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粘度法测定双酚A型聚芳酯相对分子质量的研究 被引量:2

The Determination of Molecular Weight of Bisphenol-A Polyarylester by Viscosimetry
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摘要 采用粘度法测定双酚A型聚芳酯(PAR-A)在二氯甲烷(CH2Cl2)溶液中25℃下的特性黏数([η]),通过凝胶色谱(GPC)法得到了PAR-A的Mark-Houwink方程参数.根据方程lg[η]=lgK+αlgM,以lg[η]分别对lgMn、lgMw和lgMη作图,由直线的斜率和截距得到的Mark-Houwink方程参数K1=1.630×10 4、α1=0.763 9;K2=4.245×10 6、α2=1.052 5和K3=8.634×10 7、α3=1.177 6求得相应的数均相对分子质量(Mn)、重均相对分子质量(Mw)和粘均相对分子质量(Mη)以及相对分子质量分散指数.根据得到的GPC谱图和相应的Mn、Mw和Mη,可知PAR-A的淋出时间随着[η]的增加而缩短,而相应的相对分子质量随着[η]的增加而增加.研究表明,采用相转移催化界面缩聚法制得PAR-A的相对分子质量分布较窄,双对数作图法比较可靠,其相关系数大于0.98. Determined the intrinsic viscosity([η]) of bisphenol-A polyarylester (PAR-A) by the viscometric method, in pure dichloromethane (CH2Cl2) solution at room temperature (25℃). Then Mark-Houwink equation parameters were set by the gel permeation chromatography (GPC). Based on the Mark-Houwink equation lg [η]= lgK + algA/, the lg [η] for the vertical axis, lgM(lgMn, lgMw and lgMn) as abscissa, made a series of analysis charts, respectively. The Mark-Houwink equation parameters: were obtained from the slope and intercept of the straight line: K1=1.630×10-4, a1=0.763 9; K2=4.245×10-6, a2=1.052 5 and K3=8.634×10-7, a3=1.177 6. The corresponding data can be obtained from these kinds of equation, such as the corresponding number-average molecular weight (M,), weight-average molecular weight (Mw) and viscosity-average molecular mass (M,) and molecular weight polydispersity index. From the resulting GPC spectra and the corresponding Mn, Mw and Mn, PAR-A leaching out time became shorter with the [ η] increasing while the corresponding molecular weight increased with the [η] increasing was found. The results showed that the molecular weight of PAR, which was synthesized by interracial polycondensation using phase transfer catalysis method, is narrow distribution. So the double logarithmic mapping is more reliable and the correlation coefficient is no less than 0.985.
出处 《江西师范大学学报(自然科学版)》 CAS 北大核心 2011年第6期551-555,共5页 Journal of Jiangxi Normal University(Natural Science Edition)
基金 国家自然科学基金(51003044) "十一五"军品配套课题(JPPT-115-643)资助项目
关键词 双酚A型聚芳酯 粘度法 凝胶色谱法 Mark-Houwink方程参数 bisphenol-A polyarylester viscometric method gel permeation chromatography Mark-Houwink equation
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