缓释型聚羧酸减水剂的低温制备工艺

Synthesis Process of Sustained-release Polycarboxylate Superplasticizer at Low-temperature

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关键词:

聚羧酸减水剂;异丁烯醇聚氧乙烯醚;低温合成;工艺;缓释;水泥净浆流动度

Key words:

Polycarboxylate superplasticizer; HPEG; Low-temperature synthesis; Process; Sutained-release; Cement paste fluidity

刊期:

2018年第1期

DOI:

文章编号:

1000-4637(2018)01-06-05

基金项目:

南京师范大学教育部留学回国人员科研启动基金(2006191XLH0132)资助项目

作者:

杜新康1,齐灵水2,莫祥银1,林 军1

单位:

1.南京师范大学化学与材料科学学院,210023;2.江西乐平领航新型材料有限公司,333000

摘要

摘   要:以异丁烯醇聚氧乙烯醚(HPEG)、丙烯酸(AA)为主要聚合单体,甲基丙烯酸羟乙酯(HEA)部分取代AA,巯基丙酸(MPA)为链转移剂,通过双氧水(H2O2)-抗坏血酸(Vc)引发,采用一步合成方法,在低温条件下制备了一种缓释型聚羧酸减水剂。研究分析了反应温度、酸醚比、HEA取代量、MPA用量、H2O2与Vc摩尔比、滴加时间等因素对合成减水剂产品性能的影响。利用正交试验,筛选出低温条件下较优的合成工艺:反应温度40℃,n(AA)∶n(HPEG)=4∶1,n(HEA)∶n(HPEG)=4.38:1,MPA用量(按HPEG单体质量分数计,下同)为0.65%,引发剂用量为1.17%,n(H2O2)∶n(Vc)=2.5∶1,滴加时间3h。当减水剂折固掺量为0.22%时,水泥初始净浆流动度达到280mm,0.5h后净浆流动度达到295mm,1h后净浆流动度达到302mm,相同掺量下与其他减水剂产品相比具有更好的分散性和分散保持性,且胶砂减水率达到37.5%。此外,通过傅里叶红外(FTIR)和热重分析(TGA)等手段对共聚物进行了表征。
Abstract: Sustained-release polycarboxylate superplasticizer was prepared in one step at low-temperature by using modified polyether macromer(HPEG), acylic acid(AA) as raw materials, AA partly replaced by hydroethyl methacrylate(HEA), mecraptopropionic acid(MPA) as the chain transfer agent, initiated by hydrogen peroxide(H2O2)-Vitamin C(Vc). The effect of the reaction temperature, the molar ratio of n(AA) to n(HPEG), the replace amount of HEA, the amount of MPA, the molar ratio of n(H2O2) to n(Vc), and the adding time, etc. on the properties of the production were studied. The orthogonal experimental results indicate that the optimum technology of synthesis are shown as follows: the reaction temperature is 40℃, n(AA)∶n(HPEG)=4∶1, n(HEA)∶n(AA)=4.38∶1, the MPA addition (based on the weight of HPEG, similarly hereinafter) is 0.65%, the weight of initiator is 1.17%, n(H2O2)∶n(Vc)=2.5∶1, and the adding time is 3h. The results show that the initial fluidity of cement paste can exceed 280mm, exceed 295mm after 0.5h and exceed 302mm after 1h when the dosage of polycarboxylate water reducer is 0.22% of cement mass. The polycarboxylate superplastic synthesized has higher dispersity and dispersion retention with the same addition amount than others, and the water reducing rate of mortar reaches 37.5%. In addition, the copolymer is characterized by Fourier transform infrared spectrometer(FTIR) and thermal gravimetric analysis(TGA).

结论

(1)以丙烯酸、丙烯酸羟乙酯和HPEG制备了一种高保坍缓释型聚羧酸减水剂,通过单因素实验和正交试验优化合成配比。最终得出制备的最佳条件为: n(AA)∶n(HPEG)∶n(HEA)=4.25∶1∶4.88;巯基丙酸的用量为大单体质量的0.65%;引发剂用量为1.17%;m(H2O2):m(Vc)=2.5:1;滴加温度为40℃;滴加时间为3h。
(2)使用丙烯酸羟乙酯适量取代丙烯酸,初始流动度达到280mm,1h后达305mm。且胶砂减水率达到了37.5%。表明该制备的减水剂具备了较好的分散性能和分散保持性能。
(3)工业上生产减水剂一般都需要很高的温度,本文合成的减水剂温度为40℃,下一步将继续研究将其反应温度降至室温。
 

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引用本文

杜新康,齐灵水,莫祥银,等.缓释型聚羧酸减水剂的低温制备工艺[J].混凝土与水泥制品,2018(1):6-10.

DU X K,QI L S,MO X Y,et al.Synthesis Process of Sustained-release Polycarboxylate Superplasticizer at Low-temperature[J].China Concrete and Cement Products,2018(1):6-10.


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