丙烯酰胺类聚电解质的合成及性能的研究
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摘要
本文在乙醇介质中制备出阳离子型、阴离子型、两性型的丙烯酰胺类聚电解质。主要研究内容及结果如下：
以丙烯酰胺(AM)、丙烯酰氧乙基三甲基氯化铵(DAC)为单体,以N-N'亚甲基双丙酰胺(BIS)为交联剂,偶氮二异丁腈(AIBN)为引发剂,在乙醇介质中通过沉淀聚合的方法制备阳离子聚丙烯酰胺(CPAM)。详细的研究反应时间、反应温度、单体物质量比、单体总浓度、引发剂浓度等因素对聚合物转化率的影响。研究得到的较佳合成条件是：单体总浓度为5%(wt),单体物质量比例AM:DAC=7:1,引发剂浓度为0.8%(wt),交联剂用量1mol%,反应温度为60℃,反应时间为8h。
以单体丙烯酰胺(AM)、甲基丙烯酸(MAA)为原料,在乙醇介质中通过沉淀聚合的方法制备阴离子聚丙烯酰胺(APAM)微球。系统的研究不同的反应条件对所制备的聚合物微球的粒径大小及粒径分布情况的影响；通过傅立叶红外光谱(IR)、透射电镜(TEM)、浊度法等测试手段分别对电解质的结构特征、微观形貌、pH敏感性等情况进行表征分析。成功的制备700nm-1100nm粒径范围内的单分散的微球,实现对不同粒径大小及粒径分布的单分散的微球制备的控制设计。
以AM、DAC、MAA为单体,在乙醇介质中制备出对pH、盐浓度双敏感的两性聚电解质微球。采用透射电子显微镜(TEM)和红外光谱(IR)方法对其形貌和结构进行表征。研究聚电解质微球在不同pH及不同离子强度盐溶液中粒径变化情况。研究结果表明：两性聚电解质微球具有良好的pH响应性,随着环境pH的变化,其粒径呈“U”字型变化。随着盐溶液中离子强度的增加,粒径呈现先下降,再略有上升的趋势；当盐溶液的pH值接近等电点时,对于单价态盐溶液,两性聚电解质微球表现出典型反聚电解质效应,而在多价态盐溶液的情况下,其粒径先增大再减小。
In this paper, cationic polyacrylamide, anionic polyacrylamide and gender polyacry-lamide microgel have been prepared by in ethanol. Main contents and results are as follows:
A cationic polyacrylamide(CPAM) was prepared by acrylamide(AM)、acryloylxyethyl trimethyl ammonium chloride(DAC)、N-N'methylene-bis-propionamide(BIS) and azobisiso.-butyronitrile(AIBN) as initiator in ethanol by precipitation polymerization. The influencing factors of the precipitation cationic polymerization were systematic studied, such as reaction time, reaction temperature, molar ratio, total monomer concentration, initiator concentration on the polymer conversion rate.The shape and conformation of CPAM were determined by Transmission Electron Micrograph and Infrared Spectroscopy, respectively.A better synthesis conditions was, total monomer concentration of 5%(wt), monomer molar ratio of AM:DAC=7:1, concentration of initiator 0.8%(wt), crosslinker lmol%, polymerization temperature 60℃, reaction time 8h.
In this paper, a series of poly(methacrylic acid/acrylamide) microspheres(APAM) based on acrylamide (AM), methacrylic acid (MAA) have been prepared by precipitation polymerization in ethanol.The reaction conditions, which affected size and size distribution were investigated. The structure of microspheres, morphology, pH-sensitive behavior have been characterized through Infrared Spectroscopy (FTIR), turbidimetric method and transmission electron microscopy (TEM), respectively. Monodisperse polymer polymer microspheres with different size and size distribution can be designed. Monodisperse polymer microspheres in the size range of 700nm-1100nm were prepared in reaction conditions
The polyampholyte microspheres with the pH-and salt concentration sensitive behaviors were prepared by AM、DAC and MAA in ethanol. The shape and conformation of microspheres were determined by Transmission Electron Micrograph and Infrared Spectroscopy, respectively. Meanwhile, the particle sizes change behavior of microspheres in distilled water with vairous pH values and the salt solutionswith different concentrations were investigated. The results indicated that the polyampholyte microspheres possessed a good pH-responsive behavior and a U-type of pH-volume transition. With the increasing of concentration of the salt solutions, the first decreased and then having a slight upward trend. At the isoelectric point (pI=4), dispersion exhibited typical antipolyelectrolyte effect in univalent saltl solution. However, in multivalent salt solution, the particle sizes first increased and then decreased.
以丙烯酰胺(AM)、丙烯酰氧乙基三甲基氯化铵(DAC)为单体,以N-N'亚甲基双丙酰胺(BIS)为交联剂,偶氮二异丁腈(AIBN)为引发剂,在乙醇介质中通过沉淀聚合的方法制备阳离子聚丙烯酰胺(CPAM)。详细的研究反应时间、反应温度、单体物质量比、单体总浓度、引发剂浓度等因素对聚合物转化率的影响。研究得到的较佳合成条件是：单体总浓度为5%(wt),单体物质量比例AM:DAC=7:1,引发剂浓度为0.8%(wt),交联剂用量1mol%,反应温度为60℃,反应时间为8h。
以单体丙烯酰胺(AM)、甲基丙烯酸(MAA)为原料,在乙醇介质中通过沉淀聚合的方法制备阴离子聚丙烯酰胺(APAM)微球。系统的研究不同的反应条件对所制备的聚合物微球的粒径大小及粒径分布情况的影响；通过傅立叶红外光谱(IR)、透射电镜(TEM)、浊度法等测试手段分别对电解质的结构特征、微观形貌、pH敏感性等情况进行表征分析。成功的制备700nm-1100nm粒径范围内的单分散的微球,实现对不同粒径大小及粒径分布的单分散的微球制备的控制设计。
以AM、DAC、MAA为单体,在乙醇介质中制备出对pH、盐浓度双敏感的两性聚电解质微球。采用透射电子显微镜(TEM)和红外光谱(IR)方法对其形貌和结构进行表征。研究聚电解质微球在不同pH及不同离子强度盐溶液中粒径变化情况。研究结果表明：两性聚电解质微球具有良好的pH响应性,随着环境pH的变化,其粒径呈“U”字型变化。随着盐溶液中离子强度的增加,粒径呈现先下降,再略有上升的趋势；当盐溶液的pH值接近等电点时,对于单价态盐溶液,两性聚电解质微球表现出典型反聚电解质效应,而在多价态盐溶液的情况下,其粒径先增大再减小。
In this paper, cationic polyacrylamide, anionic polyacrylamide and gender polyacry-lamide microgel have been prepared by in ethanol. Main contents and results are as follows:
A cationic polyacrylamide(CPAM) was prepared by acrylamide(AM)、acryloylxyethyl trimethyl ammonium chloride(DAC)、N-N'methylene-bis-propionamide(BIS) and azobisiso.-butyronitrile(AIBN) as initiator in ethanol by precipitation polymerization. The influencing factors of the precipitation cationic polymerization were systematic studied, such as reaction time, reaction temperature, molar ratio, total monomer concentration, initiator concentration on the polymer conversion rate.The shape and conformation of CPAM were determined by Transmission Electron Micrograph and Infrared Spectroscopy, respectively.A better synthesis conditions was, total monomer concentration of 5%(wt), monomer molar ratio of AM:DAC=7:1, concentration of initiator 0.8%(wt), crosslinker lmol%, polymerization temperature 60℃, reaction time 8h.
In this paper, a series of poly(methacrylic acid/acrylamide) microspheres(APAM) based on acrylamide (AM), methacrylic acid (MAA) have been prepared by precipitation polymerization in ethanol.The reaction conditions, which affected size and size distribution were investigated. The structure of microspheres, morphology, pH-sensitive behavior have been characterized through Infrared Spectroscopy (FTIR), turbidimetric method and transmission electron microscopy (TEM), respectively. Monodisperse polymer polymer microspheres with different size and size distribution can be designed. Monodisperse polymer microspheres in the size range of 700nm-1100nm were prepared in reaction conditions
The polyampholyte microspheres with the pH-and salt concentration sensitive behaviors were prepared by AM、DAC and MAA in ethanol. The shape and conformation of microspheres were determined by Transmission Electron Micrograph and Infrared Spectroscopy, respectively. Meanwhile, the particle sizes change behavior of microspheres in distilled water with vairous pH values and the salt solutionswith different concentrations were investigated. The results indicated that the polyampholyte microspheres possessed a good pH-responsive behavior and a U-type of pH-volume transition. With the increasing of concentration of the salt solutions, the first decreased and then having a slight upward trend. At the isoelectric point (pI=4), dispersion exhibited typical antipolyelectrolyte effect in univalent saltl solution. However, in multivalent salt solution, the particle sizes first increased and then decreased.
引文
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[2]方道斌等.聚丙烯酰胺[M].北京：化学工业出版社,2006：5-23.
[3]周华,胡瑞,陈存华.阴离子聚丙烯酞胺絮凝剂的制备及应用[J].精细石油化工,2006,3(2)：4-7.
[4]王立君,张丽华,段秀平.丙烯酸-丙烯酰胺共聚物的制备及其重金属离子敏感性研究[J].应用化工,2007,11(11)：1114-1117.
[5]李云华,刘书钗.阴离子聚丙烯酰胺的合成研究[J].黑龙江造纸,2005,1(1)：29-31.
[6]张黎明.具有反聚电解质溶液行为的两性聚合物高[J].分子通报,1998,12(4)：80-85.
[7]任静,哈鸿飞.聚两性电解质及其水凝胶的研究进展[J].高分子通报,2000,9(3)：8-15.
[8]Dimonie M.V, Boghina C..Inverse suspension polymerization of acrylamide[J]. Eur.Poly,1982,18 (7):639-645.
[9]项盛.盐水介质中两性聚电解质的分散聚合[D].长春：中国科学院应用化学研究所,2007.
[10]罗娅君,张新申,王照丽等.阳离子型高分子絮凝剂P(DMC-AM)的合成[J].四川大学学报,2003,35(3)：18-20.
[11]赵华章,岳钦艳,高宝玉等.阳离子型高分子絮凝剂PDMDAAC与P(DMDAAC-AM)的合成及分析[J].精细化工,2001,18(11)：645-649.
[12]郭东荣,高锦屏,赵福麟.季铵阳离子聚合物的制备与应用[J].石油钻探技术,1997,25(4)：19-24.
[13]杨银,邵丽,邓阳全等.智能水凝胶的制备及其在生物医学中的应用[J].化工新型材料,2010,1(1)：11-15.
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