| 摘要: |
| 利用微波技术清洁、高效、靶向等特点，分别采用微波合成法和常规油浴法，以聚乙二醇单甲醚（MPEG），甲基丙烯酸（MAA）等原材料制备甲氧基聚乙二醇甲基丙烯酸酯(MPEGMAA)，并进一步聚合成酯类聚羧酸减水剂进行性能对比.分别研究了酸醇比、催化剂用量、阻聚剂用量、反应时间、酯化温度以及微波功率对酯化大单体酯化率的影响规律，并基于微波合成法得出最优配比与工艺方案：n(MAA)∶n(MPEG)=5.0∶1.0，催化剂用量为MPEG质量的4.5%，阻聚剂用量为MAA质量的0.28%，酯化温度为120℃，酯化时间为100min，微波功率为1000W.微波合成法的酯化率为93.47%，是常规油浴法的1.14倍，反应速率为常规油浴法的4.8倍.通过水泥净浆流动度试验、流变学研究以及红外光谱分析得出，微波合成法更有利于酯化大单体酯键的形成，且合成的酯类聚羧酸减水剂分散性及分散保持性更优. |
| 关键词: 微波合成 酯类聚羧酸减水剂 酯化率 分散性 流变性能 |
| DOI：10.3969/j.issn.1007 9629.2017.03.005 |
| 分类号: |
| 基金项目:国家自然科学基金面上项目(51572293) |
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| Process and Performance of Ester Based Polycarboxylate Superplasticizer by Microwave Assisted Synthesis |
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WANG Dongmin1, FANG Kuizhen1, ZHANG Liran2, WANG Qibao1, WANG Fang1
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1.School of Chemical and Environmental Engineering, China University of Mining and Technology Beijing, Beijing 100083, China;2.Department of Civil Engineering, Tsinghua University, Beijing 100084, China
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| Abstract: |
| The use of microwave technology is clean, efficient, targeted and so on. Microwave assisted synthesis and conventional oil bath were used to prepare methoxy polyethylene glycol methacrylate(MPEGMAA) by esterification of methacrylic acid(MAA) and methoxy polyethylene glycol(MPEG), and further polymerize into esters of polycarboxylate superplasticizer for performance analysis. The effects of acid and alcohol ratio, the amount of catalyst and the polymerization inhibitor, reaction time, esterification temperature and microwave power on the esterification ratio were studied by single factor method，and it was found that the optimal ratios and process solutions based on microwave assisted synthesis was n(MAA)∶n(MPEG)=5.0∶1.0. The amount of catalyst was 45% by the mass of MPEG. Amount of the polymerization inhibitor was 0.28% by the mass of MAA. Esterification temperature was 120℃. Reaction time was 100min and the microwave power was 1000W. Esterification ratio of the method was 9347%, which was 1.14 times that of conventional oil bath oil bath method. The reaction rate was 4.8 times that of the conventional oil bath method. Through the cement paste test, infrared spectrum analysis and rheological properties study, the microwave heating method is more conducive to the formation of esterification monomer ester bond. Dispersion and dispersion maintaining performance of synthetic esters of polycarboxylate superplasticizer are better. |
| Key words: microwave assisted synthesis esters of polycarboxylate superplasticizer esterification ratio dispersion rheological property |
