Sol-gel derived oxides and mixed oxides catalysts with narrow mesoporous distribution

A novel sol-gel process for preparing oxides and mixed oxides sols from precipitation and peptization process is reported in this article. Inorganic salts are used as raw materials in this study. It is found that the amount of acid has great influence on the stability and particle diameter distribution of the precursor sols. Ultrasonic treatment is used to prepare alumina sol at room temperature. The result of Al-27 NMR shows that there exist Al-13(7+) species in the sol. By controlling the sol particles with narrow particle diameter distribution, alumina, titania and silica-alumina (SA) materials with narrow mesoporous distribution are formed by regular packing of sol particles during gelation without using any templates. The results also show that the structure and particle diameter distribution of precursor sol determine the final materials' texture.

Acid catalyzed synthesis of ordered bifunctionalized mesoporous organosilicas with large pore

Thiol-functionalized mesoporous ethane-silicas with large pore were synthesized by co-condensation of 1,2-bis(trimethoxy-sily)ethane (BTME) with 3-mercaptopropyltrimethoxysilane (MPTMS) using nonionic oligomeric polymer C1H (OCH(2)-CH(2))(10)OH (Brij-76) or poly(alkylene oxide) block copolymer (P123) as surfactant in acidic medium. The results of powder X-ray diffraction (XRD), nitrogen gas adsorption, and transmission electron microscopy (TEM) show that the resultant materials have well-ordered hexagonal mesoscopic structure with uniform pore size distributions. (29)Si MAS NNR, (13)C CP-MAS NMR. FT-IR, and UV Raman spectroscopies confirm the attachment of thiol functionalities in the mesoporous ethane-sificas. The maximum content of the attached thiol group (-SH) in the mesoporous framework is 2.48mmol/g. The ordered mesoporous materials are efficient Hg(2+) adsorbents with almost every -SH site accessible to Hg(2+). In the presence of various kinds of heavy metal ions such as Hg(2+), Cd(2+), Zn(2+), Cu(2+) and Cr(3+), the materials synthesized using poly(alkylene oxide) block cooollxmier (Pluronic 123) g(2+), as surfactant show almost similar affinity to Hg(2+), Cd(2+), and Cr(3+), while the materials synthesized using ofigomeric polymer C(18)H(37)(OCH(2)CH(2))(10)OH (Brij-76) as surfactant exhibit high selectivity to Hg(2+). (C) 2004 Elsevier Inc. All rights reserved.

Catalytic cracking of 1-butene to propene and ethene on MCM-22 zeolite

Catalytic cracking of butene to propene and ethene was investigated over HMCM-22 zeolite. The performance of HMCM-22 zeolite was markedly influenced by time-on-stream (TOS) and reaction conditions. A rapid deactivation during the first I h reaction, followed by a quasi-plateau in activity, was observed in the process along with significant changes in product distributions, which can be attributed to the fast coking process occurring in the large supercages of MCM-22.

Synthesis of zeolite NaA membranes with high permeance under microwave radiation on mesoporous-layer-modified macroporous substrates for gas separation

This article reported the NaA zeolite membranes with high permeance synthesized with microwave heating method under different conditions: (1) on a macroporous substrate in gel, (11) on a mesoporous/macroporous (top-mesoporous-layer-modified macroporous) substrate in gel, and (111) on a mesoporous/macroporous substrate in sol. In general, the H-2 permeance of the NaA membranes by microwave heating in gel was usually at the level of 10(-6) mol s(-1) m(-2) Pa-1, much higher than that by the conventional hydrothermal synthesis. At similar H-2/C3H8 permselectivity. On the substrate modified mesoporous top layer, the H-2 permeance of the NaA membranes by microwave heating in gel or sol was further enhanced, while maintaining comparable H-2/C3H8 permselectivity, due to the prevention of penetration of the reagent into the pores of the macroporous substrate. Meanwhile, the synthesis took less time in sol than in gel on the mesoporous/macroporous substrate. The NaA membranes synthesized in sol had larger permeance than those in gel and underwent transformation in shorter time. The permeation of C3H8 suggested that there existed unwanted intercrystalline pores or defects in the membranes. © 2005 Elsevier B.V. All rights reserved.

Highly ordered periodic mesoporous ethanesilica synthesized under neutral conditions

Highly ordered mesoporous ethanesilica (MES) with 2D hexagonal structure was synthesized from 1,2-bis(trimethoxysilyl) ethane under neutral conditions for the first time. Divalent salts, such as NiCl2, MgCl2, ZnCl2, ZnSO4 and Zn(NO3)(2), were used to help the formation of the ordered mesostructure. The MES samples were characterized by powder X-ray diffraction, nitrogen sorption, transmission electron microscopy, FT-IR, C-13 and Si-29 solid-state NMR and thermal gravimetric analysis. A phase transition from a disordered wormhole-like structure to an ordered P6mm structure was observed upon the addition of inorganic salts. The pore size of the MES decreases from 4.7 to 3.9 nm with increasing content of the inorganic salts. Fluoride was also found to be important for the formation of ordered MES under neutral conditions.

Structural relation properties of hydrothermally stable functionalized mesoporous organosilicas and catalysis

The surfactant assistant syntheses of sulfonic acid functionalized periodic mesoporous organosilicas with large pores are reported. A one-step condensation of tetramethoxysilane (TMOS) with 1,2-bis(trimethoxysilyi)ethane (BTME) and 3-mercaptopropyltrimethoxysilane (MPTMS) in highly acidic medium was performed in the presence of triblock copolymer Pluronic P123 and inorganic salt as additive. During the condensation process, thiol (-SH) group was in situ oxidized to sulfonic acid (-SO3H) by hydrogen peroxide (30 wt % H2O2). X-ray diffraction studies along with nitrogen and water sorption analyses reveal the formation of stable, highly hydrophobic, and well-ordered hexagonal mesoscopic structures in a wide range of -CH2CH2-concentrations in the mesoporous framework. The resultant materials were also investigated by Si-29 MAS and C-13 CP MAS NMR, thermogravimetric analyses, UV-Raman spectroscopy, and FT-IR spectroscopy. The role of the bridged organic group on the hydrothermal stability of the mesoporous materials was established, which revealed an enhancement in hydrothermal stability of the materials with incorporation of the bridged organic groups in the network. The catalytic performance of -SO3H functionalized mesoporous materials was investigated in the esterification of ethanol with acetic acid, and the results demonstrate that the ethane groups incorporated in the mesoporous framework have a positive influence on the catalytic behavior of the materials.