摘要
由9,9-二(4-羟基苯基)呫吨和对氯硝基苯反应制得二硝基化合物,继而用水合肼/钯碳将其还原得到二胺——9,9-二(4-氨基苯氧基苯基)呫吨(BAPX)。采用Yamazaki聚合体系,将BAPX与1,4(或2,6)-萘二酸进行缩聚合成了两种新型含呫吨和萘环结构的聚酰胺,二者均为无定型结构,其特性黏度、玻璃化转变温度(Tg)分别为0.98dL/g和1.0dL/g、295℃和302℃。在氮气和空气气氛中,10%的热失重温度(Td10)均在505℃以上,在氮气中,800℃时的残炭率大于65%;在常温下易溶于N-甲基-2-吡咯烷酮(NMP)、N,N-二甲基乙酰胺(DMAc)和间甲酚等极性溶剂中,可通过溶液浇铸成透明、韧性的薄膜,膜的拉伸强度、断裂伸长率和杨氏膜量依次分别为105MPa和110MPa、13.1%和13.3%、2.88GPa和3.05GPa。
Reaction of 9,9-bis（4-hydroxyphenyl）xanthene with 4-nitrchlorobenzene afforded the corresponding dinitro compound,followed by reduction in the presence of hydrazine hydrate and Pd/C catalyst to give a novel diamine monomer,9,9-bis（4-aminophenoxyphenyl）xanthene （BAPX）. Two novel aromatic polyamides containing xanthene and naphthylene moieties with the inherent viscosities （1.0 dL/g～0.98 dL/g） were prepared from BAPX with 1,4-naphalenedicarboxylic acid and 2,6-naphalenedicarboxylic acid using Yamazaki method via direct polycondensation,respectively. The new polyamides were amorphous and readily soluble in polar solvents such as N,N-dimethylacetamide （DMAc）,N-methyl-2-pyrrolidinone （NMP） and m-cresol. These polymers show relatively high glass transition temperatures of 295 ℃ and 302 ℃,10% weight loss temperatures is above 500 ℃ both in nitrogen and air,and char yield at 800 ℃ in nitrogen is higher than 65%. Transparent and flexible films of the two polymers cast from DMAc solutions exhibit tensile strengths,elongations at break and initial moduli of 105 MPa and 110 MPa,13.1 and 13.3%,2.88 GPa and 3.05 GPa,respectively.
出处
《高分子材料科学与工程》
EI
CAS
CSCD
北大核心
2010年第12期31-34,38,共5页
Polymer Materials Science & Engineering
基金
国家自然科学基金资助项目(20664001)
江西省教育厅科研基金(GJJ08166
GJJ09138)
