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连续管式反应器中降黏型聚羧酸减水剂的合成及性能

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以异戊烯醇聚氧乙烯聚氧丙烯醚(IPEPPG)、2-甲基-2-(丁基三硫代碳酸酯基)丙酸(BTMP)和马来酸酐为主要反应原料,在连续管式反应器中利用热引发可逆加成-断裂链转移(RAFT)聚合,合成了 1 种窄相对分子质量分布的降黏型聚羧酸减水剂VR-PCE-TR.采用 1HNMR、FTIR和GPC对VR-PCE-TR进行了表征,考察VR-PCE-TR对混凝土的工作性能和流变性能的影响,并与釜式反应器中采用常规水相自由基聚合制备的降黏型聚羧酸减水剂进行了性能对比.结果表明,当减水剂溶液质量分数为 10%时,VR-PCE-TR 具有最低表面张力(30.65 mN/m);当减水剂质量分数为0.8%时,VR-PCE-TR对水泥颗粒具有更高的吸附量(2.803 mg/g);在减水剂掺量(以水泥质量计,下同)0.13%时,掺加VR-PCE-TR后的水泥浆体具有更好的分散性和分散保持性;当减水剂掺量为0.4%时,掺加VR-PCE-TR后的水泥净浆具有更小的屈服应力(1.3 Pa)和更低的塑性黏度(0.26 Pa·s).连续管式反应器避免了物料除氧步骤,能够保持聚合控制性和聚合反应速率,因此,制备的VR-PCE-TR具有更窄的相对分子质量分布(多分散性指数为1.19),进而有更好的降黏效果和应用性能.
Synthesis and properties of viscosity-reducing polycarboxylate superplasticizer in continuous tubular reactor
A viscosity-reducing polycarboxylate superplasticizer VR-PCE-TR with a narrow molecular distribution was synthesized from thermally initiated reversible addition-fragmentation chain transfer(RAFT)polymerization of polyoxyethylene polyoxypropylene isopentenol ether(IPEPPG),2-methyl-2-butylsulfanyl-thiocarbonylsulfanyl-propionic acid and maleic anhydride in a continuous tubular reactor,and characterized by 1HNMR,FTIR and GPC.VR-PCE-TR was then evaluated for its influence on the working performance and rheological properties of concrete,and for performance comparison with viscosity-reducing polycarboxylic acid superplasticizers prepared by conventional aqueous free radical polymerization in tank reactor.The results showed that,when the mass fraction of polycarboxylate superplasticizer solution was 10%,VR-PCE-TR exhibited the lowest surface tension(30.65 mN/m).When the superplasticizer mass fraction was 0.8%,VR-PCE-TR displayed a higher adsorption capacity for cement particles(2.803 mg/g).When the dosage(based on the mass of cement,the same below)of superplasticizer was 0.13%,the cement slurry with VR-PCE-TR showed better dispersion and dispersion retention performance,while when the dosage of superplasticizer was 0.4%,the cement slurry with VR-PCE-TR showed a lower yield stress(1.3 Pa)and lower plastic viscosity(0.26 Pa·s).The continuous tubular reactor avoided the material deoxygenation step and could maintain the polymerization control and polymerization reaction rate,therefore,the prepared VR-PCE-TR had a narrower relative molecular mass distribution(polydispersity index was 1.19),and thus had better viscosity reduction effect and application performance.

polycarboxylate superplasticizersrelative molecular mass distributionviscosity-reducingcontinuous tubular reactorthermally initiated RAFT polymerizationbuilding chemicals

钱珊珊、陈烽、彭荩影、刘晓、王玲、姚燕

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安徽海螺材料科技股份有限公司,安徽 芜湖 241000

北京工业大学 材料与制造学部,北京 100124

中国建筑材料科学研究总院有限公司 绿色建筑材料国家重点实验室,北京 100124

聚羧酸减水剂 相对分子质量分布 降黏 连续管式反应器 热引发RAFT聚合 建筑用化学品

国家自然科学基金项目

52372020

2024

精细化工
大连化工研究院设计院 中国化工学会精细化工专业委员会 辽宁省化工研究院

精细化工

CSTPCD北大核心
影响因子:0.557
ISSN:1003-5214
年,卷(期):2024.41(9)