双邻位甲基取代聚芳醚酮酰亚胺的合成与性能研究  

STUDY ON SYNTHESIS AND PROPERTIES OF POLY(ARYL ETHER KETONE IMIDE) HAVING BIS(o-METHYL) PENDENT GROUPS

作　　者：钟鸣[1] 徐玲[1] 宋才生[1] 戴润英[1] 黄红[1] 

机构地区：[1]江西师范大学化学化工学院,南昌330022

出　　处：《高分子学报》2008年第6期616-620,共5页Acta Polymerica Sinica

基　　金："十一五"军品配套项目(项目号JPPT-115-643);科技型中小企业技术创新基金(基金号06C26213601342)资助项目

摘　　要：N,N′-(4,4′-二苯甲烷)-二偏苯三甲酰亚胺酰氯(DIDC-M)分别与4,4′-二(2,6-二甲基-苯氧基)二苯酮(o-Me2-DPOBP)和4,4′-二(2,6-二甲基-苯氧基)三苯二酮(o-Me2-DPOTPDK)进行低温溶液共缩聚,合成了两种含双邻位甲基侧基和主链含亚胺结构的聚醚酮醚酮酰亚胺(o-Me2-PEKEKI-Pa)及聚醚酮酮醚酮酰亚胺(o-Me2-PEKKEKI-Pb)共聚物.用FT-IR,1H-NMR,DSC,TGA和WAXD对共聚物的结构和性能进行了表征.研究表明Pa和Pb均为非晶态结构;具有较高的玻璃化转变温度(Pa为240℃,Pb为237℃);能溶解于DMF、DMAc、NMP、二氯甲烷、氯仿等普通有机溶剂中,溶剂挥发后成膜性良好,可制成透明薄膜.共聚物Pa,Pb的拉伸强度分别为80.0MPa,51.8MPa,断裂伸长率6.9%,4.6%,杨氏模量2.0GPa,1.8GPa.Three novel monomers were synthesized and confirmed by FT-IR and ^1H-NMR.N,N′-（4,4′-diphenylmethane）bistrimellitimide diacid chloride （DIDC-M） was synthesized by acidylated the 4,4′-bis（N-Trimellitimide）-diphenylmethane,which obtained from trimellitic anhydride with 4,4′-diaminodiphenylmethane （DDM）.2,2′,6,6′-Tetremethyl-4,4′-diphenoxydiphenylketone（o-Me2-DPOBP） and 2,2′,6,6′-tetremethyl-4,4′-diphenoxy-triphenyldiketone （o-Me2-DPOTPDK） were prepared by aromatic nucleophilic substitution reaction by 2,6-dimethylphenol with 4,4′-difluorodiphenylketone and 4,4′-difluorotriphenyldiketone respectively at the presence of sodium hydroxide,using DMSO as solvent at 200℃. Two novel poly（aryl ether ketone imide） copolymers containing bis（o-methyl） moieties were prepared by low temperature solution polycondensation of DIDC-M with o-Me2-DPOBP or o-Me2-DPOTPDK,in 1,2-dichloroethane （DCE） and at the presence of AlCl3 and N-methyl-2-pyrrolidone （NMP） as catalyst.The structure of copolymers （Pa,Pb） obtained were characterized by FTIR and ^1H-NMR.Differential scanning calorimetry（DSC） analysis indicated that the copolymers showed high glass transition temperature （Tg） 240℃ and 237℃,respectively.The single Tg＇s in the DSC cures suggested that no microphase separation occurred in the block copolymer.The copolymer also showed a high thermal stability with 5% weight-loss temperatures in excess of 464℃ in nitrogen,while 10% weight-loss temperature over 513℃,according to thermogravimetric analysis （TG）.Wide-angle X-ray diffraction （WAXD） studies revealed that Pa and Pb were amorphous,which agreed with the results of DSC,and as a result of introducing the rigid imido structure or non-planar methyl pendent to polymer backbone,the regularity of macromolecular chain destroyed.The soluble behaviours of the copolymers were tested qualitatively at room temperature in common organic solvents.It showed that the copolymers have good solubility in the

关 键 词：聚芳醚酮酰亚胺 共缩聚 双邻位甲基 结构和性能 

分 类 号：O633.22[理学—高分子化学]