Russian Journal of Applied Chemistry, 2009, Vol. 82, No. 5, pp. 889−893.
Pleiades Publishing, Ltd., 2009.
Original Russian Text
E.N. Popova, V.E. Yudin, L.A. Myagkova, N.V. Kukarkina, M.Ya. Goikhman, V.M. Svetlichnyi, 2009, published in Zhurnal Prikladnoi
Khimii, 2009, Vol. 82, No. 5, pp. 834−838.
Among polymeric materials commercially produced
today, polyimides are the most heat-resistant .
They exhibit dielectric properties, high mechanical
characteristics, and good chemical and radiation
resistance. Therefore, they are demanded by various
branches of industry such as aviation and aerospace
industry, ship building, electronics, and instrument
making. Virtually all the kinds of technical materials
capable of prolonged service in articles at temperatures
of 300°C and above, including composite materials, are
based on polyimides. At the same time, the problem of
modifying the structure and properties of composites
based on polyimide binders and extending the ﬁ elds of
their application remains topical. Therefore, it seems
appropriate to study thermal aging of ﬁ brous composites
based on heat-resistant polyimide binders.
The goal of this study was to choose the optimal
composition of the polyimide binder and to prepare on
its basis a composite material preserving the viscoelastic
and strength characteristics after keeping in air at 350°C
for 100 h.
As starting compounds for preparing binders we
used commercially available monomers widely used in
industry in production of polyimides: cis-5-norbornene-
endo-2,3-dicarboxylic anhydride (NA), 3,3',4,4'-
benzophenonetetracarboxylic dianhydride (BZP),
3,3',4,4'-(diphenyl oxide)tetracarboxylic dianhydride
(DPO), 4,4'-diaminodiphenyl ether (DADPE), and
1,3-phenylenediamine (m-PDA), without additional
To prepare composite materials, we synthesized three
types of binders.
(1) Imide binder (IDA) of the composition DPO–
DADPE was prepared by the reaction of 3,3',4,4'-
(diphenyl oxide)tetracarboxylic dianhydride with bis(4-
acetamido)diphenyl oxide in the melt at 280–290°C, with
the removal of 10% volatiles. According to the reaction
mechanism , initially a set of oligomers containing
anhydride and N-acylamino groups are formed in the
melt. This melt with a viscosity of about 100 Pa s at 270°C
was used as prepolymer for impregnation of carbon or
glass fabric. Further heat treatment at 350°C for 1–2 h
leads to the formation of a polyimide:
(2) Imide polymerizable oligomer (IPO) with
terminal norbornene groups of the composition NA–(m-
PDA–DPO–DADPE)–NA based on 3,3',4,4'-(diphenyl
oxide)tetracarboxylic dianhydride, 4,4'-diaminodiphenyl
ether, and 1,3-phenylenediamine was prepared by
AND POLYMERIC MATERIALS
Thermal Aging of Carbon- and Glass-Reinforced Plastics
Based on Heat-Resistant Polyimide Binders
E. N. Popova, V. E. Yudin, L. A. Myagkova, N. V. Kukarkina,
M. Ya. Goikhman, and V. M. Svetlichnyi
Institute of Macromolecular Compounds, Russian Academy of Sciences, St. Petersburg, Russia
Received October 29, 2008
Abstract—A series of fibrous composites, carbon- and glass-reinforced plastics based on heat-resistant polyimide
binders, were prepared. The viscoelastic and strength properties of the composites obtained confirm the enhanced
heat resistance of the binders.