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Inorganic Microporous Membranes for Gas Separation in Fossil Fuel ...

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2 Theoretical background<br />

Figure 11 Schematic draw<strong>in</strong>g of the colloidal and polymeric sol-gel technique 77<br />

The particle size of polymeric sols may be <strong>in</strong> the range of 2-20 nm whereas colloidal sols<br />

have particle sizes up to 1000 nm <strong>in</strong> diameter. Polymeric sols are prepared by add<strong>in</strong>g<br />

small amounts of water to keep the hydrolysis reaction slow, equation (6). The water can<br />

be added <strong>in</strong> a controlled method by:<br />

i) slowly add<strong>in</strong>g a high ratio alcohol/water solution,<br />

ii) <strong>in</strong> situ production of H2O by an esterification reaction,<br />

iii) dissolv<strong>in</strong>g an alkal<strong>in</strong>e base or<br />

iv) add<strong>in</strong>g a hydrated salt <strong>in</strong>to the alkoxide solution <strong>in</strong> alcohol.<br />

The catalyst can be applied to enhance the condensation reactions. Precursor modification<br />

or stabilisation is another method used to modify the precursors <strong>in</strong> order to reduce the<br />

hydrolysation rate. Ketones, am<strong>in</strong>es and carboxylic acids can stabilise the precursor and<br />

thereby decrease the hydrolysis reaction. Common precursor modifiers are acetyl acetone<br />

78,79 and diethanolam<strong>in</strong>e 78-83 <strong>for</strong> titania and zirconia polymeric sols.<br />

25

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