含硫醚和二氮杂萘酮结构聚芳醚酮的合成与性能

通过 4 ,4′ 硫代二酚 (TBP)、4 (4 羟基苯基 ) 2 ,3 二氮杂萘 1 酮 (DHPZ)与 4 ,4′ 二氟二苯酮 (DFK)反应合成出不同组分的高分子量共聚芳醚酮 .对聚芳醚酮的结构进行了FT IR、1 H NMR和1 3C NMR表征 ,表明共聚酮为无规结构 .对共聚芳醚酮的热性能、结晶性能、拉伸性能、溶解性能进行了测试 ,结果表明随硫醚结构含量的增加 ,共聚醚酮的玻璃化转变温度降低 ,材料韧性增强 ,溶解性能变差 ,所得的共聚物为无定型态 ,但由TBP和DFK制得的均聚醚酮为半结晶性

SYNTHESIS AND PROPERTIES OF POLYETHERKETONE CONTAINING SULFIDE AND PHTHALAZINONE MOIETIES

High molecular weight polyetherketones based on 4 (4 hydroxyphenyl) 1 phthalazinone(DHPZ) /4,4′ thiobisphenol TBP/4,4′ diflourodiphenylketone (DFK) were prepared by aromatic nucleophilic substitution reaction involving the toluene, N methyl 2 pyrrolidone(NMP) and anhydrous potassium carbonate.The copolymer having 50% TBP molar content was characterized by FT IR and 1H NMR.The results indicated that the copolyetherketones contained sulfide and phthalazinone moieties. 13 C NMR spectra were used to indentify the structure of copolyetherketones.According to 13 C NMR spectra,it was found that the structural repeat units were randomly distributed in the molecular chain of the copolyetherketones.The Glass transition temperatures ( T g) were determined by differential scanning calorimetry (DSC) after being kept 5 min to remove the thermal history and cooling to room temperature at approximately 100 K/min,the results showed that no melting point temperature was detected and all the polyetherketones have only one T g in the range of 137℃ to 263℃ and the T gs decrease linearly with the increase of sulfide moiety in the copolymers,which further indicated all of the polyetherketones are random or homogeneous.The wide angle X ray scattering was used to detected the crystallization of copolyetherketones.No crystal was formed for all the samples containing less than 70% TBP structure in the copolyetherketones and the polyetherketone polymerized by DFK and TBP was semicrystallization having melting point temperature of about 262℃.The results of the copolymers stress strain behavior indicated that,with the increase of sulfide moiety in the copolymers from 10% to 30%,the strain at break increased obviously.The solubility tests showed that the copolymers having more phthalazinone moiety have better solubility in some polar solvents.