Nuclear Magnetic Resonance Investigation of the Fractionation
of Water–Ethanol Mixtures with Cellulose and Its Cross-Linked
Biopolymer Forms
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Abstract
Cellulose
(CE) was cross-linked with epichlorohydrin (EPI) at variable
compositions, and the fractionation properties were investigated in
binary water–ethanol (W–E) solutions, including the
pure solvent systems. The relative uptake of each solvent was measured
using quantitative <sup>1</sup>H nuclear magnetic resonance (qNMR)
spectroscopy. This study highlights the utility of qNMR as a rapid
screening method for estimation of solvent selective fractionation
in binary mixtures. The uptake properties of CE–EPI cross-linked
polymers with ethanol and water were well-described using the Sips
isotherm model. Modeling shows that the monolayer surface coverage
(<i>Q</i><sub>m</sub>) of ethanol and water onto the polymer
materials covers a range (1.13–2.44 g/g) of values with heterogeneous
adsorption behavior, in agreement with the Sips exponential fitting
parameter (<i>n</i><sub>s</sub> ≠ 1). The CE–EPI
adsorbents display unique fractionation with water and ethanol from
binary solutions, as evidenced by the relative selectivity (<i>R</i><sub>selectivity</sub>) value in binary W–E solvent
systems. The <i>R</i><sub>selectivity</sub> [<i>Q</i><sub>m</sub>(W)/<i>Q</i><sub>m</sub>(E)] values at saturative
conditions varied (from 1.10 to 2.03) and further illustrate that
CE materials display molecular selective solvent fractionation in
binary W–E solutions. This study provides a greater molecular
level understanding for the adsorptive uptake properties of CE that
are relevant to developing CE-based adsorbent technology for the fractionation
of biofuels and related chemical separations