含β 环糊精侧基聚羧酸系减水剂的制备与性能
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国家自然科学基金资助项目(21076121)


Preparation and Properties of Polycarboxylate Superplasticizer with β cyclodextrin(β CD) as Side Chain
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    摘要:

    以马来酸酐(MAH)和β 环糊精(β CD)进行酯化反应制备了马来酸 β 环糊精(MAH β CD),讨论了n(MAH)︰n(β CD),反应时间及反应温度对MAH β CD产率的影响.结果表明,当n(MAH)︰n(β CD)为10︰1,反应温度为90 ℃,反应时间为8 h时,MAH β CD产率为75%(质量分数).以丙烯酸(AA)、烯丙基聚乙二醇(APEG)、甲基丙烯磺酸钠(MAS)和MAH β CD为原料,通过自由基共聚反应制备了一种含β CD侧基聚羧酸系减水剂(RPC).基于水泥净浆流动度测试结果,确定共聚反应单体摩尔比n(AA)︰n(APEG)︰n(MAS)︰n(MAH β CD)为5.000︰1.000︰0.500︰0.075,引发剂过硫酸铵(APS)用量为单体总量的5%(质量分数),反应温度为80 ℃,反应时间为5 h.用FTIR和1H NMR对MAH β CD和RPC的化学结构进行了表征.对 RPC在混凝土中的应用性能进行了探讨,结果表明:RPC缓凝时间为5 h,减水率大于32%(质量分数);掺入RPC后,混凝土早期抗压强度增长较快,新拌混凝土未出现泌水、离析现象.

    Abstract:

    β cyclodextrin grafted maleic anhydride(MAH β CD) was synthesized by esterification of maleic anhydride(MAH) and β cyclodextrin(β CD). The effect of n(MAH)︰n(β CD), reaction time and reaction temperature on the yield of MAH β CD was investigated. The results show that the yield of MAH β CD is 75%(by mass) when the n(MAH)︰n(β CD) is 10︰1 and reaction is carried out at 90 ℃ for 8 h. A new set retarding type polycarboxylate superplasticizer(RPC) was prepared by free radical solution copolymerization of acrylic acid(AA), allyl polyethylene glycol(APEG), sodium methylacrylsulfonate(MAS) and MAH β CD. Based on the test result of fluidity of cement paste, the synthesis process of RPC is carried out at the n(AA)︰n(APEG)︰n(MAS)︰n(MAH β CD)=5.000︰1.000︰0.500︰0.075 in the presence of 5%(mass fraction of monomers) APS at 80 ℃ for 5 h. The chemical structure of MAH β CD and RPC was characterized by FTIR and 1H NMR. The application result in concrete for RPC indicates that the set retarding time is 5 h longer and water reducing rate is as higher as 32%(by mass). The concrete with RPC does not show any segregation and bleeding, the early compressive strength is improved significantly.

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吕生华,高瑞军,段建平,李第,曹强.含β 环糊精侧基聚羧酸系减水剂的制备与性能[J].建筑材料学报,2012,(3):410-415

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  • 收稿日期:2011-01-20
  • 最后修改日期:2011-04-08
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  • 在线发布日期: 2012-06-27
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