沉淀分级法制备GPC用聚甲基丙烯酸甲酯标样
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摘要
以甲基丙烯酸甲酯为原料,采用自由基聚合反应制备得到具有不同平均分子量的标题化合物,用甲苯-石油醚对其进行沉淀分级,得到6个窄分子量分布的标题化合物,用GPC对其进行定值后,其平均分子量范围在3.1×103~4.3×104之间,分散系数<1.5,且GPC峰形对称。将上述自制标样用粘度法测定其粘均分子量,并与GPC定值结果比较,其误差<10%。将自制标样与英国Polymer Lab公司提供的单分散标题化合物标样进行比较,两者测定未知聚甲基丙烯酸甲酯样品的分子量具有很好的一致性。
Six PMMA samples with narrow molecular weight distribution were synthesized with different average molecular mass via free radical polymerization by using methyl methacrylate as raw materials,using toluene-petroleum ether to precipitation grading.The GPC results showed that the average molecular weights ranged from 3.1 × 103to 4.3 × 104,dispersion coefficients were less than 1.5,gel permeation chromatography(GPC) peak shapes were symmetrical.Viscosity average molecular weight of PMMA measured by viscosity measuring method compared to the GPC result,the error was less than 10%.Compare the homemade sample with monodisperse PMMA sample,which is provided from the English company Polymer Lab,it turns out that the determination of molecular weight of the unknown polymethyl methacrylate sample have good consistency.
Six PMMA samples with narrow molecular weight distribution were synthesized with different average molecular mass via free radical polymerization by using methyl methacrylate as raw materials,using toluene-petroleum ether to precipitation grading.The GPC results showed that the average molecular weights ranged from 3.1 × 103to 4.3 × 104,dispersion coefficients were less than 1.5,gel permeation chromatography(GPC) peak shapes were symmetrical.Viscosity average molecular weight of PMMA measured by viscosity measuring method compared to the GPC result,the error was less than 10%.Compare the homemade sample with monodisperse PMMA sample,which is provided from the English company Polymer Lab,it turns out that the determination of molecular weight of the unknown polymethyl methacrylate sample have good consistency.
引文
[1]徐丹.凝胶渗透色谱用聚甲基丙烯酸标样的制备方法[D].武汉理工大学,2012.
[2]FALLAIS I,PANTOUSTIER N,DEVAUX J,et al.Anionic synthesis of cyclic anhydride end-capped poly(methyl methacrylate)[J].Polymer,2000,41(14):5 535-5 539.
[3]CHEN Gao-jian,ZHU Xin-lin,CHENG Zheng-ping,et al.Controlled/living radical polymerization of methyl methacrylate using AIBN as the initiator under microwave irradiation[J].Radiat.Phys.Chem.,2004,69(2):129-135.
[4]YE Qiang,GE Xue-wu,ZHANG Zhi-cheng.Formation of monodisperse PMMA particles by radiation-induced dispersion polymerizationⅠ.synthesis and polymerization kinetics[J].Radiat.Phys.Chem.,2003,66(1):11-16.
[5]曹俊奎,沈家聪.窄分布聚甲基丙烯酸甲酯的合成与表征[J].高分子学报,1990,1(5):613-617.
[6]郭丽萍,陈莉,杜小弟,等.凝胶渗透色谱用聚丙烯酸标样的制备[J].应用化学,2011,28(4):443-447.
[7]WIEDERHORN N M,BROWN A R.Viscosity-molecular weight relation for polymethacrylic acid in methanol[J].J.Poly.Sci.,1952,8(6):651-656.
[2]FALLAIS I,PANTOUSTIER N,DEVAUX J,et al.Anionic synthesis of cyclic anhydride end-capped poly(methyl methacrylate)[J].Polymer,2000,41(14):5 535-5 539.
[3]CHEN Gao-jian,ZHU Xin-lin,CHENG Zheng-ping,et al.Controlled/living radical polymerization of methyl methacrylate using AIBN as the initiator under microwave irradiation[J].Radiat.Phys.Chem.,2004,69(2):129-135.
[4]YE Qiang,GE Xue-wu,ZHANG Zhi-cheng.Formation of monodisperse PMMA particles by radiation-induced dispersion polymerizationⅠ.synthesis and polymerization kinetics[J].Radiat.Phys.Chem.,2003,66(1):11-16.
[5]曹俊奎,沈家聪.窄分布聚甲基丙烯酸甲酯的合成与表征[J].高分子学报,1990,1(5):613-617.
[6]郭丽萍,陈莉,杜小弟,等.凝胶渗透色谱用聚丙烯酸标样的制备[J].应用化学,2011,28(4):443-447.
[7]WIEDERHORN N M,BROWN A R.Viscosity-molecular weight relation for polymethacrylic acid in methanol[J].J.Poly.Sci.,1952,8(6):651-656.