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以呫吨酮为起始原料,经二氯亚砜作用得到9,9-二氯呫吨中间体,继而与苯酚发生取代反应,探索了“一锅、二步”法制备含呫吨结构的双酚单体———9,9-二(4-羟基苯基)呫吨(BHPX)的新方法.在氮气保护下,在K2CO3存在下,以环丁砜为溶剂,将其与1,3-二(4-氟苯甲酰基)苯进行亲核缩聚反应,制得了一种高分子量的(数均分子量为45000,多分散性指数为1.9)新型含呫吨结构的Cardo型聚醚醚酮酮(PEEKK-X),并用FTIR,DSC,TG及WAXD等方法对其进行了分析表征.结果表明,所制得的聚合物(PEEKK-X)为无定形结构,其玻璃化转变温度(Tg)为215℃;在氮气气氛中5%的热失重温度(Td)为558℃,700℃时的残炭率为67%;在常温下易溶于非质子极性溶剂(如NMP、DMF和DMAc)和极性较弱的溶剂如CHCl3中.该聚合物可通过溶液浇铸成膜,所得到的薄膜韧性好,透明且耐折,其拉伸强度为81.5 MPa,杨氏膜量为2.48 GPa,断裂伸长率为16.8%.
Xanthones were used as starting materials to obtain 9,9-dichloro xanthene intermediates through the action of thionyl chloride, followed by substitution reaction with phenol to explore the “one-pot, two-step” method for preparing xanthene Structure of bisphenol monomer --- 9,9-bis (4-hydroxyphenyl) xanthene (BHPX) a new method under the protection of nitrogen in the presence of K2CO3 with sulfolane as solvent, and 1, 3-bis (4-fluorobenzoyl) benzene was subjected to a nucleophilic polycondensation reaction to prepare a novel high-molecular-weight Cardo-type polyether ether having a number average molecular weight of 45,000 and a polydispersity index of 1.9 (PEEKK-X) were synthesized and characterized by FTIR, DSC, TG and WAXD.The results showed that PEEKK-X was amorphous and its glass transition temperature ( Tg) of 215 ° C .; 5% weight loss temperature (Td) at 558 ° C in nitrogen atmosphere and 67% carbon residue at 700 ° C; easily soluble in aprotic polar solvents such as NMP, DMF And DMAc) and less polar solvents such as CHCl3.The polymer was film-cast by solution and the resulting film had good toughness, transparency and folding resistance with a tensile strength of 81.5 MPa and a Young’s modulus of 2.48 GPa, elongation at break of 16.8%.