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通过衣康酸与聚乙二醇的酯化反应,制备出了一种可用于合成聚羧酸系减水剂的大分子单体。用正交实验研究了反应条件对酯化反应的影响,确定了最佳的酯化反应条件为:n(衣康酸)∶n(聚乙二醇-1000)=1∶1.1,催化剂用量为聚乙二醇-1000质量的4%,反应温度100℃,反应时间6 h,带水剂用量为聚乙二醇-1000质量的30%,阻聚剂用量为衣康酸质量的2%,在该条件下单酯化率可达到98.3%。通过红外光谱、核磁共振氢谱对大分子单体的结构进行了表征。
Through the esterification of itaconic acid and polyethylene glycol, a kind of macromonomer that can be used for synthesizing polycarboxylate superplasticizer was prepared. The effects of reaction conditions on the esterification reaction were studied by orthogonal experiments. The optimal esterification conditions were as follows: n (itaconic acid): n (PEG - 1000) = 1: 1.1, the amount of catalyst 4% polyethylene glycol - 1000, the reaction temperature was 100 ℃, the reaction time was 6 h, the amount of water - borne agent was 30% of polyethylene glycol - 1000, the amount of inhibitor was 2% of itaconic acid, In this condition, the monoesterification rate can reach 98.3%. The structure of the macromer was characterized by IR and 1H NMR.