碱处理ZSM-5分子筛催化噻吩烷基化反应性能及其反应动力学
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摘要
分别采用Na2CO3和TPA+/CO_3~(2-)混合碱处理ZSM-5分子筛,用XRD、SEM、BET和Py-IR等手段对碱处理前后的ZSM-5分子筛催化剂进行表征,并考察其催化噻吩烷基化反应性能。结果表明,TPA+/CO_3~(2-)混合碱处理后的ZSM-5分子筛(HZ(CO_3~(2-)-TPA+))比表面积和孔径最大、B酸量最多且最适合催化噻吩烷基化反应。在反应温度120℃、反应压力1.0 MPa、反应空速1.0h-1、反应时间6.0h,HZ(CO_3~(2-)-TPA+)分子筛催化噻吩烷基化转化率最高,为99.1%。在最佳工艺条件下研究了碱处理前后ZSM-5分子筛催化噻吩烷基化反应动力学。结果表明,碱处理前后ZSM-5分子筛催化噻吩烷基化反应动力学均符合一级反应速率方程,HZ、HZ(CO_3~(2-))、HZ(CO_3~(2-)-TPA+)分子筛上噻吩类硫化物烷基化反应的活化能分别为57.15kJ/mol、49.14kJ/mol、43.71kJ/mol,反应指前因子分别为1.660×107 h-1、4.335×106 h-1、1.365×106 h-1。
ZSM-5 zeolites were treated by Na_2CO_3 solution and TPA+/CO_3~(2-)mixed alkali respectively.The ZSM-5 zeolites before and after alkali treatment were characterized by a complementary combination of X-ray diffraction,SEM,BET and Py-IR,The performance of the thiophene alkylation over zeolite was investigated.The results showed that after the TPAOH/Na_2CO_3 mixed alkali treatment,the specific surface area and aperture are the biggest among observed cases,and the content of Br9 nsted acidity are also the biggest.The catalyst is most suitable for thiophene alkylation.With the reaction temperature of 120℃,reaction pressure of 1.0MPa,reaction velocity of 1.0h-1,and reaction time of 6.0h,the conversion rate of thiophene alkylation was up to99.1%.The kinetic of thiophene alkylation over ZSM-5zeolite with mixed alkali treatment was studied under the optimum conditions.The results showed that with the reaction temperature of120℃,reaction pressure of 1.0 MPa,and reaction velocity of 1.0h-1,the conversion rate of thiophene alkylation was up to 99.1%.The thiophene alkylation is found to be a first order reaction.The value of the activation energy of the reaction over HZ、HZ(CO_3~(2-))、HZ(CO_3~(2-)-TPA+)is about57.15kJ/mol、49.14kJ/mol、43.71kJ/mol,and the reaction constant is 1.660×107 h-1、4.335×106 h-1、1.365×106 h-1.
ZSM-5 zeolites were treated by Na_2CO_3 solution and TPA+/CO_3~(2-)mixed alkali respectively.The ZSM-5 zeolites before and after alkali treatment were characterized by a complementary combination of X-ray diffraction,SEM,BET and Py-IR,The performance of the thiophene alkylation over zeolite was investigated.The results showed that after the TPAOH/Na_2CO_3 mixed alkali treatment,the specific surface area and aperture are the biggest among observed cases,and the content of Br9 nsted acidity are also the biggest.The catalyst is most suitable for thiophene alkylation.With the reaction temperature of 120℃,reaction pressure of 1.0MPa,reaction velocity of 1.0h-1,and reaction time of 6.0h,the conversion rate of thiophene alkylation was up to99.1%.The kinetic of thiophene alkylation over ZSM-5zeolite with mixed alkali treatment was studied under the optimum conditions.The results showed that with the reaction temperature of120℃,reaction pressure of 1.0 MPa,and reaction velocity of 1.0h-1,the conversion rate of thiophene alkylation was up to 99.1%.The thiophene alkylation is found to be a first order reaction.The value of the activation energy of the reaction over HZ、HZ(CO_3~(2-))、HZ(CO_3~(2-)-TPA+)is about57.15kJ/mol、49.14kJ/mol、43.71kJ/mol,and the reaction constant is 1.660×107 h-1、4.335×106 h-1、1.365×106 h-1.
引文
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[2]温广明,王丹,赵野,等.催化裂化汽油加氢脱硫技术进展[J].工业催化,2008,16(12):1-5.(WEN Guangming,WANG Dan,ZHAO Ye,et al.Advances in hydrogenation desulfurization technology in catalytic cracking gasoline[J].Ind Catal,2008,16(12):1-5.)
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[5]SHI Ronghui,LI Yonghong,WANG Rong.et al.Alkylation of thiophenic compounds with olefins and its kinetics over MCM-41supported phosphoric acid in FCC Gasoline[J].Catal Lett,2010,139(3/4):114-122.
[6]徐亚荣,沈本贤,徐新良,等.FCC汽油噻吩类硫化物烷基化硫转移反应机理的量子化学[J].石油学报(石油加工),2011,27(5):806-811.(XU Yarong,SHEN Benxian,XU Xinliang,et al.The quantum chemistry of reaction mechanism on the thiophene sulfide alkylation in FCC gasoline[J].Acta Petrolei Sinica(Petroleum Processing Section),2011,27(5):806-811.)
[7]刘盛林,郭晓野,张泽凯,等.MCM-22分子筛介孔对汽油烷基脱硫影响[J].石油学报(石油加工),2008,24(Z):88-91.(LIU Shenglin,GUO Xiaoye,ZHANG Zekai,et al.Effect of mesoporous MCM-22 molecular sieve on gasoline alkylation desulfurization[J].Acta Petrolei Sinica(Petroleum Processing Section),2008,24(Z):88-91.)
[8]张丽萍,李永红,赵玉芝.制备条件对FCC汽油烷基化脱硫固体磷酸催化剂性能的影响[J].工业催化,2007,15(9):10-15.(ZHANG Liping,LI Yonghong,ZHAO Yuzhi.Effect of preparation conditions on the performance of FCC gasoline alkylation desulfurization over solid phosphoric acid catalyst[J].Ind Catal,2007,15(9):10-15.)
[9]赵玉芝,李永红,李兰芳.USY分子筛催化FCC汽油的烷基化脱硫反应研究[J].分子催化,2008,22(1):17-21.(ZHAO Yuzhi,LI Yonghong,LI Lanfang.Study on alkylation desulfurization of FCC gasoline over USY molecular sieve catalyst[J].J Mol Catal,2008,22(1):17-21.)
[10]罗国华,徐新,佟泽民.分子筛催化噻吩类硫化物与烯烃烷基化脱硫研究[J].化学反应工程与工艺,2005,21(2):132-137.(LUO Guohua,XU Xin,TONG Zemin.Study on alkylation desulfurization of thiophene and olefin by molecular sieve catalyst[J].Chem React Eng Tec,2005,21(2):133-137.)
[11]TAGO T,KONNO H,SAKAMOTO M,et al.Selective synthesis for light olefins from acetone over ZSM-5zeolites with nano-and macro-crystal sizes[J].Appl Catal A:Gen,2011,403(1/2):183-191.
[12]FIROOZI M,BAGHALHA M,ASAD M.The effect of micro and nano particle sizes of HZSM-5 on the selectivity of MTP reaction[J].Catal Commun,2009,10(12):1582-1585.
[13]GROEN J C,PEFFER L A A,MOULIJIN J A,et al.Mesoporosity development in ZSM-5 zeolite upon optimized desilication conditions in alkaline[J].Colloids Surf A:Physicochem Eng,2004,214(1-3):53-58.
[14]赵岑,刘冬梅,魏民,等.多级孔ZSM-5分子筛的制备及催化噻吩烷基化性能研究[J].燃料化学学报,2013,41(10):1256-1261.(ZHAO Cen,LIU Dongmei,WEI Min,et al.Preparation and catalytic performance of ZSM-5molecular sieve with hierarchical pore[J].Fuel Chem Technol,2013,41(10):1256-1261.)
[15]PEREZ-RAMIREZ J,VERBOELEND D,BONILLA A.Zeolite catalysts with tunable hierarchy factor by poregrowth moderators[J].Adv Funct Mater,2009,19(24):3972-3979.
[16]李莎,李玉平,狄春雨,等.TPAOH/NaOH混合碱体系对ZSM-5沸石的改性及其催化性能研究[J].燃料化学学报,2012,40(5):583-587.(LI Sha,LI Yuping,DI Chunyu,et al.Study on the modification of ZSM-5by the treatment of TPAOH/NaOH mixed alkali system and its catalytic performance[J].Fuel Chem Technol,2012,40(5):583-588.)
[17]刘冬梅,翟玉春,马健,等.碱改性ZSM-5分子筛及脱硫性能的研究[J].中国稀土学报,2015,33(1):39-47.(LIU Dongmei,ZHAI Yuchun,MA Jian,et al.Study on the performance of alkali modified ZSM-5 molecular sieve and its desulfurization[J].Chin Rare Earths J,2015,33(1):39-47.)
[18]金文清,赵国良,滕加伟,等.氢氧化钠改性ZSM-5分子筛的碳四烯烃催化裂解性能[J].化学反应工程与工艺,2007,23(3):193-199.(JIN Wenqing,ZHAO Guoliang,TENG Jiawei,et al.Catalytic cracking performance over HZSM-5zeolite modified by sodium hydroxide modification[J].Chem React Eng Tec,2007,23(3):193-199.)
[19]MELIN-CABRERA I,ESPINOSA S,MENTRUIT C,et al.Alkaline leaching for synthesis of improved FeZSM-5catalysts[J].Catal Commun,2006,7(2):100-103.
[20]ABELLO S,BONILLA A.Mesoporous ZSM-5zeolite catalysts prepared by desilication with organic hydroxides and comparison with NaOH leaching[J].Appl Catal A,2009,364(1/2):191-198.
[21]GROEN J C,MOULIJN J A,PEREZ R J.Decoupling mesopomsity formation and acidity modification in ZSM-5zeolites by sequential desilication-dealumination[J].Microporous Mesoporous Mater,2005,87(2):153-161.
[22]石岗,林秀英,范煜,等.ZSM-5分子筛的脱硅改性及加氢改质性能[J].燃料化学学报,2013,41(5):589-600.(SHI Gang,LIN Xiuying,FAN Yu,et al.Modification of silicon over ZSM-5 molecular sieve and its modification of hydrogen[J].Fuel Chem Technol,2013,41(5):589-600.)
[23]潘兴朋,吴相英,杜君,等.碱处理Beta分子筛吸附脱硫动力学[J].化工学报,2016,67(9):3748-3754.(PAN Xingpeng,WU Xiangying,DU Jun,et al.Kinetics of adsorption desulfurization of Beta molecular sieve by alkali treatment[J].Chem Eng J,2016,67(9):3748-3754.)
[24]黄先亮.二次晶化法修饰改性TS-1及催化环己酮氨氧化反应的研究[D].湖南:湘潭大学,2008.
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