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Title: Hydrothermal stability of high silica zeolites
Author: Young, David
ISNI:       0000 0001 3575 6113
Awarding Body: University of Edinburgh
Current Institution: University of Edinburgh
Date of Award: 1988
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This thesis concerns the hydrothermal stability of two zeolite molecular sieves with the MFI structure, ZSM-5 and its 'aluminium free' form silicalite. Silicalite was synthesised from low pH alkali metal free aqueous gels at 95°C and characterised by XRD, SEM, DTA and TG. ZSM-5 was crystallised from similar reaction mixtures but with the addition of aluminium salts. It was found that the incorporation of aluminium into the ZSM-5 framework was favoured by higher reaction temperatures (l50°C) and the use of aluminium nitrate. Solubilities were measured for silicalite, ZSM-5, ZSM-11, ZSM-39, ZSM-48 and EU-4 at temperatures up to 95°C. The solubilities were influenced by framework structure, the presence of template within the zeolite channels and the aluminium content of the lattice. Solubility measurements over a range of liquid/solid ratios showed that calcined silicalite was contaminated with about 1% amorphous silica. Treatment with liquid water over the temperature range 95 to 230°C was used to remove amorphous silica and alnminosilicate species from silicalite and ZSM-5. This hydrothermal treatment had many other effects on the properties of these materials. The water uptake, orthorhombic to monoclinic symmetry transition, framework Si/Al ratio and thermal properties were all affected. SEM showed that the inside of the silicalite crystals was more soluble than the outer surface. The use of hydrothermally treated H-ZSM-5 as a catalyst for but-1-ene isomerisation showed that the treatment could have a marked effect on catalytic behaviour, and particularly on product selectivity.
Supervisor: Lowe, B. M. Sponsor: Science and Engineering Research Council
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: Zeolites ; Molecular sieves ; Silica