Calcination in Oxidative Atmospheres

Thermal treatment of a material in a gas oxidizing atmosphere is the simplest concept. This can be done in air, air diluted in N2, dry air, or in ultrahigh purity O2. In the laboratory practice, calcination is done in flowthrough beds, aided by fluidization, or in static box furnaces. Important aspects are the bed geometry, the removal of the generated gases, and temperature gradients. 

Thermal treatments can be applied to modify the properties of a material, for example, dealumination and optimization of crystalHne phases. These techniques do not require oxidants. Oxidative thermal treatments are generally employed to activate molecular sieves, by removing the organic templates employed during synthesis. This is one of the key steps when preparing porous catalysts or adsorbents. In air-atmosphere calcination, the templates are typically combusted between 400 

Novel Concepts in Catalysis and Chemical Reactors Improving the Efficiency for the Future. Edited by Andrzej Cybulski, Jacob A. Moulijn, and Andrzej Stankiewicz Copyright 2010 WILEY-VCH Verlag GmbH Co. KGaA, Weinheim ISBN 97S-3-527-32469-9 

Many studies on template thermal degradation have been reported on zeolites of industrial interest including ZSM5 [1-5], silicalite [1], and beta [6-8], as well as surfactant-templated mesostructured materials [9-13]. The latter are structurally more sensitive than molecular sieves. Their structure usually shrinks upon thermal treatment. The general practice is slow heating at 1 °C min (N2/air) up to 550 °C, followed by a temperature plateau. 

It is evident that dedicated studies are required for each structure to optimize the template oxidation protocol. Many structures, in particular nonsiliceous, are thermally very sensitive [14, 15]. Calcination can result in a complete breakdown due to hydrolysis, redox processes, and phase transformations. The removal of templates in those systems is critical, making the development of mild detemplation techniques necessary [16]. 

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The SC-155 material calcined in oxidizing atmosphere at 1000 "C and until constant weight produced a self supported porous silica network (the carbon was burnt out) which was called S-155 this silica structure maintained the same shape and volume as the original composite. On the other hand, the SC-155 treated with 20 % HF aqueous solution until the elimination of Si02 produced a self supported carbon network called C-155, and this carbon structure maintained the same shape and volume as the original composite. 

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