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A typical polymerization was carried out according to the following
procedure. Succinic acid (44.9 g, 0.38 mol) and isosorbide (63.4 g,
0.43 mol) were weighed into a 250 mL round-bottom glass flange
reactor. The reactor was fitted with a Vigreux column and a Dean-
Stark-type condenser
to collect the condensation product. During the
first part of the synthesis, the setup was continuously flushed with inert
gas to limit oxidation and facilitate transport of water vapor. While
being stirred, the mixture was heated to 180 ¡ãC using a heating mantle.
Titanium(IV) n-butoxide (0.02 mol % relative to succinic acid),
dissolved in toluene, was added to the melt. Subsequently, the reaction
temperature was increased stepwise to maintain distillation of the
formed water. The maximum reaction temperature was 250 ¡ãC. After
4 h, vacuum processing was started at 230-250 ¡ãC, with typical
pressures ranging from 1 to 5 mba
r. Vacuum was applied for 4 h, after
which the polymer was discharged from the reactor and left to cool
and solidify.

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[ Last edited by wizardfox on 2008-9-10 at 15:09 ]
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