Sn对V_2O_5/Al_2O_3催化剂在异丁烷脱氢反应中的影响
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摘要
以Al_2O_3为载体,采用等体积浸渍法制备了负载型高分散氧化钒催化剂(12%V_2O_5/Al_2O_3),并选择Sn作为助剂对12%V_2O_5/Al_2O_3催化剂的表面性质进行调控,采用XRD、N2等温吸脱附、NH3-TPD、H2-TPR、XPS、TEM和Raman光谱等方法对催化剂进行表征,结合活性评价实验,研究了催化剂表面物种分散状态、酸性和活性物种价态的变化与异丁烷脱氢活性和稳定性之间的关系。表征结果显示,Sn对V_2O_5/Al_2O_3表面的酸性和V物种在催化剂表面的分布和价态具有一定的调节作用,当Sn质量分数为1%时,氧化锡在催化剂表面分散均匀,对表面积和孔结构影响较小,同时,表面酸性变化较小,表面低价态的钒物种增多。活性评价结果表明,该催化剂在临氢反应条件下保持了最佳的脱氢活性及稳定性,异丁烷脱氢反应480min后,异丁烷转化率为46.8%,异丁烯收率为39.8%。
The highly dispersed vanadium oxide catalyst(12%V_2O_5/Al_2O_3) supported by Al_2O_3 was prepared by impregnation. The surface properties of 12%V_2O_5/Al_2O_3 catalyst were controlled by using Sn as an auxiliary agent. The changes in the dispersion state, acidity, and the valence of active species of the catalyst were studied, and their influences on the dehydrogenation activity and stability of isobutane were discussed. The catalysts were characterized by XRD, N2 adsorption-desorption isotherms, NH3-TPD, H2-TPR, XPS, TEM and Raman spectra. The characterization results showed that Sn could regulate the surface acidity of V_2O_5/Al_2O_3 and the distribution and valence state of V species on the surface of the catalyst. When 1%(wt) Sn was added, SnO2 was uniformly dispersed on the surface of the catalyst, and it show little impact on the specific surface area and pore structure. At the same time, the change in surface acidity was small and the vanadium species with low valence increased. The performance evaluation results showed that the catalyst maintained the best reactivity and stability with the presence of hydrogen.After dehydrogenation of isobutane for 480 min, the isobutane conversion was 46.8% and the isobutene yield was 39.8%.
The highly dispersed vanadium oxide catalyst(12%V_2O_5/Al_2O_3) supported by Al_2O_3 was prepared by impregnation. The surface properties of 12%V_2O_5/Al_2O_3 catalyst were controlled by using Sn as an auxiliary agent. The changes in the dispersion state, acidity, and the valence of active species of the catalyst were studied, and their influences on the dehydrogenation activity and stability of isobutane were discussed. The catalysts were characterized by XRD, N2 adsorption-desorption isotherms, NH3-TPD, H2-TPR, XPS, TEM and Raman spectra. The characterization results showed that Sn could regulate the surface acidity of V_2O_5/Al_2O_3 and the distribution and valence state of V species on the surface of the catalyst. When 1%(wt) Sn was added, SnO2 was uniformly dispersed on the surface of the catalyst, and it show little impact on the specific surface area and pore structure. At the same time, the change in surface acidity was small and the vanadium species with low valence increased. The performance evaluation results showed that the catalyst maintained the best reactivity and stability with the presence of hydrogen.After dehydrogenation of isobutane for 480 min, the isobutane conversion was 46.8% and the isobutene yield was 39.8%.
引文
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[2]栗士瑞.异丁烷脱氢制异丁烯生产技术问题探析[J].化工设计通讯, 2016, 42(4):177.LI Shirui. Production of technical problems isobutene dehydrogenation of isobutane[J]. Chemical Engineering Design Communications, 2016,42(4):177.
[3]刘洋,柯明.异丁烷氧化脱氢制异丁烯催化剂研究进展[J].化工进展, 2017, 36(3):909-917.LIU Yang, KE Ming. Research progress on catalysts for oxydehydrogenation of isobutane to isobutene[J]. Chemical Industry and Engineering Progress, 2017, 36(3):909-917.
[4]周庆祥,刘洋,柯明.异丁烷直接脱氢制异丁烯的催化剂的研究进展[J].化学通报, 2017(9):835-844.ZHOU Qingxiang, LIU Yang, KE Ming. Research progress of catalysts for isobutane direct dehydrogenation to isobutene[J]. Chemistry Bulletin, 2017(9):835-844.
[5] SATTLER J J, RUIZ-MARTINEZ J, SANTILLAN-JIMENEZ E, et al.Catalytic dehydrogenation of light alkanes on metals and metal oxides[J]. Chemical Reviews, 2014, 114(20):106-113.
[6] WANG G J, MA H C, LI Y, et al. Dehydrogenation of isobutane over V2O5/γ-Al2O3catalyst[J]. Reaction Kinetics&Catalysis Letters, 2001,74(1):103-10.
[7]曾铁强,缪长喜,吴文海,等.高分散型钒氧化物催化剂上异丁烷催化脱氢的研究[J].化学世界, 2014, 55(9):524-529.ZENG Tieqiang, MIAO Changxi, WU Wenhai, et al. Dehydrogenation of isobutane to isobutene over highly dispersed VOx spercies[J].Chemical World, 2014, 55(9):524-529.
[8]孙楠楠,王国玮,韩东敏,等. V2O5负载量对VOx/MgAl2O4催化异丁烷脱氢制异丁烯的影响[J].石油炼制与化工, 2014, 45(4):45-49.SUN Nannan, WANG Guowei, HAN Dongmin, et al. Effect of V2O5load on VOx/MgAl2O4catalytic dehydrogenation of isobutane to isobutylene[J]. China Petroleum Processing Petrochemical Technology, 2014, 45(4):45-49.
[9] RODEMERCK U, SOKOLOV S, STOYANOVA M, et al. Influence of support and kind of VOx species on isobutene selectivity and coke deposition in non-oxidative dehydrogenation of isobutane[J]. Journal of Catalysis, 2016, 338:174-183.
[10] MCGREGOR J, HUANG Z, SHIKO G, et al. The role of surface vanadia species in butane dehydrogenation over VOx/Al2O3[J]. Catalysis Today, 2009, 142(3/4):143-151.
[11] WACHS I E, WECKHUYSEN B M. Structure and reactivity of surface vandium oxide species on oxide supports[J]. Applied Catalysis A:General, 1997, 157(1/2):67-90.
[12]马红超,王振旅,朱万春,等.异丁烷脱氢催化剂V-O-Al水热-流体干燥法合成[J].高等学校化学学报, 2003, 24(6):1103-1105.MA Hongchao, WANG Zhenglü, ZHU Wanchun, et al. Hydrothermalfluid drying aynthesis of V-O-Al catalyst for isobutane dehydrogenation[J]. Chemical Journal of Chinese Universities, 2003, 24(6):1103-1105.
[13] MURGIA V, TORRES E M F, GOTTIFREDI J C, et al. Sol-gel synthesis of V2O5-SiO2catalyst in the oxidative dehydrogenation of nbutane[J]. Applied Catalysis A:General, 2006, 312(1):134-143.
[14] QIAO K, PENG P, HU C, et al. Synthesis of vanadium-based catalysts and their excellent catalytic behaviors on dehydrogenation of C4hydrocarbons[J]. Applied Petrochemical Research, 2015, 5(4):321-327.
[15] SOKOLOV S, STOYANOVA M, RODEMERCK U, et al. Comparative study of propane dehydrogenation over V-, Cr-, and Pt-based catalysts:time on-stream behavior and origins of deactivation[J].Journal of Catalysis, 2012, 293(9):67-75.
[16] WACHS I E, WECKHUYSEN B M. Structure and reactivity of surface vanadium oxide species on oxide supports[J]. Applied Catalysis A:General, 1997, 157(1/2):67-90.
[17] TIAN Y P, BAI P, LIU S M, et al. VOx-K2O/γ-Al2O3catalyst for nonoxidative dehydrogenation of isobutane[J]. Fuel Processing Technology, 2016, 151:31-39.
[18]马红超,刘子玉,王振旅,等.镧对V2O5/γ-Al2O3催化剂在异丁烷脱氢中活性的影响[J].高等学校化学学报, 2002, 23(5):857-860.MA Hongchao, LIU Ziyu, WANG Zhenlü, et al. Effect of La on the activity of V2O5/γ-Al2O3catalyst in dehydrogenation of isobutane[J].Chemical Journal of Chinese Universities, 2002, 23(5):857-860.
[19] WU T F, LIU G, ZENG L, et al. Structure and catalytic consequence of Mg-modified VOx/Al2O3catalysts for propane dehydrogenation[J].AIChE Journal, 2017, 63(11):4911-4919.
[20] HARLIN M E, NIEMI V M, KRAUSE A O I, et al. Effect of Mg and Zr modificationontheactivityofVOx/Al2O3catalystsinthedehydrogenation of butanes[J]. Journal of Catalysis, 2001, 203(1):242-252.
[21] GUERREROP REZ M O, KIM T, BA ARES M A, et al. Nature of catalytic active sites for Sb-V-O mixed metal oxides[J]. Journal of Physical Chemistry C, 2008, 112(43):16858-16863.
[22]庞玉锋.混合C4烷烃脱氢制混合C4烯烃[D].北京:中国石油大学,2011.PANG Yufeng. Dehydrogenation of mixed C4alkanes to mixed C4olefins[D]. Beijing:China University of Petroleum, 2011.
[23]马红超.异丁烷脱氢制异丁烯钒基催化剂的研究[D].长春:吉林大学, 2003.MA Hongchao. Study on vanadium-based catalyst for dehydrogenation of isobutylene to isobutylene[D]. Changchun:Jilin University, 2003.
[24] BAO K V, SONG M B, AHN I Y, et al. Propane dehydrogenation over Pt-Sn/rare-earth-doped Al2O3:influence of La, Ce or Y on the formation and stability of Pt-Sn alloys[J]. Catalysis Today, 2011, 164(1):214-220.
[25] LEE M H, NAGARAJA B M, LEE K Y, et al. Dehydrogenation of alkane to light olefin over PtSn/θ-Al2O3catalyst:effects of Sn loading[J]. Catalysis Today, 2014, 232(4):53-62.
[26] NAGARAJA B M, SHIN C H, JUNG K D. Selective and stable bimetallic PtSn/θ-Al2O3catalyst for dehydrogenation of n-butane to nbutenes[J]. Applied Catalysis A:General, 2013, 467:211-223.
[27] ZHANG Y, ZHOU Y, SHI J, et al. Comparative study of bimetallic PtSncatalystssupportedondifferentsupportsforpropanedehydrogenation[J].JournalofMolecularCatalysisA:Chemical,2014,381(1):138-147.
[28] FU Y, MA H, WANG Z L, et al. Characterization and reactivity of SnO2-doped V2O5/γ-Al2O3catalysts in dehydrogenation of isobutane to isobutene[J]. Journal of Molecular Catalysis A:Chemical, 2004, 221(1):163-168.
[29]陈桂芳,李静,杨向光. V2O5/Al2O3上异丁烷脱氢反应研究[J].工业催化, 2007, 15(9):30-32.CHEN Guifang, LI Jing, YANG Xiangguang. Study on dehydrogenation of isobutane over V2O5/Al2O3catalyst[J]. Industrial Catalysis, 2007, 15(9):30-32.
[30] SONKER R K, SHARMA A, TOMAR M, et al. Low temperature operated NO2gas sensor based on SnO2-ZnO nanocomposite thin film[J]. Journal of Computational&Theoretical Nanoscience, 2014, 20(5).DOI:10.1166/asl.2014.5461.
[31] NARAYANAN S, SULTANA A, LE Q T, et al. A comparative and multitechnical approach to the acid character of templated and nontemplated ZSM-5 zeolites[J]. Applied Catalysis A:General, 1998, 168(168):373-384.
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