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

Inactive Publication Date: 2015-08-19
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the field of traditional dielectric materials, barium titanate and other ferroelectrics are typical representatives of high dielectric materials. They have a high dielectric constant and excellent dielectric properties, but they have disadvantages such as heavy weight, high molding temperature, and brittleness. Apps are increasingly restricted

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a preparation method of aromatic thermosetting resin containing polycarboxyl metal phthalocyanine. The method includes: employing a phthalic anhydride method to prepare polycarboxyl metal phthalocyanine, adding the metal phthalocyanine into an aromatic thermosetting resin prepolymer monomer and mixing them uniformly, leaving the mixture to undergo a high temperature reaction so as to obtain two prepolymers, i.e. Cx-MPc-COOH and Ax-MPc-COOH, mixing the two prepolymers uniformly, performing high temperature curing, thus obtaining an aromatic thermosetting resin composite material containing polycarboxyl metal phthalocyanine. The various monomers for synthesizing the aromatic thermosetting resin are terminated by carboxyl and ester groups, the polycarboxyl metal phthalocyanine can undergo chain transfer reaction with the monomers so as to be introduced into a molecular network structure of aromatic thermosetting resin. The method makes use of the excellent electron donating ability of metal phthalocyanine to perform coupling with the conjugated structure of aromatic thermosetting resin, thus reaching the purpose of improving dielectric properties of aromatic thermosetting resin. With the properties of high temperature resistance, ablation resistance, easy adhesion and the like, the aromatic thermosetting resin prepared by the invention has important applications in micro-electronics, semiconductors, electromagnetic materials, electrical smart materials and other fields.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a preparation method of an aromatic thermosetting resin containing polycarboxyl metal phthalocyanine. Background technique [0002] With the rapid development of information technology and the continuous advancement of electronic technology, dielectric materials are widely used in the preparation of passive devices (capacitors and resistors, etc.), embedded capacitors, ferroelectric storage memory, pyroelectric detectors, ferroelectric optics Devices, electrical insulating materials and other devices. In the field of traditional dielectric materials, barium titanate and other ferroelectrics are typical representatives of high dielectric materials. They have a high dielectric constant and excellent dielectric properties, but they have disadvantages such as heavy weight, high molding temperature, and brittleness. Applications are increasingly restricted. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/68
Inventor 邱军李旦
Owner TONGJI UNIV
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