Introduction Catalysis is a vital part of the production of many industrially significant chemicals today.

Roughly 90% of all commercially produced chemical products involve catalysts at some stage in the manufacturing process [1]. A catalyst is a substance that increases the rate of a chemical reaction without being consumed or undergoing any permanent chemical change. It works by providing a lower activation energy thermodynamic pathway for the reaction to occur and so its use results in an increase in reaction rate (Richardson, 1989). Catalysts can be homogeneous (act in same phase as reactants) or heterogeneous (act in different phase to reactants). At present, heterogeneous catalysts are more commonly used and so this report will discuss the synthesis, characterization and industrial uses of zeolite of type ZSM-5 (Lloyd, 2011). Zeolites are highly crystalline microporous aluminosilicate minerals consisting of a SiO4 and AlO4 tetrahedra three-dimensional structure [2]. Their framework contains channels in which water and cations are located [4]. 4+ 3+ The cations balance the negative charge produced from the isomorphous substitution of Si and Al within the 3-D structure and their mobility along with the presence of Bronsted and Lewis acid sites (located within crystalline structure) is the main reason for the ion-exchange properties and catalytic activity of zeolite [2]. The general empirical formula of zeolite is: ( ) ( ) ( ) [4]

Where: M=cation, m = number of moles of water of crystallization, x= number of AlO4 tetrahedra in unit cell, y= number of SiO4 tetrahedra in unit cell. ZSM-5 is usually synthesized from alkaline aqueous gels at high temperature (70 to 300 C) in a Teflon autoclave [4]. Its synthesis involves 3 solutions. The first contains a source of alumina, sodium ions, and hydroxide ions, the second a tetrapropylammonium cation and the third a source of silica [7]. The preparation procedure of ZSM is described in further detail in section 1.1. Catalyst properties that need to be considered to achieve good catalytic ZSM-5 performance are catalytic activity, selectivity and stability (Lloyd, 2011). An important parameter that also requires attention is the Si/Al ratio of the ZSM-5 to be produced, as this effects the severity of reaction conditions required. The higher the aluminium content the lower the intensity of process conditions required [3].
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Preparation The course of nucleation and crystallization of zeolite can generally be described by a characteristic S-shaped crystallization curve, in which the amount of crystalline material is plotted against crystallization time. A schematic diagram of the first and second steps for ZSM-5 preparation is reported in figx, according to Jacobs [30].

(1) Binding and forming. Extrusion is a widely applied method of shaping a zeolite into a pellet. For this a purpose a binder must be used. In fact by extruding a zeolite alone poor mechanical strengths are obtained. The binder can be selected among aluminas and silicaaluminas. In this case a pseudobohemite (Laroche V-450) is added with the zeolite powder in the weight ratio of 1. A paste is obtained by mixing the powder with an aqueous solution containing a plasticizer (1% Methocel, Fluka) and a peptizer (acetic acid, 2% of pseudo-bohemite). The mixing is performed in a Z-blade mixer till a homogeneous paste is obtained (about 2 h). The paste is then aged at room temperature for 2 h and o extruded. The extrudate is then aged (overnight, at room temperature), dried (at 100 C under o vacuum) and calcined (at 550 C in air flow for 10 h). The extrudate (cylinders of 2 3 mm) so obtained contains ZSM-5 (60.5%) and Al2O3 (39.5%).

complete transformation into the acidic form requires the elimination of Na . . The solid is then dried and calcined at 550 C under air flow.
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Preparation

The preparation method of a heterogeneous catalyst (e.g zeolite ZSM-5) has a strong influence on its catalytic properties and performance [4]. Properties that require attention during preparation to achieve good catalytic performance are catalytic activity, selectivity and stability (Lloyd, 2011). An important parameter that also requires attention is the Si/Al ratio of the ZSM-5 to be produced, as this effects the severity of reaction conditions required. The higher the aluminium content the lower the intensity of process conditions required [3]. At present, many preparation methods for the synthesis of zeolite ZSM-5 exist. However, most commonly o zeolite ZSM-5 is synthesized from alkaline aqueous gels at high temperature (70 to 300 C) in a Teflon autoclave [4]. Its synthesis involves 3 solutions. The first contains a source of alumina, sodium ions, and hydroxide ions, the second a tetrapropylammonium cation and the third a source of silica [7]. The tetraproplammonium ion acts as a template and is used to achieve a high pH, required to ensure aluminate ions stability [3]. The preparation of zeolite ZSM-5 comprises of 3 main steps: 1. 2. 3. Hydrothermal synthesis, Ionic exchange, Binding and shaping [4].

Hydrothermal synthesis The hydrothermal synthesis of zeolite ZSM-5 consists of 3 steps; production of reaction mixture gel (at o o temperatures below 60 C), crystallization of the synthesis gel (at 150 C) and separation, washing and drying of the resulting zeolite crystals [3]. To produce the reaction mixture gel firstly Aerosil, fumed silica prepared from the flame pyrolysis of SiCl4, is [4][8] added to an aqueous solution of tetrapropyl ammonium hydroxide (TPAOH) . A second solution, made from dissolving sodium aluminate in a concentrated NaOH solution, is then added to the primary solution under [4][3] intense agitation and a gel of the molar composition (TPA2O)24 (Na2O)0.3(Al2O3)(SiO2)60(H2O)1550 is formed . Inside it, equilibrium exists between the silicate and aluminate oligomers (solution) and the condensed silicate and aluminate components (gel phase). Crystallization of zeolite is achieved by elevating the gel temperature to 150 C in an agitated autoclave and [3][4] heating and ripening for 3 days under autogenous pressure . The initial increase in gel temperature causes dissociation of the silicate and aluminate oligomers and results in an increase in monomeric silicate and o aluminate components concentration. Once the gel reaches crystallization temperature (150 C), crystallization commences. The process takes 3 days to be completed. The zeolite crystals are then separated from the [3] mother liquor via filtration, washed with distilled water (5) and dried . Ion exchange The solid zeolite crystals produced via hydrothermal treatment consist of Na and TPAOH. These must be removed to obtain the required form of zeolite (ZSM-5). Therefore, firstly to remove the organic cation (TPAOH) and hence achieve access to the intercrystalline pore channel structure the zeolite crystals are calcined and undergo burning and thermal decomposition. The o o process consists of continuous calcination under dry nitrogen flow at 300 C (1 C/min heating rate) and air flow o up to 550 C for a period of three hours. It causes the decomposition of the organic cation and results in the production of protonic sites in the three-dimensional zeolite structure. Next, to remove the sodium cation from the zeolite structure ion exchange is carried out under reflux conditions using a 0.5 M ammonium nitrate (NH4NO3) solution with a liquid/solid ratio of 50. This process is
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repeated many times until he desired efficiency is achieved. The resulting solid is then dried and undergoes calcination be

Today, there exist many preparation methods of zeolite ZSM-5. One common method of synthesis is from o alkaline aqueous gels at high temperature (70 to 300 C) in a Teflon autoclave [4]. The method involves 3 solutions. The first contains a source of alumina, sodium ions, and hydroxide ions, the second a tetrapropylammonium cation and the third a source of silica [7]

References [1] ^ "Recognizing the Best in Innovation: Breakthrough Catalyst". R&D Magazine, September 2005,

pg 20. [2] nigerian kaolin [3] Preparation of catalyst supports, zeolites and mesoporous materials [4] catalyst preparation methods
[7]. ^
ab

U.S. Patent 3,702,886

Lloyd, L., 2011. Handbook of Industrial Catalysts. 1st ed. London: Springer. Richardson, J. T., 1989. Principles of Catalyst Development (Fundamental and Applied Catalysis). New York: Plenum Publishing Co.

[8] ^ Garrett, P.R. (1992). Defoaming. Theory and Industrial applications. USA: CRC Press. pp. 239 240. ISBN 0-8247-8770-6.