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1. 中南大学化学化工学院,长沙,410083
2. 大连理工大学精细化工国家重点实验室 大连 116012>
纸质出版日期:2012-8-20,
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李斌, 伍绍飞, 刘俊灵, 熊绍辉, 谭海军, 喻桂朋, 潘春跃, 蹇锡高. 含1,3,5-三嗪芳香二酸及其可溶性聚芳酰胺的合成[J]. 高分子学报, 2012,(8):870-875.
Bin Li, Shao-fei Wu, Jun-ling Liu, Shao-hui Xiong, Hai-jun Tan, Gui-peng Yu, Chun-yue Pan, Xi-gao Jian. SYNTHESIS OF A 1,3,5-TRIAZINE-CONTAINING AROMATIC DIACID MONOMER AND ITS SOLUBLE AROMATIC POLYAMIDES[J]. Acta Polymerica Sinica, 2012,(8):870-875.
李斌, 伍绍飞, 刘俊灵, 熊绍辉, 谭海军, 喻桂朋, 潘春跃, 蹇锡高. 含1,3,5-三嗪芳香二酸及其可溶性聚芳酰胺的合成[J]. 高分子学报, 2012,(8):870-875. DOI: 10.3724/SP.J.1105.2012.11379.
Bin Li, Shao-fei Wu, Jun-ling Liu, Shao-hui Xiong, Hai-jun Tan, Gui-peng Yu, Chun-yue Pan, Xi-gao Jian. SYNTHESIS OF A 1,3,5-TRIAZINE-CONTAINING AROMATIC DIACID MONOMER AND ITS SOLUBLE AROMATIC POLYAMIDES[J]. Acta Polymerica Sinica, 2012,(8):870-875. DOI: 10.3724/SP.J.1105.2012.11379.
以2
4-二氯-6-苯基-1
3
5-三嗪为原料
通过傅克和氧化反应制备了一种新型芳香二酸2
4-二(4-甲酸基苯基)-6-芳基-1
3
5-三嗪(PTDA)
并采用1H-NMR
FTIR
MS和元素分析等对其结构进行了表征.利用正交试验
重点考察了氧化反应条件对产率的影响
结果表明反应温度为25℃、反应时间为8 h、HAc与H2SO4摩尔比为10:1、CrO3与PTDA配比为4:1时
氧化产率最高
达81.3%.以PTDA和间苯二胺(BD)为原料
制备了新型含1
3
5-三嗪聚芳酰胺PPA
其特性黏数为0.49 dL/g.该聚酰胺表现出较好的溶解性能以及优异的热稳定性和机械性能
室温下可溶于 N-甲基-2-吡咯烷酮、 N
N-二甲基乙酰胺等溶剂中
由其溶液可制得透明薄膜;玻璃化转变温度达315℃
氮气中起始分解温度T5%为493℃
700℃下残炭率高达59%;薄膜的拉伸强度为82 MPa
断裂伸长率在8.2%
起始模量为2.3 GPa.
The synthesis
characterization and properties of phenyl-1
3
5-triazine functional monomers and aromatic polyamides are described.A novel aromatic diacid
namely 4
4'-(6-phenyl-1
3
5-triazine-2
4-diyl)dibenzoic acid (PTDA) was successfully prepared by a two-step reaction including Friedel-Crafts reaction and oxidation starting from 2
4-dichloro-6-phenyl-1
3
5-triazine (DCPT).Its chemical structure was characterized by 1H-NMR
FTIR
MS and Elemental analysis.Optimal conditions of the oxidation were chosen on the basis of the yield by using orthogonal experiments with respect to oxidizer content
solvent ratio
heating temperature and reaction time.The reaction
which was achieved at the temperature of 25℃ for 8 h with a CH3COOH/H2SO4 ratio of 10 and a CrO3/PTDA ratio of 4
gave the targeted product with a highest yield of 81.3%.A new aromatic polyamide (PPA) with an inherent viscosity of 0.49 dL/g was obtained by direct phosphorylation polycondensation of PTDA with benzene-1
4-diamine.The obtained polymer possesses good solubility.It is readily soluble in N-methylpyrrolidone
N
N-dimethyl acetamide (DMAc) and sulfolane
and can be easily cast into transparent thin films.Such polymer exhibits glass transition temperature (Tg) up to 315℃
and possesses excellent thermal and thermo-oxidative stability without significant weight loss up to temperatures of approximately 500℃.Its decomposition temperature for 5% mass-loss is in excess of 493℃ in nitrogen and it retains 90% weight at round 520℃.The obtained films exhibits attractable mechanical properties with tensile strengths of 82 MPa
elongation at break of 8.2% and initial moduli of 2.3 GPa.
135-三嗪聚芳酰胺高性能聚合物
135-Triazine
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