Macromolecules, Vol. 35, No. 13, 2002
Hyperbranched Poly(arylene-ether-ketone-imide) 4959
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ether-ketone-imide) (0.1 g, 0.22 mmol), potassium carbonate
(0.2 g, 14.5 mmol), epichlorohydrin (0.30 g, 2.52), and NMP
(10 mL) were placed. The reaction mixture was then heated
and maintained at 80-90 °C for 10 h. During this time period,
the orange solution became light yellow in color and homoge-
neous. After it had been allowed to cool on its own, the mixture
was filtered through a cake of Celite 545 to remove any
insoluble salts. The filtrate poured in a beaker containing 5%
hydrochloric acid (300 mL), and the mixture was warmed
around 60-70 °C for 2 h. The white powder was collected and
dried under the reduced pressure in the presence of phospho-
rus pentoxide at 50 °C for 48 h. The yield was essentially
quantitative. [η] ) 0.08 dL/g; Tg ) 174 °C. Anal. Calcd for
C
31H17NO6: C, 74.55%; H, 3.43%; N, 2.80%; O, 19.22%.
1
Found: C, 73.07%; H, 3.82%; N, 2.70%; O, 17.99%. H NMR
(DMSO-d6, δ in ppm): 3.33 (s, 2H, -CH2-CH(O)CH2), 3.70
(s, 1H, -CH2-CH(O)CH2), 3.95 (s, 2H, -CH2-CH(O)CH2), and
7.16-8.38 (m, 14H, Ar-H).
Solu tion Blen d in g of AT-P AEKI w ith BP A-BMI. A stock
solution was first prepared by dissolving AT-PAEKI (0.1 g)
completely in THF (10 mL). It was then added to the vials
containing predetermined amounts of BPA-BMI (0.098-0.068
g) so as to prepare the solutions with AT-PAEKI content
ranging from 2 to 32 wt %. Each vial was then diluted with
additional THF until the mixture became homogeneous over-
night. The solvent was then removed from the blend solutions
via rotary evaporation. The resulting solid blends (all formed
a coating on the vial walls) were pulverized with a spatula.
The power samples were then dried under reduced pressure
at 70 °C for 48 h prior to thermal analysis. The DSC
thermograms were recorded on the powder samples after they
had been heated to 150 °C, cooled to 20 °C (first cycle), heated
again to 320 °C, cooled again to 20 °C (second cycle), finally
heated to 350 °C and cooled to room temperature (third cycle),
all with heating or cooling rate of 10 °C/min. The thermal data
are summarized in Table 2. Figure 5a shows the initial scans
(after first and second cycles) for BMI-BPA and its blends
with AT-PAEKI. No thermal transition was detected for all
samples during the third cycle scans (Figure 5b).
Ack n ow led gm en t. We are grateful to Charles Ben-
ner (University of Dayton Research Institute) for GPC
data, Marlene Houtz (University of Dayton Research
Institute) for TGA data, and Dr. Kevin Church (Depart-
ment of Chemistry, University of Dayton) for NMR
spectra.
(27) (a) Stenzenberger, H. D.; Romer, W.; Herzog, M.; Konig, P.
Int. SAMPE Symp. 1988, 33, 1546. (b) Stenzenberger, H. D.;
Romer, W.; Hergenrother, P. M.; J ensen, B. J . Int. SAMPE
Symp. 1989, 34, 2054. (c) Stenzenberger, H. D.; Romer, W.;
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(29) BPA-BMI (2,2-bis[4-(4-maleimidophenoxy)phenyl]propoane)
was reported to have mp 119-120 °C, an exotherm with onset
and peak temperatures at 203 and 302 °C, respectively, and
complete cure at 344 °C; a cure at Tg 312 °C (determined by
TMA) after it was cured for 10 h at 280 °C. See: Takeda, S.;
Akiyama, H.; Kakiuchi, H. J . Appl. Polym. Sci. 1988, 35,
1341.
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