连续RAFT光聚合法合成聚羧酸减水剂
作者:
作者单位:

1.江苏奥莱特新材料股份有限公司 江苏省(奥莱特)混凝土高分子助剂工程技术研究中心,江苏 南京 211505;2.北京工业大学 材料科学与工程学院,北京 100124;3.中国建筑材料科学研究总院 绿色建筑材料国家重点实验室,北京 100124

作者简介:

彭荩影(1993—),女,安徽宣城人,江苏奥莱特新材料股份有限公司研发工程师,硕士.E-mail:aritpjy@163.com

通讯作者:

钱珊珊(1987—),男,安徽安庆人,江苏奥莱特新材料股份有限公司研发总监,北京工业大学博士生.E-mail:aritqss@163.com

中图分类号:

TU528.042.2

基金项目:

国家自然科学基金资助项目(51578025);北京市属高校高水平教师队伍建设支持计划青年拔尖人才培育计划项目(CIT&TCD201804008)


Preparation of Polycarboxylate-Based Superplasticizer by Continuous Photo-Mediated RAFT Polymerization
Author:
Affiliation:

1.Jiangsu Province Engineering Research Center (ARIT) of Concrete Polymer Additives, Jiangsu China Railway ARIT New Materials Co., Ltd., Nanjing 211505, China;2.College of Materials Science and Engineering, Beijing University of Technology, Beijing 100124, China;3.Sate Key Laboratory of Green Building Materials, China Building Materials Academy, Beijing 100124, China

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    摘要:

    以甲基丙烯酸聚乙二醇单甲醚酯和丙烯酸为主要原料,通过光调控水相可逆加成-断裂链转移(RAFT)聚合,在连续管式反应器中成功合成了聚羧酸减水剂,并采用核磁共振仪(NMR)、傅里叶红外光谱仪(FTIR)、凝胶渗透色谱仪(GPC)和动态光散射仪(DLS)等表征了减水剂的结构.结果表明:RAFT聚合聚羧酸减水剂的相对分子质量分布更集中,分散性和分散保持性更好;连续RAFT聚合工艺可以实现可控聚合物的连续化生产,连续管式反应器中有限的氧含量使得RAFT聚合可以在不预先除氧的情况下成功进行,为聚羧酸减水剂的可控合成提供了新的思路.

    Abstract:

    A kind of polycarboxylate-based superplasticizer(PCE) was successfully synthesized by photo-mediated reversible addition-fragmentation chain transfer(RAFT) polymerization with poly(ethylene glycol)methyl ether methacrylate(PEGMA) and acrylic acid(AA) as the main material. The molecular structure of the products was characterized by nuclear magnetic resonance(NMR), gel permeation chromatography(GPC), infra-red spectrum(IR) and dynamic light scattering(DLS). The results show that the product has narrow distribution of the relative molecular mass, the advantages of strong disperse ability and excellent slump retention. Moreover, continuous RAFT process can realize continuous production of controlled polymers. The limited oxygen content in the continuous tubular reactor allows RAFT polymerization to be successfully carried out without prior deoxygenation process, which can provide a new idea for controlled synthesis of polycarboxylate-based superplasticizer.

    表 4 3种PCE在混凝土中应用性能对比Table 4 Performance comparison of 3 kinds of PCE in concrete
    表 1 3种PCE的GPC数据Table 1 GPC results of 3 kinds of PCE
    图1 连续光调控RAFT聚合法制备聚羧酸减水剂示意图Fig.1 Diagram of PCE prepared by continuous photo-mediated RAFT polymerization
    图2 3种聚羧酸减水剂的FTIR图谱Fig.2 FTIR spectra of 3 kinds of PCE
    图3 3种聚羧酸减水剂的1H NMR图谱Fig.3 1H NMR spectra of 3 kinds of PCE
    图4 3种聚羧酸减水剂的GPC流出曲线Fig.4 GPC traces of 3 kinds of PCE
    图5 不同停留时间聚羧酸减水剂的1H NMR图谱Fig.5 1H NMR spectra of PCE for different polymerization times
    图6 聚合过程分析Fig.6 Analysis of polymerization steps
    图7 PCE聚合方式对水泥净浆流动度的影响Fig.7 Effect of different polymerization methods on fluidity of cement paste
    图8 连续管式反应器中的RAFT聚合示意图Fig.8 Diagram of RART polymerization in continuous tubular reactor
    表 3 不同停留时间聚羧酸减水剂的转化率及GPC数据Table 3 Conversion and GPC results of PCE for different polymerization times
    表 2 3种聚羧酸减水剂的粒径及粒径分布Table 2 Size and size distribution of 3 kinds of PCE
    参考文献
    [1] 余文志. RAFT法合成聚羧酸减水剂及相对分子质量参数对其应用性能影响的研究[D]. 广州:华南理工大学, 2015.
    [2] YU B, ZENG Z, REN Q, et al. Study on the performance of polycarboxylate-based superplasticizers synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization[J]. Journal of Molecular Structure, 2016, 1120:171-179.
    [3] 李东旭, 陈洋, 周生态, 等. RAFT法制备嵌段型聚羧酸减水剂及其水化性能[J]. 合成化学, 2019, 27(7):513-517.
    [4] EZZAT M, XU X, CHEIKH K, et al. Structure-property relationships for polycarboxylate ether superplasticizers by means of RAFT polymerization[J]. Journal of Colloid and Interface Science, 2019, 553:788-797.
    [5] LU L, ZHANG H, YANG N, et al. Toward rapid and well-controlled ambient temperature RAFT polymerization under UV-Vis radiation:Effect of radiation wave range[J]. Macromolecules, 2006, 39(11):3770-3776.
    [6] XU J, JUNG K, ATME A, et al. A robust and versatile photoinduced living polymerization of conjugated and unconjugated monomers and its oxygen tolerance[J]. Journal of the American Chemical Society, 2014, 136(14):5508-5519.
    [7] MCKENZIE T, FU Q, WONG E, et al. Visible light mediated controlled radical polymerization in the absence of exogenous radical sources or catalysts[J]. Macromolecules, 2015, 48(12):3864-3872.
    [8] CAMBIE D, BOTTECCHIA C, STRAATHOF N, et al. Applications of continuous-flow photochemistry in organic synthesis, material science, and water treatment[J]. Chemical Reviews, 2016, 116(17):10276-10341.
    [9] PENG J, XU Q, NI Y, et al. Visible light controlled aqueous RAFT continuous flow polymerization with oxygen tolerance[J]. Polymer Chemistry, 2019, 10(16):2064-2072.
    [10] WILMS D, KLOS J, FREY H. Microstructured reactors for polymer synthesis:A renaissance of continuous flow processes for tailor-made macromolecules?[J]. Macromolecular Chemistry and Physics, 2008, 209(4):343-356.
    [11] TAO L, LIU J, DAVIS T. Branched polymer-protein conjugates made from mid-chain-functional P(HPMA)[J]. Biomacromolecules, 2009, 10(10):2847-2851.
    [12] TRUONG N, DUSSERT M, WHITTAKER M, et al. Rapid synthesis of ultrahigh molecular weight and low polydispersity polystyrene diblock copolymers by RAFT-mediated emulsion polymerization[J]. Polymer Chemistry, 2015(6):3865-3874.
    [13] ABDOLLAHI H, NAJAFI V, ZIAEE F, et al. Radical copolymerization of acrylic acid and OEGMA475:Monomer reactivity ratios and structural parameters of the copolymer[J]. Macromolecular Research, 2014, 22(12):1330-1336.
    [14] DECKER C, JENKINS A. Kinetic approach of oxygen inhibition in ultraviolet- and laser-induced polymerizations[J]. Macromolecules, 1985, 18(6):1241-1244.
    [15] O’BRIEN A, CRAMER N, BOWMAN C. Oxygen inhibition in thiol-acrylate photopolymerizations[J]. Journal of Polymer Science Part A:Polymer Chemistry, 2006, 44(6):2007-2014.
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彭荩影,钱珊珊,姚燕,王子明,郑春扬.连续RAFT光聚合法合成聚羧酸减水剂[J].建筑材料学报,2021,24(6):1328-1334

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  • 收稿日期:2020-03-25
  • 最后修改日期:2020-04-27
  • 录用日期:2020-05-11
  • 在线发布日期: 2021-12-28
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