Polymer fractionation using chromatographic column packed with novel regenerated cellulose beads modified with silane

摘要

Novel microporous beads with the particle size of about 90 mum were prepared, for the first time, from cellulose and konjac glucomannan (RC/KGM3) in 1.5 M NaOH/0.65 M thiourea aqueous solution by emulsification method. The microporous beads were then modified with silane to avoid the adsorption of polymers containing hydroxyl groups, coded as RC/KGM3-Si. A preparative size-exclusion chromatographic (SEC) column (500 mm x 20 mm) was packed with RC/KGM3-Si, and its exclusion limit and fractionation range of the stationary phase were, respectively, weight-average molecular masses (M-w) of 4.8 x 10(5) g/mol and 5.3 x 10(3)-4.8 x 10(5) g/Mol for polystyrene in tetrahydrofuran. The preparative SEC column was used to fractionate poly(epsilon-caprolactone) (PCL, M-w = 8.31 x 10(4) g/Mol polydispersity index d = 1.55) in tetrahydrofuran and a polysaccharide PC3-2 (M-w = 1.21 x 10(5) g/mol, d= 1.70) in 0.05 M NaOH aqueous solution, respectively. The M-w values of the fractions determined by analytical SEC combined with laser light scattering were from 1.2 x 10(4) to 1.84 x 10(5) for PCL and from 8.5 x 10(4) to 2.13 x 10(5) for PC3-2, as well as d from 1.2 to 1.5. The results indicated that the preparative SEC has good fractionation efficiency in both organic solvent and alkaline aqueous solution for the various polymers. (C) 2004 Elsevier B.V. All rights reserved.