The poly(cyanoarylether) was a new thermoplast being used as the basis of resin and engineering material in high property composite material.It exhibited high temperature stability,and resistance to radiation and to solvent attack.Crystalline ploy(cyanoarylether) could be prepared by the polycondensation of 2,6 difluorobenzonitrile with resorcinol at 200℃ in N methylpyrrolidone (with less water) in the presence of sodium carbonate.The reaction was affected by some conditions like temperature,polymer concentration and reaction time. A reaction temperature of at least 200℃ was necessary to attain high molecular weight polymer.Less water that was added in reaction mixture could improve reaction rate,and enhance molecular weight of the polymer.Spectral data indicated that the polymer had the structure of a poly(meta-phenylene ether) with pendent nitrile.The glass transition temperature and the melting temperature of the polymer were examined to be 148℃ and 335℃ bu turn.A cool crystalline exothermal peak appeared at 214.4℃.The decomposition temperature(loss weight 5%)and all weight loss by 900℃ of polymer were speculated from TG curve.The results showed the polymer had a fire-resistance and aging resistance properties.The glass temperature and the melting temperature of the polymer were almost the same as the poly(ether ether ketone)(PEEK).The crystalline behaviour of the polymer was studied bu X-ray diffraction method.The degree of crystallization was 30.7%.The polymer had five evident diffraction peak,which indicated the polymer had better crystalline behaviour.The poly(cyanoarylether) exhibited also excellent solvent resistance compared with the corresponding phenolphthalein polymer.This showed the molecular structure would affect on the solubility of the polymers.The crystal structune of the polymer was discussed by comparing with that of the poly(ether ether ketone).The poly(cyanoarylether) was the same as poly(ether ether ketone) to be attributed to orthorhombic system.The space unit parameter were computed.