Direct Synthesis of New Soluble and Thermally Stable
Poly(urethane-imide)s from an Imide Ring-Containing
Dicarboxylic Acid Using Diphenylphosphoryl Azide
Hossein Behniafar
Department of Chemistry, Damghan University of Basic Sciences, 3671616549, Damghan, Iran
Received 3 May 2005; accepted 16 October 2005
DOI 10.1002/app.23483
Published online in Wiley InterScience (www.interscience.wiley.com).
ABSTRACT: The direct preparation of various aromatic
poly(urethane-imide)s from 4-p-biphenyl-2,6-bis(4-trimelliti-
midophenyl)pyridine (1) using diphenylphosphoryl azide
(DPPA) was investigated. The polymers were mainly ob-
tained by the conversion of imide ring-containing diacid 1 to
corresponding di(carbonyl azide) 2 with DPPA and then to
diisocyanate 3 through the Curtius rearrangement of com-
pound 2 followed by polyaddition of 3 in different amounts
with aromatic dihydroxy compounds. The molecular
weights of the resulting poly(urethane-imide)s were evalu-
ated viscometrically. All of the resulted polymers were thor-
oughly characterized by spectroscopic methods and elemen-
tal analyses. The poly(urethane-imide)s exhibited an excel-
lent solubility in a variety of polar solvents. Crystallinity
nature of the polymers was estimated by means of WXRD.
The glass-transition temperatures of the polymers deter-
mined by DSC method were in the range of 191–202°C. The
10% weight loss temperatures of the poly(urethane-imide)s
from their thermal gravimetric analysis curves were found
to be in the range of 392– 416°C in nitrogen. The films of the
resulting polymers were also prepared by casting the solu-
tion. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 869 – 877,
2006
Key words: direct polycondensation; poly(urethane-imide)s;
inherent viscosity; diphenylphosphoryl azide
INTRODUCTION
Diisocyanates are widely used as initial monomers for
the preparation of various kinds of polymers.
1–4
The
commercial use of the most diisocyanates is often
limited because of their poor stability, and in fact,
these compounds are very susceptible to deterioration
during storage.
5
In the field of polymeric materials,
one approach to solving this problem is to employ
di(carbonyl azide) precursors as starting monomers in
stead of diisocyanates for direct synthesis of them. In
1983, Ghatge and Jadhav reported the synthesis of m-
and p-hydroxyethoxy benzoyl azides, and the direct
polymerization of these monomers to homo- and ran-
dom copolyurethanes. Because it was difficult to iso-
late monomers with reactive groups, these workers
generated isocyanate groups in situ of the polymer-
ization stage.
6
Thereafter, in 1991, various kinds of
polyurethanes were prepared by Nishi et al. through
the reaction of a hydroxyl group with the isocyanate
group that was formed by Curtius rearrangement of
the carbonyl azide precursor.
7
In general, the most
carbonyl azides are readily converted to correspond-
ing isocyanates, which react in situ with hydroxylic
compounds to form urethanes.
8,9
Moreover, it is mentionable that a major drawback
of polyurethanes is their poor resistance toward me-
chanical strains and high temperatures. Generally,
their acceptable mechanical properties vanish above
80°C and thermal degradation takes place above
200°C.
10
Various attempts have been made to incor-
porate imide heterocyclic units into polyurethane
backbone.
11–17
On the other hand, the most heat resis-
tant homopolyimides have almost poor processability
because of their insolubility in common organic sol-
vents. However, it is found that the synthesis of co-
polyimides by the introduction of other functional
groups into the polymer backbone remarkably en-
hance their positive properties.
18 –21
Therefore, the
presence of urethane linkages by the side of imide
groups into a copolymer chain is useful both for poly-
urethane and polyimide. This putting together in-
creases thermal stability and processability of polyure-
thane and polyimide, respectively.
In our previous studies, we successfully prepared a
series of wholly aromatic poly(amide-imide)s, poly(es-
ter-imide)s, and poly(urethane-imide)s from a number
of new imide-containing dicarboxylic acids.
22–27
Among
them, a dicarboxylic acid bearing two imide rings 4-p-
biphenyl-2,6-bis(4-trimellitimidophenyl)pyridine, 1, was
used for some polymerization purposes. The results
Correspondence to: H. Behniafar (h_behniafar@dubs.ac.ir).
Contract grant sponsor: Research Council of Damghan
University of Basic Sciences.
Journal of Applied Polymer Science, Vol. 101, 869 – 877
(2006)
© 2006 Wiley Periodicals, Inc.