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poly(amic acid), terminated by 4-(aminophenyl)trimethoxysilane; monomer(s): 4,4\-oxydiphthalic anhydride; 4,4\-oxydianiline; 4-(aminophenyl)trimethoxysilane[ No CAS ]
With phosphoric acid; water; In 1,2-dichloro-benzene; at 80℃;vacuum;Product distribution / selectivity;
The purpose of this Example was to show that without decantation, a relatively higher level of impurities levels were present in the 4,4'-oxydiphthalic anhydride that was produced, as compared to Examples 4 and 5 where decantation is practiced. 2645 parts of a WC of material consisting of 68.7 wt% 4,4'-oxydiphthalic anhydride, 13.3 wt% of potassium chloride, 18 wt% of ortho-dichlorobenzene based on total weight of the WC, and some minor impurities such as hexaethylguanidinium chloride (1146 ppm) and chlorophthalic anhydride (1591ppm), was mixed with 528 parts of phosphoric acid (85 wt%) and 11877 parts of water and heated under vacuum until boiling, about 80 C. Under these conditions, 4,4'-oxydiphthalic anhydride and <n="41"/>chlorophthalic anhydride react with the water to form 4,4'-oxydiphthalic tetraacid (ODTA) and chlorophthalic acid (ClDA). The oDCB was removed from the mixture as an azeotrope with water. The weight of the reactor was maintained constant by adding the corresponding amount of water back to the reactor. The process took approximately 25 hours. Subsequently, the mixture was cooled to 14 C and centrifuged. The WC was washed with 10 parts of water per part of 4,4'- oxydiphthalic tetraacid. 1492 parts of the final WC was obtained and it contained 85% of 4,4'-oxydiphthalic tetraacid and less than 30 ppm of hexaethylguanidinium chloride, 464 ppm of chlorophthalic acid and 64 ppm of potassium, with the balance (-15 wt%) being water.[0082] The example illustrates a method of purifying 4,4'-oxydiphthalic anhydride by aqueous hydrolysis and centrifugation.
poly(4-phenyl-ethynyl-phthalic anhydride)-co-(3,4'-oxydianiline)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In 1-methyl-pyrrolidin-2-one; at 100 - 350℃; for 1h;
Example 5; Synthesis of imide oligomer by Using 4-phenyl ethynyl phthalic anhydride Obtained in Example 3 and Comparative Examples 1 to 3 as Terminal End Groups; In accordance with the method as described in Non-Patent Document No. 2, a solution of an amide-acid oligomer having an average molecular weight of about 9,000 was prepared from the 4-phenyl ethynyl phthalic anhydrides obtained in Example 3 and Comparative Examples 1 to 3, and 3,4'-oxydianiline and an N-methylpyrrolidone solution of 4,4'-oxydiphthalic anhydride. The thus-prepared amide-acid oligomer was centrifuged, applied, dried and subjected to thermal treatments for one hour at 100° C., 225° C. and 350° C. in this order, to thereby obtain films of cross-linked imide oligomer. On the other hand, toluene was added to an N-methylpyrrolidone solution of the amide-acid oligomer and, the mixture was subjected to the steps of azeotropic dehydration, cooling, filtration, rinsing with water and methanol in this order, and drying, to thereby isolate an imide oligomer. Tg and kinetic properties at 23° C. of each film prepared in accordance with the above-described method corresponding to 4-phenyl ethynyl phthalic anhydrides obtained in Example 3 and Comparative Examples 1 to 3 were measured in accordance with a method as specified in ASTM D882 and, also a temperature at which 5percent by mass of the imide oligomer was reduced was measured by using a thermobalance. These results are shown in Table 1. TABLE 1 Production method for 4-phenyl Film of cross-linked Temper- ethynyl imide oligomer (23° C.) ature of phthalic Tensile Elastic Elongation 5percent mass anhydride Tg strength modulus at break reduction Example 3 252° C. 122.2 MPa 3.0 GPa 55percent 518° C. Comparative 250° C. 120.1 Mpa 2.6 GPa 31percent 514° C. Example 1 Comparative 252° C. 118.8 MPa 2.8 GPa 36percent 511° C. Example 2 Comparative 251° C. 119.7 MPa 2.7 GPa 36percent 514° C. Example 3
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