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Synthesis, Characterization, and Gas Permeation Properties

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t-Butylcarbamates of Cellulose Derivatives<br />

wavenumber range. Moreover, the absence of the peak around 2270–2100 cm -1 ,<br />

assignable to the isocyanate group of the starting material, provided a clear evidence of<br />

the product purification.<br />

Figure 3. FTIR spectra of 1, 2, 1a, <strong>and</strong> 2a.<br />

The molecular weights of the starting as well as the derivatized polymers were<br />

determined by the gel permeation chromatography <strong>and</strong> the data are summarized in<br />

Table 1. The molecular weight determination of ethyl cellulose (1; DSEt, 2.69 <strong>and</strong> 2;<br />

DSEt, 2.50), cellulose acetate (3; DSAc, 2.46), <strong>and</strong> their carbamate derivatives (1a–3a)<br />

was carried out by making use of THF as eluent while for 4 <strong>and</strong> 4a, elution was<br />

effected with LiBr solution (10 mM) in DMF because of the insolubility of cellulose<br />

acetate (4; DSAc, 1.80) in THF. The carbamoylation of cellulose derivatives<br />

accompanied an increase in the molecular weight of the polymers, e.g., the Mn of 3 <strong>and</strong><br />

4 were observed to be 64 000 <strong>and</strong> 89 000 while those for 3a <strong>and</strong> 4a were 70 000 <strong>and</strong><br />

93 000, respectively. Moreover, the polydispersity indices (Mw/Mn) of the carbamate<br />

derivatives (1a–4a) were not quite different from those of 1–4, for instance, the Mw/Mn<br />

of 2 <strong>and</strong> 2a were 2.6 <strong>and</strong> 2.4 <strong>and</strong> for 3 <strong>and</strong> 3a were 2.3 <strong>and</strong> 2.2, respectively, thus<br />

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