sugioka, M. and Matsuhashi, H., Bull. Chem. Soc. Japan, 74, (2l), p (13) Sugioka, M. and Kurosaka, T., J. Japan Petrol. Inst., 45, (22), p (14) Kanda, Y., Kobayashi, T., Uemichi, Y. and Sugioka, M., Stud. Surf. Sci. Catal., 156, (25), p (15) Sugioka, M., Kanda, Y., Kobayashi, T. and Uemichi, Y., Mem. Muroran Inst. Tech., 54, (24), p
7 Yasuharu KANDA, Takao KOBAYASHI, Yoshio UEMICHI and Masatoshi SUGIOKA 白 金 担 持 金 属 酸 化 物 触 媒 によるチオフェンの 水 素 化 脱 硫 反 応 神 田 康 晴 *, 小 林 隆 夫 *, 上 道 芳 夫 *, 杉 岡 正 敏 * 種 々の 金 属 酸 化 物 (MO X ;Al 2 O 3,SiO 2,TiO 2,MgO,ZnO)に 担 持 した 白 金 (Pt) 触 媒 のチオフェ ン 水 素 化 脱 硫 (HDS) 反 応 に 対 する 活 性 (35 o C)について 検 討 した. 担 持 白 金 触 媒 のHDS 活 性 は 常 圧 固 定 床 流 通 式 反 応 装 置 を 用 いて 検 討 した.その 結 果,Pt/MO X のHDS 活 性 の 序 列 はPt/Al 2 O 3 > Pt/SiO 2 > Pt/TiO 2 > Pt/MgO > Pt/ZnOとなることがわかった.MO X 担 体 の 表 面 積, 酸 塩 基 特 性 およびPtの 分 散 度 を 窒 素 吸 着 法,2-プロパノールの 分 解 反 応,XRDおよび 水 素 吸 着 法 で 評 価 し たところ,Pt 担 持 MO X 触 媒 のHDS 活 性 はMO X のBET 表 面 積 および 酸 塩 基 特 性 には 依 存 しない が,Ptの 分 散 度 に 強 く 依 存 することが 明 らかとなった. キーワード: 水 素 化 脱 硫, 金 属 酸 化 物, 貴 金 属, 担 持 白 金 触 媒 * 応 用 化 学 科 38
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