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机构地区:[1]广西水电科学研究院,广西南宁530021 [2]南京理工大学材料系,江苏南京210094 [3]烟台大学土木工程学院,山东烟台264005
出 处:《烟台大学学报(自然科学与工程版)》2010年第2期148-153,共6页Journal of Yantai University(Natural Science and Engineering Edition)
基 金:广西电网攻关资助项目(TM08H76)
摘 要:以400,600,2000 3种分子质量的甲氧基聚乙二醇(MPEG)和过量甲基丙烯酸(MAA)为主要原料,通过酯化反应制备了聚羧酸盐减水剂所用大单体甲氧基聚乙二醇甲基丙烯酸酯(MPEGMA).研究了酯化反应时间、酸醇比、酯化温度、催化剂、阻聚剂对酯化反应的影响;结果表明:酯化反应时间以7~8 h较为合理,MAA与MPEG物质的量之比对酯化率的影响最为显著,其次是反应温度,催化剂用量对低分子量MPEG的酯化反应影响较小,但随着MPEG分子量增大催化剂的影响变得显著.MPEG400的最佳酯化条件为:nMAA∶nMPEG为2∶1,反应温度100℃,催化剂为总质量的2%,阻聚剂为甲基丙烯酸质量的0.5%;MPEG600的最佳酯化条件为:nMAA∶nMPEG为2.5∶1,反应温度110℃,催化剂用量为总质量的4%,阻聚剂为甲基丙烯酸质量的0.5%;MPEG2000的最佳酯化条件为:nMAA∶nMPEG为5∶1,反应温度110℃,催化剂为总质量的6%,阻聚剂为甲基丙烯酸质量的0.5%.红外图谱表明3种分子量的MPEG与MAA反应后均生成了酯化大单体.Methoxy polyethylene glycol methacrylate( MPEGMA), the macromer used for polycarboxylate su- perplasticizer, is prepared by esterification of methacrylic acid (MAA) and methoxy polyethylene glycol (MPEG) with average molecular weight 400,600 and 2000. The effects of reaction time, ratio of nMAA to nMPEC, reaction temperature as well as the amounts of catalyst and inhibitor on esterification are investigated. The results show that the rational time of esterification is about 7 - 8 hours. The most significant factor on esterification is the ratio of nMAA to nMPEC, and the secondary one is reaction temperature. The amounts of catalyst has the minimal influence on the esterification of low-molecular-weight MPEG and increasing influence on the esetirification of higher-molecular-weight MPEG. The optimal conditions for MPEG400 esterification are as follows: the ratio of nMAs to nMPEC is 2.0, the reaction temperature is 100 ℃, the amount of catalyst is 2% of the total mass, the amount of inhibitor is 0.5 % of the mass of MAA. The optimal conditions for MPEG600 esterification are as follows : the ratio of nMAa to nMPEC is 2.5, the temperature is 110 ℃, the amount of catalyst is 4% of the total mass, the amount of inhibitor is 0.5% of the mass of MAA. The optimal conditions, for MPEG2000 esterification are as follows: the ratio of nMAA to nMPEC is 5. 0, the temperature is 110℃, the amount of catalyst is 6% of the total mass and the amount of inhibitor is 0.5% of the mass of MAA. IR spectra demonstrate the existence of MPEGMA after esterification of MPEG400, MPEG600 and MPEG2000.
关 键 词:聚羧酸盐减水剂 酯化 甲氧基聚乙二醇 甲氧基聚乙二醇甲基丙烯酸酯
分 类 号:TU53[建筑科学—建筑技术科学]
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