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纸质出版日期:2002-10-20,
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廖功雄, 蹇锡高, 何伟, 靳奇峰, 李荃, 吴立豪. 含硫醚和二氮杂萘酮结构聚芳醚酮的合成与性能[J]. 高分子学报, 2002,(5):641-646.
LIAO Gongxiong, JIAN Xigao, HE Wei, JIN Qifeng, LI Quan, WU Lihao. SYNTHESIS AND PROPERTIES OF POLYETHERKETONE CONTAINING SULFIDE AND PHTHALAZINONE MOIETIES[J]. Acta Polymerica Sinica, 2002,(5):641-646.
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、1H-NMR和13C-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.
High molecular weight polyetherketones based on 4-(4-hydroxyphenyl)-l-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.13C-NMR spectra were used to indentify the structure of copolyetherketones.According to 13C-NMR spectra
it was found that the structural repeat units were randomly distributed in the molecular chain of the copolyetherketones. The Glass transition temperatures (Tg) 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 Tg in the range of 137℃ to 263℃ and the Tgs 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.
聚芳醚酮44′硫代二酚4(4羟基苯基)23二氮杂萘1酮高性能聚合物
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