Synthesis of ZSM-5 from impure and beneficiated Grahamstown kaolin: Effect of kaolinite content, crystallisation temperatures and time

2016 
Abstract Raw kaolin obtained from Grahamstown, South Africa was beneficiated using wet sieving and filtration before use in the synthesis of ZSM-5 zeolite via hydrothermal treatment at various temperatures (120–190 °C) and times (24–96 h) under autogenous pressure. The impacts of kaolinite content and crystallisation parameters (i.e. temperature and time) on ZSM-5 formation were investigated. The mineralogical phases, morphology, surface area and porosity characteristics of the synthesised materials were investigated using XRF, XRD, FT-IR, HRSEM-EDS and N 2 physisorption (BET) analyses. Catalytic tests were carried out in a fixed bed reactor, WHSV of 8 h − 1 and a temperature of 350 °C at atmospheric pressure using 1-hexene as a feed. Beneficiation decreased the impurity content in the clay and increased kaolinite content which resulted in the formation of pure ZSM-5 zeolite. XRD and HR-SEM revealed that ZSM-5 synthesised from raw kaolin contained quartz and formed a ZSM-5/quartz coated composite. Temperature and time were critical in controlling phase purity and crystallinity of ZSM-5. At a synthesis temperature of 190 °C ZSM-5 transformed into a more thermodynamically stable quartz phase. The optimum condition for synthesising pure ZSM-5 from this clay was found to be 150 °C for 48 h. Morphology, surface area and porosity of ZSM-5 changed with an increase in crystallisation time. ZSM-5 with a high external surface area and presence of mesopores were observed in products synthesised at 150 °C for 24 h. Microporosity further developed as time increased and the ZSM-5 became more crystalline. The catalyst performance studies indicated that the ZSM-5 synthesised from raw and beneficiated kaolin at crystallisation conditions 150 °C and 48 h had good 1-hexene transformation activity and high selectivity to gasoline range hydrocarbons. The presence of quartz in the catalyst enhanced catalyst stability and selectivity to C 10  + hydrocarbons.
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