A monomer of tetrachloroterephthaloyl chloride (TCTPC) was prepared by the chlorination of terephthaloyl chloride catalyzed by ferric chloride at 175～180℃ for 10 h,and confirmed by FTIR,MS and elemental analysis.A s...A monomer of tetrachloroterephthaloyl chloride (TCTPC) was prepared by the chlorination of terephthaloyl chloride catalyzed by ferric chloride at 175～180℃ for 10 h,and confirmed by FTIR,MS and elemental analysis.A soluble polychloro substituted poly(aryletherketoneketone) (C-PEKK) was prepared by low temperature solution electrophilic Friedel-Crafts reaction of TCTPC and diphenyl ether (DPE) in 1,2-dichloroethane in the presence of AlCl 3 and N-methyl-2-pyrrolidinone(NMP).Effects of the molar ratio of monomers and the amounts of AlCl 3 and NMP on the polycondensation were investigated.Some propersites of the polymer was characterized by FT-IR,DSC,TGA and WAXD,etc.The results shown that the glass transition temperature(270℃) of the polymer is higher than that of pure PEEK and PEKK,and the polymer was noncrystalline.The polymer was soluble in common organic solvents such as DMF,DMSO,NMP,CHCl 3 and THF at room temperature and showed excellent thermal stability at temperature over 500℃ in air,high char yields of 61% in nitrogen and 54% in air at 700℃.展开更多
文摘A monomer of tetrachloroterephthaloyl chloride (TCTPC) was prepared by the chlorination of terephthaloyl chloride catalyzed by ferric chloride at 175～180℃ for 10 h,and confirmed by FTIR,MS and elemental analysis.A soluble polychloro substituted poly(aryletherketoneketone) (C-PEKK) was prepared by low temperature solution electrophilic Friedel-Crafts reaction of TCTPC and diphenyl ether (DPE) in 1,2-dichloroethane in the presence of AlCl 3 and N-methyl-2-pyrrolidinone(NMP).Effects of the molar ratio of monomers and the amounts of AlCl 3 and NMP on the polycondensation were investigated.Some propersites of the polymer was characterized by FT-IR,DSC,TGA and WAXD,etc.The results shown that the glass transition temperature(270℃) of the polymer is higher than that of pure PEEK and PEKK,and the polymer was noncrystalline.The polymer was soluble in common organic solvents such as DMF,DMSO,NMP,CHCl 3 and THF at room temperature and showed excellent thermal stability at temperature over 500℃ in air,high char yields of 61% in nitrogen and 54% in air at 700℃.
