Method for preparing high glass-transition temperature crystal type polyethylene-ketone-ketone resin material

Abstract

The invention belongs to a new high performance and high polymer material synthesis field, in particular to a method for preparing a novel high glass-transition temperature crystal type polyethylene-ketone-ketone resin material in a such way that a monomer solutions of diphenyl ether and aromatic acyl chloride are dropwise added in a system, and a Friedel-Crafts low temperature solution electrophilic substitution polymerization is carried out. The viscosity of the resin materials synthesized by the method can be precisely controlled within 0.50-1.10+ / -0.10 dL / g, the glass-transition temperature can be controlled between 168 DEG C and 175 DEG C, and the melting temperature can be controlled between 310 DEG C and 360 DEG C. Compared with the FC of the same kind of already commercialized products, under the condition that the materials maintain excellent melting processing performance, the polymer has the glass-transition temperature 15 DEG C higher than that of the products, so that the invention has excellent heatproof performance.

Description

technical field The invention relates to the synthesis of a novel high glass transition temperature crystalline polyaryl ether ketone resin material, belonging to the field of novel high-performance polymer material synthesis. Background technique Crystalline polyether ketone ketone resin material with full aromatic ring structure has excellent properties, such as excellent mechanical properties, solvent resistance and chemical corrosion resistance (almost only soluble in concentrated sulfuric acid at room temperature), radiation resistance, good resistance Flammability and electrical insulation. Highly demanding applications in automotive, aerospace, electronics, and petroleum. Polyaryl ether ketone resin materials with many excellent properties can be prepared by two different methods, one is to form aryl ether ketone segments through electrophilic substitution reactions; the other is to form aryl ether ketone segments through nucleophilic substitution reactions chain s...

AI Technical Summary

Problems solved by technology

The two-step synthesis method developed by DuPont includes first synthesizing an oligomer with a regular sequence structure and a low activity of the aromatic hydrogen atom and a high positioning, and then by first low-temperature polymerization of the aromatic oligomer and an aromatic acid chloride, and then rapidly The two-step method of transferring to high-temperature (150°C) stage polymerization, due to the limitation of many synthesis steps and harsh production conditions, the output of a single batch is low, resulting in high production costs; and the Lewis acid-Lewis base developed by Raychem Synchronous catalytic method is owing to be subjected to the influence of branching side reaction, can not obtain high molecular weight polymer material (US4826947) with diphenyl ether as starting material, also needs at first synthetic active lower ketone-containing aromatic ether monomer, and then Polymerization with aromatic acid chloride monomers also prolongs the reaction route and increases production costs

Domestic research on the synthesis of polyetherketoneketone by electrophilic substitution began in the 1990s, basically following Raychem's Lewis acid-Lewis base synchronous catalytic method, and the glass transition of polyetherketoneketone (PEKK) materials that have been reported The temperature is low (165°C), and the crystallization temperature is sensitive to the change of the ratio of the middle position / para acid chloride structure of the polymer main chain, and it is not easy to unify the processing conditions and processing methods; it is different from the above-mentioned commercialized polyether ketone ketone (PEKK ) materials, under the premise of having the same meta-parasite ratio structure, its crystallization temperature is as high as 365°C, which will lead to its processing temperature approaching or exceeding 400°C, which basically exceeds the processing capacity of existing equipment. These constraints lead to The application of synthetic materials using this method has been greatly limited