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November 2005 Synthesis of zeolites and their application as soil amendments to increase crop yield and potentially act as controlled release fertilizers A thesis presented for the degree of Doctor of Philosophy by Vijay S. Jakkula November 2005 Synthesis of zeolites and their application as soil amendments to increase crop yield and potentially act as controlled release fertilizers Vijay S. Jakkula, B. Sc., M. Sc. A Thesis Submitted in partial fulfilment of the requirements of the University of Wolverhampton for the degree of Doctor of Philosophy. November 2005 This work or any part thereof has not previously been presented in any form to the University or to any other body whether for the purposes of assessment, publication or for any other purpose (unless otherwise indicated). Save for any express acknowledgments, references and/or bibliographies cited in the work, I confirm that the intellectual content of the work is the result of my own efforts and of no other person. The right of Vijay S. Jakkula to be identified as author of this work is asserted in accordance with ss.77 and 78 of the Copyright, Designs and Patents Act 1988. At this date copyright is owned by the author. Signature………………………………………. Date…………………………………………….. Abstract Zeolites have been used in agriculture since the 1960s, due to the effectiveness of these crystalline microporous solids as soil amendments for plant growth, their cation exchange capacity (CEC) and slow-release fertilizer properties. Most work on slow-release fertilizers has focused on natural Clinoptilolite, Phillipsite and Chabazite. The aim of this study was to synthesize zeolites, study their effectiveness as soil amendments and their ability to act as controlled release fertilizers to decrease nitrate leaching. Nitrate pollution of groundwater is a major agro-environmental concern. The zeolites Phillipsite and Linde-type F were synthesized from aluminosilicate gels; ion exchanged to introduce ammonium and characterized using X-ray diffraction (XRD), X-ray fluorescence (XRF), Thermo-gravimetric analysis (TGA) and Scanning electron microscopy (SEM) techniques, both before and after ion exchange. Ammonium- exchanged Phillipsites (natural and synthetic), ammonium-exchanged synthetic Linde-type F (the zeolite having highest affinity towards ammonium) and ammonium exchanged Phillipsites (high crystalline and high aluminium) were compared with conventional NPK fertilizer. Three glasshouse experiments were performed to study the effects of zeolite-amended soils on maize growth. Ion exchanged synthetic and natural Phillipsites were first used as soil amendments (w/w 2, 4, 8% zeolite to soil). Synthetic Phillipsite, at 2% loading, resulted in the most significant improvement in both plant growth and phased ammonium release. The synthetic ammonium-exchanged zeolites Phillipsite and Linde-type F (at w/w 1, 2, 4%) were then compared; synthetic Phillipsite, at 2% loading, again resulted in the most significant plant growth response with an increase (≥15%) in shoot dry weight and a decrease (≥30%) in nitrate leaching. Experiments using unexchanged synthetic Phillipsite (at w/w 2%), but with added NPK fertilizer, showed increased plant growth and decreased nitrate leaching, compared with parallel experiments containing unexchanged synthetic Linde-type F (at w/w 2%) and a conventional fertilizer amended soil. This revealed the beneficial effect of Phillipsite for soil amendment, even without ion exchange to the ammonium form. To study the physico-chemical properties affecting the release of ammonium from the Phillipsite framework; high crystalline/low aluminium and low crystalline/high aluminium forms were synthesized and ion exchanged. Both forms were introduced as soil amendments (at w/w 1 and 2%) and experiments showed that the lower zeolite crystallinity decreased cation exchange and therefore decreased nitrate leaching. Experimental results from the glasshouse experiments and cation exchange capacity (CEC) experiments suggest that synthetic Phillipsite, at lower loadings (1 and 2% w/w zeolite to soil) have most potential as soil amendments for both plant growth and controlled-release applications. This conclusion is supported by soil leachate and shoots dry weight analysis. Furthermore, Phillipsite, synthesized in a low crystalline and low ammonium form, may be an even better soil amendment for controlled release of ammonium, which will thereby further decrease nitrate pollution. Chapter 1 Introduction and Literature Review Introduction This study focuses on application of zeolites (alumino-silicate minerals) as soil amendments, to study plant growth responses from the slow/controlled release of ammonium from ion-exchanged zeolites used as fertilizer substitutes. Chapter 1 gives a brief overview of zeolites in general, their background, classification, application and ion exchange properties. A general overview of maize along with its nutrient requirements and aspects of nitrate pollution are also discussed in this chapter. 1.1. Zeolites 1.1.1. Historical Perspective The study of zeolites dates back to the 18th century, with the discovery of the mineral Stilbite by a Swedish mineralogist, A.F. Cronstedt in 1756 (Mumpton, 1978). The mineral lost water when heated with a blowpipe flame, a process now known as intumescence. He called this mineral “zeolite” from the Greek ‘zeo’, to boil and ‘lithos’, stone (Gottardi and Galli, 1985). Since then, zeolites have been recognized as a separate group of minerals, one of the most abundant on earth. Following their discovery, work has been performed on the hydration, dehydration, synthesis and ion exchange of these minerals. As cited in Van Bekkum et al. (2001), Eichhorn (1858) first reported reversibility of ion exchange on zeolite minerals and Damour (1840) showed that zeolite could be reversibly dehydrated with no apparent change in their transparency or crystal morphology. As cited in Szostak (1989), Friedel and Bull (1896) proposed that the structure of dehydrated zeolites consists of open porous frameworks. This was confirmed by occlusion of liquids, such as alcohol, benzene and chloroform, by dehydrated zeolites. Grandjean (1909) demonstrated that dehydrated Chabazite adsorbs ammonia, air, hydrogen and other molecules. The first molecular sieve effect was reported by Weigel and Steinhoff (1925), who observed that dehydrated Chabazite crystals rapidly absorbed water, methyl alcohol, ethyl alcohol and formic acid, but 1 essentially excluded acetone, ether or benzene. As cited in Van Bekkum et al. (2001), Schafhautle (1845) reported the hydrothermal synthesis of quartz by heating ‘gel’ silica with water in an autoclave. Levynite was the first hydro-thermally synthesized zeolite, as reported by St. Claire Deville (1862), who claimed to have made this zeolite from a solution of Na and K-silicates heated in a sealed glass tube to 170oC. The tubular hexagonal crystals formed had the composition: Ca0.25Na2.68K2.80[(AlO2)6.5(SiO2)11.5]. 16.8 H2O (1.1) Although the synthesis of zeolites has been reported from 1862 onwards, it was only after 1930 with the availability of X-ray diffraction techniques, that the synthesised products could be assigned complete based on their crystalline structure. As cited in Occelli and Robson (1992), Leonard (1927) first described the use of X-ray diffraction for identification purposes of mineral synthesis. Professor R.M. Barrer and his researchers early pioneering work in adsorption and synthesis began the era of synthetic zeolites in the mid-1930s. Barrer (1948) reported the first definitive synthesis of zeolites, including the synthetic analogue of zeolite mineral mordenite. The starting composition for this zeolite was Na2O: Al2O3: 8.2-12.3 SiO2. From this, Barrer explored the composition range to optimize the SiO2/Al2O3 ratio that would produce mordenite topology (Barrer, 1982). Inspired by Barrer’s work, studies were carried out on zeolite synthesis by both individuals as well as industries in search of new approaches for separation and air purification. In a span between 1949-1954 Milton and co-worker Breck discovered several zeolite types, zeolites A, X and zeolite Y were some of the important ones among them. Based on the properties of synthetic zeolites Union Carbide commercialized them as a new class of industrial materials for separation and purification in 1954. Mobil Oil introduced synthetic zeolite X as a cracking catalyst (breaking up large hydrocarbon molecules into smaller and more useful bits) in 1962. As cited in Barrer (1982), Zeolite Y was modified to “ultrastable zeolite Y” based on modification chemistry of steaming the zeolite (Grace, 1969). Henkel (1974) introduced zeolite A in detergents as a replacement for phosphates. More than 70 novel distinct framework structures of zeolites have been synthesized in recent decades. Some of the more important zeolite types that have been used in 2 commercial applications include natural minerals Mordenite, Chabazite, Phillipsite, Erionite and Clinoptilolite, and synthetic zeolites type A, X, Y, L, Mordenite, ZSM- 5, Beta, MCM-22, and zeolite F and W. 1.1.2. Introduction (a) Background After the discovery of zeolites, work was carried out to study their physical and chemical properties. In the 1930s a new term “molecular sieves” was introduced. McBain (1932) defined the term “molecular sieve” to describe a class of materials that exhibited selective adsorption properties. These materials contain other elements in addition to, or in lieu of, silicon and aluminium. Only two classes
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