Polymeric compositions comprising per(phenylethynyl) arene derivatives
a technology of phenylethyl and isne derivatives, which is applied in the direction of solid-state devices, basic electric elements, semiconductor devices, etc., can solve the problems of difficult to solve polymeric thermoset systems, art has not managed to solve problems,
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example 1
Preparation of the Per(phenylethynyl)arene polymer 1,2,4,5-tetra(phenylethynyl)benzene
[0070]
[0071]A three-necked, glass reaction vessel is fitted with a thermometer, magnetic stir bar, condenser, static nitrogen inlet, and addition funnel then charged with 9.00 grams (g) (0.0229 mol) of 1,2,4,5-tetrabromobenzene, 0.2232 g (0.318 mmol) of bis(triphenylphosphine)palladium (II) chloride, 0.1668 g (0.636 mmol) of triphenylphosphine, 0.1211 g (0.636 mmol) of copper (I) iodide, and 180 g of triethylamine. The solution was heated to 70° C. with stirring. A solution of 9.34 g (0.0914 mol) of phenylacetylene and 50 g of triethylamine was then added drop-wise over the course of 2 hours. The addition rate was such that the temperature of the reaction mixture did not exceed 80° C. After complete addition, the reaction mixture was stirred for an additional 17 hours at 80° C. The reaction mixture is then cooled to room temperature and the precipitate is removed via filtration. The filter cake is ...
example 2
Preparation of Polymeric Composition comprising PAE-2 and 1,2,4,5-tetrakis(phenylethynyl)
[0072]0.2999 g of PAE-2 and 0.2008 g of 1,2,4,5-tetrakis(phenylethynyl) prepared in accordance with Example 1 were combined in ˜15 mL of tetrahydrofuran and dried briefly at 100° C. on a hotplate, followed by overnight at 120° C. in an oven. The residue was subjected to 220° C. in nitrogen atmosphere for 30 minutes (10 C / min ramp), which resulted in a weight loss of 1.24%, then cooled and reheated to 400° C. at 10° C. / minute and held at 400° C. for 120 minutes. The residue had 3.42% weight loss at 400° C. isothermal. The DSC showed a melt endotherm at 185° C. and a two peak exotherm at ˜305° C. and 390° C. on the first heat. The second heat was predominantly featureless, indicating crosslinking had occurred, and an interpenetrating network had formed.
example 3
Adhesion Results for Polymeric Composition comprising PAE-2 and 1,2,4,5-tetrakis(phenylethynyl)benzene
[0073]A solution was prepared from 1,2,4,5-tetrakis(phenylethynyl)benzene and PAE-2 (prepared in accordance with Example 2) was as follows:
[0074]
[0075]A 0.3997 g portion of 1,2,4,5-tetrakis(phenylethynyl)benzene and 0.6003 g of the poly(arylene ether) PAE-2 were dissolved in 9.0 g of distilled cyclohexanone. The solution was applied to six 1″×4.25″×0.32″ cold roll steel coupons provided by Act Laboratories Inc., Part #APR14839. The coupons were overlapped to form three test pieces with 0.5 sq. inch overlap area. All three pieces were heated to 400° C. and held at temperature for 10 minutes with a 10 lb. weight resting on each piece. The three pieces were subjected to Lap Shear Analysis, ASTM method D-1002 (metal). The results of this analysis are provided in the Table II below. The results show good adhesion for the cured polymer matrix to the steel substrate.
[0076]
TABLE IIStress at...
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