A kind of preparation method of polycarboxy metal phthalocyanine-aromatic copolyester
A metal phthalocyanine and polycarboxyl technology, which is applied in the field of preparation of aromatic thermosetting resins, can solve the problems of high molding temperature, application limitation, weight and the like, and achieves the improvement of dielectric properties, excellent dielectric properties, and wide application range. Effect
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Embodiment l
[0024] Embodiment 1: take octacarboxy phthalocyanine copper as the initial raw material, respectively mix and react with monomers of aromatic copolyester oligomers to obtain Cx-CuPc-COOH and Ax-CuPc-COOH two kinds of oligomers, and then The two oligomers are uniformly mixed, heated and solidified to obtain copper phthalocyanine-aromatic copolyester.
[0025] Step (1): Using pyromellitic anhydride, urea, and cuprous chloride as raw materials and ammonium molybdate tetrahydrate as a catalyst, octacarboxyphthalocyanine copper is synthesized by a solid-phase method. In a 500ml three-necked flask equipped with a thermometer, a stirring rod, and a condenser tube, add 10.9g (0.05mol) pyromellitic anhydride, 3g (0.05mol) urea, 1.24g (0.0125mol) cuprous chloride, 0.1g Ammonium molybdate tetrahydrate. Stir mechanically, slowly heat to 190°C, react for 3 hours, then heat up to 210°C, react for 6 hours, cool and grind. Boil the powder with 4mol / L hydrochloric acid solution, suction filt...
Embodiment 2
[0029] Embodiment 2: using copper tetracarboxy phthalocyanine as raw material, uniformly mix with the monomer of aromatic copolyester oligomer respectively, high temperature reaction obtains two kinds of oligomers of Cx-CuPc-COOH and Ax-CuPc-COOH, and then The two oligomers are uniformly mixed, heated and solidified to obtain copper phthalocyanine-aromatic copolyester.
[0030] Step (1): Using 1,2,4-trimesic acid anhydride, urea, and cuprous chloride as raw materials and ammonium molybdate tetrahydrate as a catalyst, synthesize copper tetracarboxyphthalocyanine by a solid-phase method. Add 9.6g (0.05mol) of 1,2,4-trimesic anhydride, 3g (0.05mol) of urea, 1.24g (0.0125mol) of chlorinated chlorinated Copper, 0.1 g ammonium molybdate tetrahydrate. Stir mechanically, heat slowly to 240°C, react for 3 hours, cool and grind finely. Boil the powder with 5mol / L hydrochloric acid solution, suction filter while hot, wash with ethanol, and bake at 80°C for 10h. Then use 50% sodium hyd...
Embodiment 3
[0034] Example 3: Using octacarboxyl cobalt phthalocyanine as the initial raw material, they were evenly mixed with the monomers of the oligomers of the aromatic copolyester respectively, and reacted at high temperature to obtain two oligomers of Cx-CoPc-COOH and Ax-CoPc-COOH , and then the two oligomers are uniformly mixed, heated and solidified to obtain octacarboxyl phthalocyanine cobalt-aromatic copolyester.
[0035] Step (1): Using pyromellitic anhydride, urea, and cobalt chloride as raw materials, ammonium molybdate tetrahydrate as a catalyst, and nitrobenzene as a solvent to synthesize cobalt octacarboxyphthalocyanine. In a 500ml there-necked flask equipped with a thermometer, a stirring rod, and a condenser tube, add 10.9g (0.05mol) pyromellitic anhydride, 3g (0.05mol) urea, 1.625g (0.0125mol) cobalt chloride, 0.1g four Hydrated ammonium molybdate, 50ml nitrobenzene. Stir mechanically, slowly heat to 200°C, react for 1 hour, then raise the temperature to 240°C, react ...
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