分散型纳米二硫化钼的制备及其对模拟油浆的加氢处理催化性能
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摘要
以二烷基二硫代氨基甲酸钼(Mo-DTC)和六羰基钼(Mo(CO)_6)为前驱体、水热法合成了分散型纳米MoS_2,采用Xray射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱分析(XPS)和程序升温脱附法(NH_3-TPD)等方法对其进行了表征。利用三种烯烃(辛烯、苯乙烯、反式二苯乙烯)、苯并噻吩和蒽等构建模拟油浆体系,结合气相色谱-质谱(GC-MS)分析,对分散型纳米MoS_2的模拟油浆加氢处理催化性能进行了研究。结果表明,不同预处理条件下制备出的催化活性样品均为2H-MoS_2,但各样品的结晶度、颗粒尺寸、硫化程度及其酸性质等均有所不同,其中,总酸量差别较小;以Mo-DTC和Mo(CO)_6为前驱体的优选硫化条件分别为380℃/30 min和370℃/30 min,所得到的催化剂对烯烃和噻吩的加氢活性较高。其中,Mo-DTC基纳米MoS_2催化剂的烯烃加氢饱和转化率高达98.10%,加氢脱硫率为94.51%,而蒽的部分加氢饱和转化率则较低,为29.47%,且无八氢蒽(8HN)或全氢蒽的生成。Mo(CO)_6基纳米MoS_2催化剂的加氢效果则略差,烯烃加氢饱和转化率为94.01%,加氢脱硫率为89.01%,对蒽的加氢饱和转化率为24.20%,无8HN或全氢蒽的生成。总体而言,由Mo-DTC所制备的MoS_2催化剂具有烯烃高效饱和、含硫化合物高效脱硫、芳烃浅度加氢饱和的效果,且油浆加氢处理反应的选择性及催化稳定性均更高。
A series of dispersed nano molybdenum disulfide( MoS_2) catalysts were prepared with molybdenum dialkyl dithiocarbamate( Mo-DTC) and molybdenum hexacarbonyl( Mo(CO)_6) as the precursors by hydrothermal methods and characterized by X-ray diffraction( XRD), transmission electron microscopy( TEM),X-ray photoelectron spectroscopy( XPS) and temperature programmed desorption( NH_3-TPD). By using a simulated oil slurry containing three kinds of olefins( octane,styrene and trans-dibenzylethene),benzothiophene and anthracene,the catalytic performance of nano MoS_2 in the hydrogenation was investigated,with the help of gas chromatography-mass spectrometry( GC-MS). The results indicate that all the prepared catalysts are in the form of 2H-MoS_2; however,their crystallinity,particle size,vulcanization degree,and acid property are influenced by the pretreatment conditions; the preferred vulcanization conditions for the M o-DTCand Mo(CO)_6-based MoS_2 catalysts are 380 ℃/30 min and 370 ℃/30 min,respectively,to achieve a relatively high activity in the hydrogenation of olefins and benzothiophene. Over the M o-DTC-based nano-MoS_2 catalyst,the saturation conversion of olefins hydrogenation is 98. 10% and the hydrodesulfurization rate is 94. 51%,whereas the saturation conversion of anthracene hydrogenation is 29.47%,without forming octahydroanthracene( 8HN) or perhydroanthracene. In contrast,the activity of Mo(CO)_6-based nano-MoS_2 catalyst is slightly lower,with the saturation conversion of olefins hydrogenation being 94.01% and the hydrodesulfurization rate being 89.01%; similarly, the saturation conversion for anthracene hydrogenation is 24. 20%, without 8HN or perhydroanthracene in the product. As a whole,in comparison with the Mo(CO)_6-based MoS_2 catalyst,the nano MoS_2 catalyst derived from M o-DTC displays higher efficiency in both olefins saturation and sulfur-containing compounds desulfurization,and lowdegree hydrogenation of aromatic hydrocarbons; moreover,it also exhibits higher hydro-treating selectivity for the catalytic cracking slurry and higher stability during hydrogenation.
A series of dispersed nano molybdenum disulfide( MoS_2) catalysts were prepared with molybdenum dialkyl dithiocarbamate( Mo-DTC) and molybdenum hexacarbonyl( Mo(CO)_6) as the precursors by hydrothermal methods and characterized by X-ray diffraction( XRD), transmission electron microscopy( TEM),X-ray photoelectron spectroscopy( XPS) and temperature programmed desorption( NH_3-TPD). By using a simulated oil slurry containing three kinds of olefins( octane,styrene and trans-dibenzylethene),benzothiophene and anthracene,the catalytic performance of nano MoS_2 in the hydrogenation was investigated,with the help of gas chromatography-mass spectrometry( GC-MS). The results indicate that all the prepared catalysts are in the form of 2H-MoS_2; however,their crystallinity,particle size,vulcanization degree,and acid property are influenced by the pretreatment conditions; the preferred vulcanization conditions for the M o-DTCand Mo(CO)_6-based MoS_2 catalysts are 380 ℃/30 min and 370 ℃/30 min,respectively,to achieve a relatively high activity in the hydrogenation of olefins and benzothiophene. Over the M o-DTC-based nano-MoS_2 catalyst,the saturation conversion of olefins hydrogenation is 98. 10% and the hydrodesulfurization rate is 94. 51%,whereas the saturation conversion of anthracene hydrogenation is 29.47%,without forming octahydroanthracene( 8HN) or perhydroanthracene. In contrast,the activity of Mo(CO)_6-based nano-MoS_2 catalyst is slightly lower,with the saturation conversion of olefins hydrogenation being 94.01% and the hydrodesulfurization rate being 89.01%; similarly, the saturation conversion for anthracene hydrogenation is 24. 20%, without 8HN or perhydroanthracene in the product. As a whole,in comparison with the Mo(CO)_6-based MoS_2 catalyst,the nano MoS_2 catalyst derived from M o-DTC displays higher efficiency in both olefins saturation and sulfur-containing compounds desulfurization,and lowdegree hydrogenation of aromatic hydrocarbons; moreover,it also exhibits higher hydro-treating selectivity for the catalytic cracking slurry and higher stability during hydrogenation.
引文
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[17]LI J H,WAN D E,MA H J.Ionic liquid assisted hydrothermal synthesis of MoS2double-shell polyhedral cages w ith enhanced catalytic hydrogenation activities[J].RSC Adv,2017,7(38):23523-23529.
[18]LI M,WANG D E,LI J H.Facile hydrothermal synthesis of MoS2nano-sheets with controllable structures and enhanced catalytic performance for anthracene hydrogenation[J].RSC Adv,2016,6(75):71534-71542.
[19]任萍,兰新哲,周军,宋永辉,张秋利.水热法制备二硫化钼微球花及其结构表征[J].有色金属(冶炼部分),2011,(10):47-49.(REN Ping,LAN Xin-zhe,ZHOU Jun,SONG Yong-hui,ZHANG Qiu-li.Hydrothermal synthesis and characterization of MoS2flow er-sphere[J].Nonferrous Met Extr Metall,2011,(10):47-49.)
[20]黄继武.多晶材料X射线衍射-实验原理、方法与应用[M].北京:冶金工业出版社,2006:119-132.(HUANG Ji-wu.X-ray Diffraction of Polycrystalline Materials-Experimental Principle,Method and Application[M].Beijing:Metallurgical Industry Press,2006:119-132.)
[21]YANG Y Q,TYE C T,SMITH K J.Influence of MoS2catalyst morphology on the hydride-oxygenation of phenols[J].Catal Commun,2008,9(6):1364-1368.
[22]吴壮志.纳米结构二硫化钼(钨)的制备及其性能研究[D].长沙:中南大学,2012.(WU Zhuang-zhi.Preparation and properties of nanostructured molybdenum disulfide(tungsten)[M].Changsha:Central South University,2012.)
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[26]LIU K K,ZHANG W,LEE Y H,LIN Y C,CHANG M T,SU C Y,CHANG C S,LI H,SHI Y M.Growth of large-area and highly crystalline M oS2thin layers on insulating substrates[J].Nano Lett,2012,12(3):1538-1544.
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[2]郭爱军,郑文林,焦守辉,陈坤,刘贺,王宗贤,王子豪.催化裂化油浆中烯烃分布研究[J].燃料化学学报,2018,46(4):413-418.(GUO Ai-jun,ZHENG Wen-lin,JIAO Shou-hui,CHEN Kun,LIU He,WANG Zong-xian,WANG Zi-hao.Study on olefin distribution of catalytic cracking slurry[J].J Fuel Chem Technol,2018,46(4):413-418.)
[3]尚猛,李传,邓文安,田广华,阙国和.渣油悬浮床加氢裂化油溶性催化剂的性能[J].石油学报(石油加工),2011,27(3):361-366.(SHANG Meng,LI Chuan,DENG Wen-an,TIAN Guang-hua,QUE Guo-he.Performance of residual oil hydrocracking oil-soluble catalyst[J].Acta Pet Sin(Pet Process Sect),2011,27(3):361-366.)
[4]倪术荣,徐伟池,姜维,张全国,郭金涛.非负载型加氢脱硫催化剂研究进展[C]//全国工业催化技术及应用年会.2016.(NI Shu-rong,XU Wei-chi,JIANG Wei,ZHANG Quan-guo,GUO Jin-tao.Research progress on unsupported hydrodesulfurization catalysts[C]//National Industrial Catalysis Technology and Application Annual Meeting.2016.)
[5]PANARITI N,BIANCO A D,PIERO G D,MARCHIONNA M,CARNITI P.Petroleum residue upgrading with dispersed catalysts:Part 2.Effect of operating conditions[J].Appl Catal A:Gen,2000,204(2):215-222.
[6]刘晨光,阙国和.孤岛渣油在分散型催化剂存在下加氢裂化反应的研究[J].石油炼制与化工,1993,24(3):57-62.(LIU Chen-guang,QUE Guo-he.Study on hydrocracking reaction of Gudao residue in the presence of dispersed catalyst[J].Pet Process Petrochem,1993,24(3):57-62.)
[7]CLOSE M R,PETERSEN J L,KUGLER E L.Synthesis and characterization of nanoscale molybdenum sulfide catalysts by controlled gas phase decomposition of M o(CO)6and H2S[J].Inorg Chem,1999,38(7):1535-1542.
[8]王亚男,李广学,刘银.二硫化钼催化剂的制备与应用[J].广东化工,2009,36(3):37-41.(WANG Ya-nan,LI Guang-xue,LIU Yin.Preparation and application of molybdenum disulfide catalyst[J].Guangdong Chem Ind,2009,36(3):37-41.)
[9]ROMERO-RIVERA R,VALLE M D,ALONSO G,FLORES E,CASTILLON F,FUENTES S,CRUZ-REYES J.Cyclohexene hydrogenation w ith molybdenum disulfide catalysts prepared by ex situ,decomposition of ammonium thiomolybdate-cetyltrimethylammonium thiomolybdate mixtures[J].Catal Today,2008,130(2):354-360.
[10]BACKES C,BENERN C,CHEN X,LAFARGUE P,LAPIACE P,FREELEY M,DUESBERG G S,COLEMA J N,MCDONALD A R.Functionalization of liquid-exfoliated tw o-dimensional 2H-M oS2[J].Angew Chem Int Ed,2015,54(9):2638-2642.
[11]TANG G,WANG Y,CHEN W,TANG H,LI C.Hydrothermal synthesis and characterization of novel flowerlike MoS2hollow microspheres[J].Mater Lett,2013,100:15-18.
[12]XIE J,ZHANG J,LI S,GROTE F,ZHANG X,ZHANG H,WANG R,LEI Y,PAN B,XIE Y.Controllable disorder engineering in oxygen-incorporated M oS2ultrathin nanosheets for efficient hydrogen evolution[J].J Am Chem Soc,2014,136(4):17881-17888.
[13]PENG Y,MENG Z,ZHONG C,LU J,YU W,YANG Z,QIAN Y.Hydrothermal synthesis of MoS2and its pressure-related crystallization[J].J Solid State Chem,2001,159(1):170-173.
[14]WATANABE I,OTAKE M,YOSHIMOTO M,SAKANISHI K,KORAIY,MOCHIDA I.Behaviors of oil-soluble molybdenum complexes to form very fine M oS2particles in vacuum residue[J].Fuel,2002,81(11):1515-1520.
[15]张倩倩,邓文安,李传,沐宝泉.不同有机钼催化剂在重油加氢反应中的差异及其原因初探[J].石油炼制与化工,2015,46(5):61-65.(ZHANG Qian-qian,DENG Wen-an,LI Chuan,MU Bao-quan.Preliminary study on the differences and causes of different organic molybdenum catalysts in heavy oil hydrogenation[J].Pet Process Petrochem,2015,46(5):61-65.)
[16]SAKANISHI K,WATANABE I,MOCHIDA I.Characterization of soluble Mo complex catalyst during hydro-treatment of vacuum residues[J].ACS Symp,2005:197-203.
[17]LI J H,WAN D E,MA H J.Ionic liquid assisted hydrothermal synthesis of MoS2double-shell polyhedral cages w ith enhanced catalytic hydrogenation activities[J].RSC Adv,2017,7(38):23523-23529.
[18]LI M,WANG D E,LI J H.Facile hydrothermal synthesis of MoS2nano-sheets with controllable structures and enhanced catalytic performance for anthracene hydrogenation[J].RSC Adv,2016,6(75):71534-71542.
[19]任萍,兰新哲,周军,宋永辉,张秋利.水热法制备二硫化钼微球花及其结构表征[J].有色金属(冶炼部分),2011,(10):47-49.(REN Ping,LAN Xin-zhe,ZHOU Jun,SONG Yong-hui,ZHANG Qiu-li.Hydrothermal synthesis and characterization of MoS2flow er-sphere[J].Nonferrous Met Extr Metall,2011,(10):47-49.)
[20]黄继武.多晶材料X射线衍射-实验原理、方法与应用[M].北京:冶金工业出版社,2006:119-132.(HUANG Ji-wu.X-ray Diffraction of Polycrystalline Materials-Experimental Principle,Method and Application[M].Beijing:Metallurgical Industry Press,2006:119-132.)
[21]YANG Y Q,TYE C T,SMITH K J.Influence of MoS2catalyst morphology on the hydride-oxygenation of phenols[J].Catal Commun,2008,9(6):1364-1368.
[22]吴壮志.纳米结构二硫化钼(钨)的制备及其性能研究[D].长沙:中南大学,2012.(WU Zhuang-zhi.Preparation and properties of nanostructured molybdenum disulfide(tungsten)[M].Changsha:Central South University,2012.)
[23]DREW M G B,MITCHELL P C H,KASZTELAN S.Computer modelling of a molybdenum disulfide catalyst[J].Polyhedron,1990,8(86):697-702.
[24]李敏,刘忠杉,王冬娥,潘振栋,马怀军,姜玉霞,田志坚.纳米二硫化钼的制备及其蒽加氢性能[J].石油学报(石油加工),2018,34(2):253-260.(LI Min,LIU Zhong-shan,WANG Dong-e,PAN Zhen-dong,MA Huai-jun,JIANG Yu-xia,TIAN Zhi-jian.Preparation of nanometer molybdenum disulfide and its hydrogenation performance[J].Acta Pet Sin(Pet Process Sect),2018,34(2):253-260.)
[25]HAO L,XIONG G,LIU L P,LONG H Y,JIN F Y,WANG X S.Preparation of highly dispersed desulfurization catalysts and their catalytic performance in hydrodesulfurization of dibenzothiophene[J].Chin J Catal,2016,37(3):412-419.
[26]LIU K K,ZHANG W,LEE Y H,LIN Y C,CHANG M T,SU C Y,CHANG C S,LI H,SHI Y M.Growth of large-area and highly crystalline M oS2thin layers on insulating substrates[J].Nano Lett,2012,12(3):1538-1544.
[27]WANG H W,SKELDON P,THOMPSON G E.XPS studies of MoS2formation from ammonium tetrathiomolybdate solutions[J].Surf Coat Technol,1997,91(3):200-207.
[28]RAO C N R,NAG A.Inorganic analogues of graphene[J].Eur J Inorg Chem,2010,(27):4244-4250.
[29]BAKER M A,GILMORE R,LENARDI C,GISSLER W.XPS investigation of preferential sputtering of S from MoS2and determination of M oSxstoichiometry from M o and S peak positions[J].Appl Surf Sci,1999,150(14):255-262.
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