Register      Login
Australian Journal of Chemistry Australian Journal of Chemistry Society
An international journal for chemical science
RESEARCH ARTICLE

Characterization and Acidic Properties of AlMCM-41 Prepared by Conventional and Post-Synthesis Alumination

Maria J. F. Costa A E , Thiago Chellappa D , Antonio S. Araujo A , Viviane M. Fonseca B , Valter J. Fernandes Jr A , Rubens M. Nascimento D and José G. A. Pacheco C
+ Author Affiliations
- Author Affiliations

A Federal University of Rio Grande do Norte, Institute of Chemistry, 59078-970, Natal RN, Brazil.

B Federal University of Rio Grande do Norte, Department of Textile Engineering, 59060-300, Natal RN, Brazil.

C Federal University of Pernambuco, Department of Chemical Engineering, 50740-521, Recife PE, Brazil.

D Federal University of Rio Grande do Norte, Department of Mechanical Engineering, 59060-300, Natal RN, Brazil.

E Corresponding author. Email: mariadedeia@hotmail.com

Australian Journal of Chemistry 68(1) 99-105 https://doi.org/10.1071/CH13679
Submitted: 13 December 2013  Accepted: 30 March 2014   Published: 23 June 2014

Abstract

The catalysts analysed in the current work are variations of MCM-41. The properties of these highly ordered mesoporous aluminosilicates were adjusted by an isomorphous substitution of Si by a trivalent cation, in this case Al3+, generating catalysts of the AlMCM-41 type. The materials were synthesized with a silicon/aluminium ratio of 40, through two methods of impregnation of the metal: conventional and post-synthesis alumination. With the aim of determining the density of the acid sites of the Al40MCM-41 prepared by post-synthesis and conventional alumination, studies of the adsorption of n-butylamine probe molecule were carried out. Further, the studied material was characterized by thermogravimetry measurements, providing the profile of decomposition of the samples, which allowed calculation of the densities of the acid sites. The model-free kinetic algorithms were applied in order to determinate conversion and apparent activation energy. Comparison of energy-dispersive X-ray fluorescence and X-ray photoelectron spectroscopy measurements indicated that the post-synthesis method was more favourable based on the metal positioning, ‘anchored’ in the surface of the catalyst. The textural properties of the calcined Al40MCM-41 prepared by post-synthesis and conventional alumination were characterized by X-ray diffraction, N2 isothermal adsorption measurements (Brunauer–Emmett–Teller and Barrett–Joyner–Halenda), transmission electron microscopy, and X-ray photoelectron spectroscopy.


References

[1]  M. Oliverio, A. Procopio, T. N. Glasnov, W. Goessler, C. O. Kappe, Aust. J. Chem. 2011, 64, 1522.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BC3MXhsVOqu7zJ&md5=e7e1bace987c02265ba8144f54b1121eCAS |

[2]  R. Franchi, P. J. E. Harlick, A. Sayari, Stud. Surf. Sci. Catal. 2005, 156, 879.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD2MXhtFKjtLfM&md5=e9d7f39d83271d2ee410d5d52bbd6c37CAS |

[3]  N. Hondow, J. Harowfield, G. Koutsantonis, G. Nealon, M. Saunders, Microporous Mesoporous Mater. 2012, 151, 264.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BC3MXhs12gsrfO&md5=ac2c4a06f6dd33d222c61d0f1f1e256eCAS |

[4]  S. K. Jana, H. Takahashi, M. Nakamura, M. Kaneko, R. Nishida, H. Shimizu, T. Kugita, S. Namba, Appl. Catal. A Gen. 2003, 245, 33.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD3sXjvVOisLk%3D&md5=536216d391599cc465769842930862bfCAS |

[5]  S. Ajaikumar, A. Pandurangan, J. Mol. Catal. Chem. 2007, 266, 1.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD2sXjtVegsLg%3D&md5=b766f6529b538c0c0abc66d9fdbc400aCAS |

[6]  N. Saadatjoo, M. Golshekan, S. Shariati, H. Kefayati, P. Azizi, J. Mol. Catal. Chem. 2013, 377, 173.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BC3sXht1SkurvJ&md5=0cb62726cc85a9fd8eb86f14e60aca23CAS |

[7]  L. Y. Chen, Z. Ping, G. K. Chuah, S. Jaenicke, G. Simon, Microporous Mesoporous Mater. 1999, 27, 231.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK1MXit1Ogs7o%3D&md5=2485024f8f572508023d5d5ea2791a7cCAS |

[8]  A. S. Araujo, V. J. Fernandes, M. J. B. Souza, O. S. A. Silva, J. M. F. B. Aquino, Thermochim. Acta 2004, 413, 235.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD2cXhsVOnt7s%3D&md5=a3cec1bc2ce142fba9e0c37b9e86cda2CAS |

[9]  H. Polli, L. A. M. Pontes, A. S. Araujo, J. M. F. Barros, V. J. Fernandes, J. Therm. Anal. Calorim. 2009, 95, 131.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD1MXis1altrY%3D&md5=fe21a876ca4853f5300ddecfcc7bab01CAS |

[10]  S. Arias, M. M. Prieto, B. Ramajo, A. Espina, J. R. García, J. Therm. Anal. Calorim. 2009, 98, 457.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD1MXhtlWnsb3O&md5=dcd7297520c5f6e74b560da2594c5f17CAS |

[11]  R. P. Rodríguez, R. Sierens, S. Verhelst, J. Therm. Anal. Calorim. 2009, 96, 897.
         | Crossref | GoogleScholarGoogle Scholar |

[12]  S. Vyazovkin, N. Sbirrazzuoli, Macromol. Rapid Commun. 2006, 27, 1515.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD28XhtFWqtLjI&md5=351891dd6ffea1124a76da07648cf3beCAS |

[13]  S. Vyazovkin, V. Goryachko, Thermochim. Acta 1992, 194, 221.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK38Xpt1Citg%3D%3D&md5=63385d48682823c81cfad722e2072a25CAS |

[14]  S. Vyazovkin, Int. J. Chem. Kinet. 1996, 28, 95.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK28XpsVagtg%3D%3D&md5=36d0d81e38342a52b883a16f009a20c8CAS |

[15]  S. Vyazovkin, N. Sbirrazzuoli, Anal. Chim. Acta 1997, 355, 175.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK2sXnvVSgtrg%3D&md5=87520b8aa29f62dca57d49cbcd19bfb9CAS |

[16]  S. Vyazovkin, C. A. Wight, Int. Rev. Phys. Chem. 1998, 17, 407.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK1cXls1ektr8%3D&md5=2780a4c775136a5ccf2760b00163ca5fCAS |

[17]  S. Vyazovkin, C. A. Wight, Thermochim. Acta 1999, 53, 340.

[18]  M. J. B. Souza, A. O. S. Silva, V. J. Fernandes, A. S. Araujo, J. Therm. Anal. Calorim. 2005, 79, 425.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD2MXkt1ChsLo%3D&md5=25f93db21dc631d420067ff4bd7001b8CAS |

[19]  F. W. T. Goh, Z. Liu, X. Ge, Y. Zong, G. Du, T. S. A. Hor, Electrochim. Acta 2013, 114, 598.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BC3sXhvFOisLrL&md5=8fa5cb68af5a7aa31c9fb44e73a3d80aCAS |

[20]  S. Brunauer, P. H. Emmett, E. Teller, J. Am. Chem. Soc. 1938, 60, 309.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaA1cXivFaruw%3D%3D&md5=d6b3a66aa466a7b74dd33c777b119faaCAS |

[21]  E. P. Barrett, L. G. Joyner, P. P. Halenda, J. Am. Chem. Soc. 1951, 73, 373.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaG3MXjsVygsg%3D%3D&md5=56bf005cd7b00dd5bf1c4a14083b57a1CAS |

[22]  M. J. B. Souza, A. S. Araujo, A. M. G. Pedrosa, B. A. Marinkovic, P. M. Jardim, E. Morgado, Mater. Lett. 2006, 60, 2682.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD28XmslChur4%3D&md5=bd278453c99dbd4d2b6f5545a1084bfeCAS |

[23]  M. J. Remy, M. J. Genet, G. Poncelet, P. F. Lardinois, P. P. Notte, J. Phys. Chem. 1992, 96, 2614.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK38XhsVaqsb4%3D&md5=722ca3085095755f8d7419c24d1c7afdCAS |

[24]  M. Kruk, M. Jaroniec, Y. Sakamoto, O. Terasaki, R. Ryoo, H. Ko, J. Phys. Chem. B 2000, 104, 292.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaK1MXnvVSlt7o%3D&md5=45d0d54620145fb77109c117d8ad9008CAS |

[25]  K. S. W. Sing, D. H. Everett, R. A. W. Haul, L. Moscow, R. Apierotti, T. Rouquerol, T. Siemienewska, Pure Appl. Chem. 1985, 57, 603.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DyaL2MXhvFWrtb4%3D&md5=483f745ef6f65402d89c9eaab5b28f7bCAS |

[26]  J. van den Brand, P. C. Snijders, W. G. Sloof, H. Terryn, J. H. W. de Wit, J. Phys. Chem. B 2004, 108, 6017.
         | Crossref | GoogleScholarGoogle Scholar | 1:CAS:528:DC%2BD2cXjt1Wls7s%3D&md5=2064a77a34e0cd23977eeec6d6bc800dCAS |