An effective technique for the synthesis of microporous gels is develo
ped along with correlations between synthesis conditions and microstru
cture. Such gels have substantially different properties than their no
nporous analogues. Microporous hydroxypropyl cellulose (HPC) gels were
prepared by heating aqueous HPC solutions above their lower critical
solution temperatures (LCST's) while cross-linking the polymer with di
vinyl sulfone. The effective porosity of the gel increased from 23 to
76% by decreasing HPC concentration from 22.6 to 9 wt%, as anticipated
from the system phase diagram. The pore size range decreased from 0.5
-9.0 to 0.05-0.2 mu m by increasing reaction time before phase separat
ion from 1.5 to 25 min, demonstrating that cross-linking in the homoge
neous state limits the extent of phase separation possible. Gel morpho
logy changed from open-celled to closed-celled by decreasing reaction
time in the phase-separated state, which limits cross-linking in the p
olymer-rich phase.