减水保坍型聚羧酸减水剂的合成及性能研究

摘要/Abstract

摘要： 以4-羟丁基乙烯基聚氧乙烯醚(VPEG)大单体、丙烯酸(AA)为主要原料,引入保坍单体丙烯酸羟乙酯(HEA),以巯基丙酸(MPA)为链转移剂,在H₂O₂/L-抗坏血酸(V_C)氧化还原引发体系下,通过自由基聚合制备出减水保坍型聚羧酸减水剂(V-HEA)。通过红外光谱、凝胶色谱测试对合成的V-HEA进行分子结构表征,并与市售保坍型聚羧酸减水剂(HPWR-S)进行水化热与混凝土性能对比分析。结果表明,V-HEA的最佳合成工艺参数为酸醚比4.4,酯醚比2.5,引发剂、硫酸亚铁和链转移剂掺量分别占大单体质量的0.76%、0.10%和0.74%。掺入硫酸亚铁可提高单体的转化率,且V-HEA的数均分子量为17 650,重均分子量为42 713,单体转化率高达95.03%。掺入V-HEA时混凝土的水化峰值温度较掺入HPWR-S时延迟4 h 24 min,且第二水化速率峰出现时间延迟约4 h,更加延缓水泥的水化。掺入V-HEA的混凝土2 h坍落度仅损失5.8%,且混凝土强度与掺入HPWR-S产品相当,V-HEA具有较好的应用前景。

关键词: 聚羧酸减水剂, VPEG大单体, 自由基聚合, 保坍型, 分子结构表征, 水化热分析

Abstract: The water-reducing and slump-protecting polycarboxylate superplasticizer (V-HEA) was prepared by free-radical polymerization with 4-hydroxybutyl vinyl polyoxyethylene ether (VPEG) macromonomer and acrylic acid (AA) as the main raw materials by adding the slump-preserving monomer hydroxyethyl acrylate (HEA), and mercapto-propionic acid (MPA) as chain transferr agent under the H₂O₂/L-vitamin C (V_C) oxidation-reductioninitiator system. The synthesized V-HEA was characterized by infrared spectroscopy, gel chromatography testing, and it was subjected to hydration heat analysis and concrete performance comparison analysis with commercially available slump-preserving polycarboxylate superplasticizer (HPWR-S). The results show that the optimal synthesis process parameters of V-HEA are acid-ether ratio of 4.4, ester-ether ratio of 2.5, and the dosage of initiator, ferrous sulfate and chain transfer agent accounted for 0.76%, 0.10% and 0.74% of the mass of the macromonomer, respectively. The incorporation of ferrous sulfate could improve the conversion rate of monomers, and the number average molecular weight of V-HEA is 17 650, the weight average molecular weight is 42 713, and the conversion rate of monomers is as high as 95.03%. The peak temperature of hydration reaches by the incorporation of V-HEA is delayed by 4 h 24 min compared with HPWR-S, and the occurrence time of the second hydration rate peak is delayed by about 4 h, which further delays the hydration of cement. In comparison test of concrete performance, the 2 h slump only decreases by 5.8% with the addition of V-HEA, and the strength of concrete is comparable to that of HPWR-S products, so V-HEA has good application prospects.

Key words: polycarboxylate superplasticizer, VPEG macromonomer, radical polymerization, slump-preserving type, molecular structure characterization, hydration heat analysis

中图分类号:

TU528.042.2

董建统, 刘志勇, 胡忠帅, 朱丹丹, 丁怡, 张伟强, 来福琨. 减水保坍型聚羧酸减水剂的合成及性能研究[J]. 硅酸盐通报, 2024, 43(1): 52-60.

DONG Jiantong, LIU Zhiyong, HU Zhongshuai, ZHU Dandan, DING Yi, ZHANG Weiqiang, LAI Fukun. Synthesis and Properties of Water-Reducing and Slump-Protecting Polycarboxylate Superplasticizer[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2024, 43(1): 52-60.

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