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Title: Development of zeolites and zeolite membranes from Ahoko Nigerian kaolin
Author: Kovo, Abdulsalami Sanni
ISNI:       0000 0004 2737 2760
Awarding Body: University of Manchester
Current Institution: University of Manchester
Date of Award: 2011
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Zeolites and zeolite membranes are two important advanced chemical materials which are widely used in chemical processes. The manufacture of these materials usually involves the use of expensive chemicals. This study involves the use of Ahoko Nigerian kaolin (ANK) as precursor material for the development of zeolites and zeolite membranes. The synthesis of zeolite A, Y and ZSM-5 was successfully obtained following a sequence, collection of the raw clay from Nigeria, metakaolinization, dealumination and actual hydrothermal synthesis of the zeolites. Raw ANK was refined using sedimentation technique and about 97% kaolin was recovered from the raw sample. A novel metakaolinization technique was developed to convert kaolin into a reactive metastable phase. Amorphous metakaolin was obtained at a temperature of 600°C and exposure time of 10 min. This is a significant result because previous studies use higher temperatures and longer exposure times for the metakaolinization step. The metakaolin was used to prepare a number of different zeolites under various conditions. Highly crystalline zeolite A was obtained at an ageing time of 12 h, crystallization time of 6 h and crystallization temperature of 100oC. Zeolite Y was obtained at an ageing time of 3 h, crystallization time of 9 h and crystallization temperature of 100oC. Zeolite Y was also synthesised by using a dealuminated kaolin and highly crystallized zeolite Y with Si/Al ratio of 1.56 and BET surface area was obtained of 630 m2/g. ZSM-5 was synthesised using an ageing period of 36 h, crystallization time of 48 h and temperature of 140oC. The results obtained from zeolite powder synthesis from ANK were then used as guide to prepare supported zeolite films and membranes by a hydrothermal method. The effect of the support surface (stainless steel) was investigated using two synthesis methods namely modified in-situ and secondary (seeded) growth. Zeolite A, Y and ZSM-5 films were successfully prepared from ANK for the first time and on two modified supports, etched and oxidised. The zeolite films and membranes developed showed complete coverage on the two supports with the oxidised showing better adhesion and intergrowth. The separation performance of the three developed zeolite membrane was tested by pervaporation of water/ethanol mixture. The results of pervaporation of ethanol/water mixture showed that zeolite A membrane is highly selective towards water mainly because of hydrophilic properties occasioned by the high aluminium content. Zeolite Y membrane show a similar response when their separation performance was evaluated but with less selectivity because of reduced aluminium content. ZSM-5 showed selectivity towards ethanol because of it hydrophobicity allowing only ethanol to permeate. In all the zeolite membranes, the flux is lower in comparison to commercial zeolite membranes due mainly to the thickness of the zeolite layer. Oxidised support membranes showed better performance because of their better interaction between the oxide surface and the aluminosilicate gel. The results show that ANK can successfully be used to prepare zeolites and zeolite membrane.
Supervisor: Holmes, Stuart Sponsor: Petroluem Technology Development Fund
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: Zeolites ; Zeolite membranes ; Characterization ; Zeolite A ; Zeolite Y ; ZSM-5 ; Ahoko Nigerian Kaolin