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具有自愈和阻燃性能的多功能缓释有机-无机杂化微胶囊的合成与表征

Synthesis and Characterization of a Multifunctional Sustained-Release Organic-Inorganic Hybrid Microcapsule with Self-Healing and Flame-Retardancy Properties.

作者信息

Jiang Wenjing, Zhou Gang, Duan Jinjie, Liu Dong, Zhang Qingtao, Tian Fuchao

机构信息

College of Safety and Environmental Engineering, Shandong University of Science and Technology, Qingdao 266590, China.

State Key Laboratory of Mining Disaster Prevention and Control Co-founded by Shandong Province and the Ministry of Science and Technology, Shandong University of Science and Technology, Qingdao 266590, China.

出版信息

ACS Appl Mater Interfaces. 2021 Apr 7;13(13):15668-15679. doi: 10.1021/acsami.1c01540. Epub 2021 Mar 23.

Abstract

As their service life increases, cement-based materials inevitably undergo microcracking and local damage. In response to this problem, this study used phacoemulsification-solvent volatilization to prepare a multifunctional sustained-release microcapsule (SFRM) with self-healing and flame-retardant characteristics. The synthesis of SFRM is based on the modification of ethyl cellulose with nano-SiO particles and cross-linking with a silane coupling agent to form an organic-inorganic hybrid wall material. The epoxy resin is blended with hexaphenoxy cyclotriphosphazene (HPCTP) to form a composite core emulsion. The surface morphology, particle size distribution, core-shell composition, and thermal stability of SFRM were analyzed via scanning electron microscopy (SEM), energy-dispersive spectrometry (EDS), Malvern, Fourier-transform infrared (FT-IR), and TD-DSC-DTG. It is concluded that SFRM was successfully synthesized with superior particle size distribution and thermal stability. When the ratio of SiO solution and EC alcohol solution reached 1:2, the particle size distribution of the microcapsules was 30-190 μm, and the decreased to 70 μm. The core material content, slow-release performance, and flame retardancy of SFRM were measured using a UV-1800 spectrophotometer and Hartmann tubes, and the compressive and repair properties of SFRM were evaluated by uniaxial compression tests. The results demonstrate that SFRM has satisfactory slow-release and flame-retardancy properties, the LC is 67%, and the first-order kinetic model shows the best fit and conforms to the non-Fickian diffusion mechanism. The SFRM repair rate can reach approximately 61%. This is of substantial significance to the field of self-repairing cement-based materials.

摘要

随着水泥基材料使用寿命的增加,不可避免地会出现微裂纹和局部损伤。针对这一问题,本研究采用超声乳化-溶剂挥发法制备了具有自修复和阻燃特性的多功能缓释微胶囊(SFRM)。SFRM的合成基于用纳米SiO₂颗粒对乙基纤维素进行改性,并与硅烷偶联剂交联以形成有机-无机杂化壁材。将环氧树脂与六苯氧基环三磷腈(HPCTP)共混以形成复合核乳液。通过扫描电子显微镜(SEM)、能谱仪(EDS)、马尔文粒度分析仪、傅里叶变换红外光谱仪(FT-IR)和热重-差示扫描量热-微商热重联用仪(TD-DSC-DTG)对SFRM的表面形貌、粒径分布、核壳组成和热稳定性进行了分析。结果表明,成功合成了具有优异粒径分布和热稳定性的SFRM。当SiO₂溶液与EC醇溶液的比例达到1:2时,微胶囊的粒径分布为30-190μm,且d50降至70μm。用UV-1800分光光度计和哈特曼管测定了SFRM的芯材含量、缓释性能和阻燃性能,并通过单轴压缩试验评估了SFRM的抗压和修复性能。结果表明,SFRM具有令人满意的缓释和阻燃性能,LC为67%,一级动力学模型拟合效果最佳,符合非菲克扩散机制。SFRM的修复率可达61%左右。这对自修复水泥基材料领域具有重要意义。

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