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(VC)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。
Synthesis and Properties of Water-Reducing and Slump-Protecting Polycarboxylate Superplasticizer
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 H2 O2/L-vitamin C(Vc)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.