作者：李格丽, 林倩, 方云辉

作者单位：科之杰新材料集团有限公司, 福建 厦门 361100

关键词：聚羧酸减水剂;大单体;超滤;核磁共振氢谱

摘要：

采用超滤和核磁技术,建立分析未知聚羧酸减水剂中大单体的方法。结果表明,未知聚羧酸减水剂样品依次经过30,10,3 kD(道而顿)超滤膜后,大分子量的组分被逐级滤去;超滤滤液再经过500D的透析袋预处理去除杂质,得到相对较纯的大单体。应用核磁共振氢谱技术对常见的已知大单体进行鉴别分析,进而解析出未知聚羧酸样品使用的大单体为异戊烯醇聚乙二醇醚(TPEG)。该法为聚羧酸高分子样品的剖析提供重要的分析手段,对聚合物的分析具有一定的借鉴作用。

Qualitative analysis of polycarboxylate superplasticizers macromer by ultrafiltration and ¹H NMR

LI Geli, LIN Qian, FANG Yunhui

KZJ New Materials Co., Ltd., Xiamen 361100, China

Abstract: Thetechnology of ultrafiltration and nuclear magnetic resonance hydrogen spectrum (¹H NMR) was established to analyze the type of macromer for unknown polycarboxylate superplastericizer (PC). The results showed that large molecular weight components of unknown PC were filtered step by step after the pretreatment by 30kD,10kD and 3kD ultrafiltration membrane; To obtain relatively puremacromonomer,the filtrate with impurities was further treated by 500D dialysis bag. The technology of ¹H NMR was used to identify common known macromonomer, then parsed the type of macromonomer used in unknown PC was TPEG. This method was provided an important analyticaltool for dissecting PC samples, giving reference to other polymers analysis.

Keywords: polycarboxylate superplasticizers;macromer;ultrafitration;¹H NMR

2015, 41(7): 46-50  收稿日期: 2014-11-18;收到修改稿日期: 2015-1-24

基金项目: 

作者简介: 李格丽(1986-),女,河南商丘市人,助理工程师,硕士,研究方向为混凝土外加剂。

参考文献

[1] Li Y W, Yang C L, Zhang Y F, et al. Study on dispersion,adsorption and flow retaining behaviors of cement mortars with TPEG-type polyether kind polycarboxylatesuperplasticizers[J]. Construction and Building Materials,2014(64):324-332.
[2] Perrot A, Rangeard D, Picandet V, et al. Hydro-mechanical properties of fresh cement pastes containing polycarboxylatesuperplasticizer[J]. Cement and Concrete Research,2013(53):221-228.
[3] Yao B, Lei J H, Du X D, et al. Effect of crosslink structure of bridge polycarboxylatesuperplasticizers on dispersion ability[J]. Journal of Wuhan University of Technology-Mater Sci,2013,28(2):339-342.
[4] Fernández J M, Duran A, Navarro-Blasco I, et al. Influence of nanosilica and a polycarboxylate ether superplasticizer on the performance of lime mortars[J]. Cement & Concrete Research,2013(43):12-24.
[5] 张永玲. 大分子单体及其梳形接枝聚合物的合成及应用[J].齐鲁石油化工,1994(1):65-71.
[6] 王怀斌,程相利,苍大强,等. 高炉钛渣提高混凝土强度的作用机理[J]. 建筑材料学报,2009,12(4):402-406.
[7] Lange A, Plank J. Study on the foaming behaviour of allyl ether-based polycarboxylatesuperplasticizers[J]. Cement and Concrete Research,2012(2):484-489.
[8] Ng S, Plank J. Interaction mechanisms between na-montmorillonite clay and MPEG-based polycarboxylate superplasticizers[J]. Cement and Concrete Research,2012,42(6):847-854.
[9] 张建峰,宋永良,王政伟,等. 大单体结构对聚羧酸减水剂性能的影响[J]. 新型建筑材料,2014,41(4):68-72.
[10] 季春伟,汤世伟,朱云鹤,等. 聚醚单体结构同聚羧酸高性能减水剂性能关系研究[C]//“科隆杯”混凝土外加剂征文-协会第十二次会员代表大会论文集,2013:197-204.
[11] 李强,王晓轩,赵明哲,等. 不同结构大单体合成聚羧酸高效减水剂及其性能研究[J]. 新型建筑材料,2007,34(10):37-42.
[12] 李雪峰,马铁岩,周立明,等. 聚羧酸减水剂聚醚大单体的研究进展及展望[J]. 日用化学品科学,2013(11):21-23.
[13] 韩勇. 论超滤技术在化工工艺工程的应用[J]. 黑龙江科技信息,2014(13):10-11.
[14] 韩志萍,黄茂芳,静玮,等. 超滤分离纯化菠萝蛋白酶的研究[J]. 食品工艺科技,2013,34(8):282-286.
[15] 黄洲,缪冶炼,陈介余,等. 溶液中木质素和葡萄糖的超滤分离[J]. 生物加工工程,2014,12(2):56-62.
[16] 柯余良,方云辉,温庆如,等. 三元共聚羧酸盐减水剂的合成及应用[J]. 新型建筑材料,2011(3):6-7.
[17] 于飞宇,郭鑫祺,麻秀星. 熔融酯化法制备聚羧酸类高效减水剂中间大分子单体[J]. 新型建筑材料,2008(11):80-83.
[18] 赵辉鹏,张琰,查刘生,等. 用NMR分析可生物降解的两亲性嵌段共聚物的分子量和组成[J]. 分析测试学报,2006,25(4):6-10.