基于镁铝水滑石的Mo/Al2O3-MgO催化剂制备及其加氢脱硫性能

doi:10.11949/j.issn.0438-1157.20170727

化工学报 ›› 2018, Vol. 69 ›› Issue (1): 405-413.DOI: 10.11949/j.issn.0438-1157.20170727

• 催化、动力学与反应器 • 上一篇下一篇

基于镁铝水滑石的Mo/Al₂O₃-MgO催化剂制备及其加氢脱硫性能

岳源源¹, 郑晓桂¹, 康颖¹, 白正帅¹, 袁珮¹, 朱海波¹, 鲍晓军^1,2

1 福州大学石油化工学院, 化肥催化剂国家工程研究中心, 福建福州 350002;
2 福州大学能源与环境光催化国家重点实验室, 福建福州 350116

收稿日期:2017-06-05 修回日期:2017-08-02 出版日期:2018-01-05 发布日期:2018-01-05
通讯作者: 鲍晓军
基金资助:
国家自然科学基金联合基金项目（U1462203）；国家自然科学基金青年基金项目（21506034）。

Mo/Al₂O₃-MgO catalyst preparation from MgAl-hydrotalcite and their hydrogenation desulfurization performance

YUE Yuanyuan¹, ZHENG Xiaogui¹, KANG Ying¹, BAI Zhengshuai¹, YUAN Pei¹, ZHU Haibo¹, BAO Xiaojun^1,2

1 National Engineering Research Center of Chemical Fertilizer Catalyst, School of Chemical Engineering, Fuzhou University, Fuzhou 350002, Fujian, China;
2 State Key Laboratory of Photocatalysis on Energy & Environment, Fuzhou University, Fuzhou 350116, Fujian, China

Received:2017-06-05 Revised:2017-08-02 Online:2018-01-05 Published:2018-01-05
Contact: 10.11949/j.issn.0438-1157.20170727
Supported by:
supported by the Joint Funds of the National Natural Science Foundation of China(U1462203) and the Young Scientists Fund of the National Natural Science Foundation of China (21506034).

摘要/Abstract

摘要：

生产低硫或无硫柴油是当今世界范围内清洁燃料发展的趋势，加氢脱硫（HDS）是大规模生产清洁柴油最为有效的技术之一，而研制高活性的HDS催化剂成为该技术的关键。以镁铝水滑石与氧化铝的复合氧化物为载体，通过等体积浸渍法制备了一系列Mo/Al₂O₃-MgO催化剂，以二苯并噻吩（DBT）的正庚烷溶液为原料，在固定床反应器上评价所得催化剂的HDS活性，考察了不同镁铝比的水滑石、焙烧温度和添加量对催化剂物化性质和催化性能的影响。研究结果表明，镁铝比、焙烧温度和添加量均影响催化剂的酸性、金属还原性、硫化性能和MoS₂片晶的堆垛度等，当镁铝摩尔比为3、焙烧温度为800℃、成型时水滑石加入量为10%（质量分数）时，所制备催化剂的HDS活性最高，其脱硫率可达96.2%。这是由于该催化剂的酸性较适宜，活性组分与载体间的相互作用力适中，活性组分更易硫化，有助于提高MoS₂片晶的堆垛度进而改善催化剂的HDS性能。

关键词: 镁铝水滑石, Mo/Al₂O₃-MgO, 催化剂, 加氢脱硫, 活性

Abstract:

Diesel production with low/no sulfur content is a major trend in world-wide development of clean fuels. Among many alternative technologies, hydrogenation desulfurization (HDS) is most effective to produce clean diesel at industrial scale, which development of highly active catalysts is the key. In this study, a series of Mo/Al₂O₃-MgO catalysts were prepared by metal oxide composites of MgAl-hydrotalcite and alumina as carriers with incipient-wetness impregnation method. Their catalytic performance was evaluated on dibenzothiophene (DBT) solution in n-heptane as raw material in a fixed-bed reactor. The results showed that Mg/Al molar ratio, calcination temperature, and additive amount all affected acidity, reduction and sulfidation of the catalysts and stacking degree of MoS₂ crystallites. When Mg/Al molar ratio was 3, calcination temperature was 800℃, and hydrotalcite was 10% (mass), the obtained catalyst has the highest HDS activity with up to 96.2% desulfurization rate. Appropriate catalyst acidity and suitable interaction between active component and carrier make it easier to sulfide the active component, which is beneficial to improve stacking degree of MoS₂ crystallites and enhance catalytic performance.

Key words: MgAl-hydrotalcite, Mo/Al₂O₃-MgO, catalyst, hydrogenation desulfurization, reactivity

中图分类号:

TE624

岳源源, 郑晓桂, 康颖, 白正帅, 袁珮, 朱海波, 鲍晓军. 基于镁铝水滑石的Mo/Al₂O₃-MgO催化剂制备及其加氢脱硫性能[J]. 化工学报, 2018, 69(1): 405-413.

YUE Yuanyuan, ZHENG Xiaogui, KANG Ying, BAI Zhengshuai, YUAN Pei, ZHU Haibo, BAO Xiaojun. Mo/Al₂O₃-MgO catalyst preparation from MgAl-hydrotalcite and their hydrogenation desulfurization performance[J]. CIESC Journal, 2018, 69(1): 405-413.

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[34]	USMAN, YAMAMOTO T, KUBOTA T, et al. Effect of phosphorus addition on the active sites of a Co-Mo/Al2O3 catalyst for the hydrodesulfurization of thiophene[J]. Applied Catalysis A:General, 2007, 328(2):219-25.
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[2]	刘志红, 王豪, 鲍晓军. 提高柴油加氢精制催化剂活性的方法[J]. 化工进展, 2008, 27(2):173-179. LIU Z H, WANG H, BAO X J. Methods for improving the activity of diesel hydrotreatring catalysts[J]. Chemical Industry and Engineering Progress, 2008, 27(2):173-179.
[3]	TAGUCHI A, SCHÜTH F. Ordered mesoporous materials in catalysis[J]. Microporous & Mesoporous Materials, 2005, 77(1):1-45.
[4]	BREYSSE M. Overview of support effects in hydrotreating catalysts[J]. Catalysis Today, 2004, 86(z1):5-16.
[5]	KLICPERA T, ZDRA?IL M. Preparation of high-activity MgO-supported Co-Mo and Ni-Mo sulfide hydrodesulfurization catalysts[J]. Journal of Catalysis, 2002, 206(2):314-320.
[6]	KALU?A L, GULKOVÁ D, VÍT Z, et al. High-activity MgO-supported CoMo hydrodesulfurization catalysts prepared by non-aqueous impregnation[J]. Applied Catalysis B:Environmental, 2015, 162:430-436.
[7]	TREJO F, RANA M S, ANCHEYTA J. CoMo/MgO-Al2O3 supported catalysts:An alternative approach to prepare HDS catalysts[J]. Catalysis Today, 2008, 130(2-4):327-336.
[8]	SOLÍSCASADOS D, ESCOBAR J, OROZCO I G, et al. Effect of potassium content on the performance of CoMo/Al2O3-MgO-K2O(x) catalysts in hydrodesulfurization of dibenzothiophene[J]. Industrial & Engineering Chemistry Research, 2010, 50(5):2755-2761.
[9]	WAN D, LIU Y D, XIAO S H, et al. Uptake fluoride from water by caclined Mg-Al-CO3 hydrotalcite:Mg/Al ratio effect on its structure, electrical affinity and adsorptive property[J]. Colloids and Surfaces A:Physicochemical and Engineering Aspects, 2015, 469:307-314.
[10]	ZHAO C Y. Synthesis of novel MgAl layered double oxide grafted TiO2 cuboids and their photocatalytic activity on CO2 reduction with water vapor[J]. Catalysis Science & Technology, 2015, 5(6):3288-3295.
[11]	杨博文, 祝琳华, 司甜, 等. 以催化剂为应用背景的水滑石类插层材料的应用研究进展[J]. 化工科技, 2016, 24(4):72-77. YANG B W, ZHU L H, SI T, et al. Research progress of hydrotalcite-like intercalation materials on the background of catalyst[J]. Science & Technology in Chemical industry, 2016, 24(4):72-77
[12]	ARDHAYANTI L I, SANTOSA S J. Synthesis of magnetite-Mg/Al hydrotalcite and its application as adsorbent for navy blue and yellow F3G dyes[J]. Procedia Engineering, 2016, 148:1380-1387.
[13]	KAI C, GALLUCCI F, PIO G, et al. On the influence of steam on the CO2 chemisorption capacity of a hydrotalcite-based adsorbent for SEWGS applications[J]. Chemical Engineering Journal, 2017, 314:554-569.
[14]	ZHANG L H, ZHU J, JIANG X R, et al. Influence of nature of precursors on the formation and structure of Cu-Ni-Cr mixed oxides from layered double hydroxides[J]. Journal of Physics & Chemistry of Solids, 2006, 67(8):1678-1686.
[15]	LI D L, DING Y Y, WEI X F, et al. Cobalt-aluminum mixed oxides prepared from layered double hydroxides for the total oxidation of benzene[J]. Applied Catalysis A:General, 2015, 507:130-138.
[16]	李大塘, 郭军, 沈俭一, 等. 焙烧温度对Mg(Al)O复合物结构和表面酸碱性质影响的研究[J]. 化学物理学报, 2000, 13(2):220-226. LI D T, GUO J, Shen J Y, et al. Exploration on influence of calcination temperature on structure and surface acidity and basicity of Mg(Al)O composite oxide[J]. Chinese Journal of Chemical Physics, 2000, 13(2):220-226.
[17]	MI J X, LAN Z X, CHEN J J, et al. MgAl-LDO mixed oxide derived from layered double hydroxide:A potential support for CoMo sulfur-resistant water-gas shift catalyst[J]. Catalysis Communications, 2016, 78:44-47.
[18]	张岩, 王继锋, 赵德智, 等. γ-Al2O3载体孔结构及酸性的调变[J]. 石化技术与应用, 2015, 33(4):366-370. ZHANG Y, WANG J F, ZHAO D Z, et al. The modification of pore structure and acidity of γ-Al2O3 support[J]. Petrochemical Technology & Application, 2015, 33(4):366-370.
[19]	HINNEMANN B, MOSES P G, N RSKOV J K. Recent density functional studies of hydrodesulfurization catalysts:Insight into structure and mechanism[J]. Journal of Physics:Condensed Matter, 2008, 20(6):064236.
[20]	QU L L, ZHANG W P, KOOYMAN P J, et al. MAS NMR, TPR, and TEM studies of the interaction of NiMo with alumina and silica-alumina supports[J]. Journal of Catalysis, 2003, 215(1):7-13.
[21]	KUMAR M, ABERUAGBA F, GUPTA J K, et al. Temperature-programmed reduction and acidic properties of molybdenum supports on MgO-Al2O3 and their correlation with catalytic activity[J]. Journal of Molecular Catalysis A Chemical, 2004, 213(2):217-223.
[22]	FAN Y, BAO X J, WANG H, et al. A surfactant-assisted hydrothermal deposition method for preparing highly dispersed W/γ-Al2O3 hydrodenitrogenation catalyst[J]. Journal of Catalysis, 2007, 245(2):477-484.
[23]	HENSEN E J M, DE BEER V H J, VAN VEEN J A R, et al. A refinement on the notion of Type I and Ⅱ (Co)MoS phases in hydrotreating catalysts[J]. Catalysis Letters, 2002, 84(1-2):59-67.
[24]	QIU L M, XU G T. Peak overlaps and corresponding solutions in the X-ray photoelectron spectroscopic study of hydrodesulfurization catalysts[J]. Applied Surface Science, 2010, 256(11):3413-3417.
[25]	LIU B, CHAI Y M, LI Y P, et al. Effect of sulfidation atmosphere on the performance of the CoMo/γ-Al2O3, catalysts in hydrodesulfurization of FCC gasoline[J]. Applied Catalysis A:General, 2014, 471:70-79.
[26]	FAN Y, XIAO H, SHI G, et al. Citric acid-assisted hydrothermal method for preparing NiW/USY-Al2O3, ultradeep hydrodesulfurization catalysts[J]. Journal of Catalysis, 2011, 279(1):27-35.
[27]	HENSEN E J M, KOOYMAN P J, VAN DER MEER Y, et al. The relation between morphology and hydrotreating activity for supported MoS2 particles[J]. Journal of Catalysis, 2001, 199(2):224-235.
[28]	OKAMOTO Y, OCHIAI K, KAWANO M, et al. Evaluation of the maximum potential activity of Co-Mo/Al2O3 catalysts for hydrodesulfurization[J]. Journal of Catalysis, 2004, 222(1):143-151.
[29]	连奕新, 王会芳, 张元华, 等. 焙烧温度对镁铝复合氧化物载体性能的影响[J]. 石油化工, 2009, 38(6):622-629. LIAN Y X, WANG H F, ZHANG Y H, et al. Effect of calcination temperature on performance of Mg-Al composite oxide support[J]. Petrochemical Technology, 2009, 38(6):622-629.
[30]	上官荣昌. 焙烧温度对镁铝水滑石焙烧产物物性影响的研究[J]. 淮阴师范学院学报(自然科学版), 2002, 1(1):67-69. SHANGGUAN R C. Effects of calcine temperature on the thermal stability of calcine product obtained from magnesium-aluminum hydrotalcites[J]. Journal of Huaiyin Teachers College (Natural Science Edition), 2002, 1(1):67-69.
[31]	TOPS E H. The role of Co-Mo-S type structures in hydrotreating catalysts[J]. Applied Catalysis A:General, 2007, 322:3-8.
[32]	HAN W, YUAN P, FAN Y, et al. Preparation of supported hydrodesulfurization catalysts with enhanced performance using Mo-based inorganic-organic hybrid nanocrystals as a superior precursor[J]. Journal of Materials Chemistry, 2012, 22(48):25340-53.
[33]	YUE Y Y, NIU P L, JIANG L L, et al. Acid-modified natural bauxite mineral as a cost-effective and high-efficient catalyst support for slurry-phase hydrocracking of high-temperature coal tar[J]. Energy & Fuels, 2016, 30(11):9203-9.
[34]	USMAN, YAMAMOTO T, KUBOTA T, et al. Effect of phosphorus addition on the active sites of a Co-Mo/Al2O3 catalyst for the hydrodesulfurization of thiophene[J]. Applied Catalysis A:General, 2007, 328(2):219-25.
[35]	VAN VEEN J A R, GERKEMA E, VAN DER KRAAN A M, et al. A 57CO Mössbauer emission spectrometric study of some supported CoMo hydrodesulfurization catalysts[J]. Journal of Catalysis, 1992, 133(1):112-23.

基于镁铝水滑石的Mo/Al₂O₃-MgO催化剂制备及其加氢脱硫性能

Mo/Al₂O₃-MgO catalyst preparation from MgAl-hydrotalcite and their hydrogenation desulfurization performance

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