Alič Branko, Šebenik Urška, Krajnc Matjaž
University of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, 1000 Ljubljana, Slovenia.
Polymers (Basel). 2024 Aug 29;16(17):2463. doi: 10.3390/polym16172463.
This paper presents a two-stage microencapsulation process that uses pH modulation to enhance the thermal stability of microcapsules that consist of a melamine-formaldehyde (MF) shell and a butyl stearate core. In the first stage, the pH value was modulated between 6.0 and 8.0. Rising the pH value to 8.0 slowed the polycondensation rate, allowing the MF resin with a lower degree of polymerization to migrate to the capsule surface and form a smooth shell. Lowering the pH value to 6.0 accelerated polycondensation. In the second stage, a relatively fast, continuous reduction in the pH value to 5.0 led to further MF polycondensation, hardening the shell. Post-curing at 100 °C prevented shell damage caused by the liquid-gas phase transition of the core material during the process. The microcapsules produced by increasing the pH value to 8.0 twice demonstrated improved thermal stability, with only a minimal overall weight loss of 5% at 300 °C. Significant weight loss was observed between 350 and 400 °C, temperatures at which the methylene bridges in the MF shell undergo thermal degradation. The results from differential scanning calorimetry, electron microscopy, and thermogravimetry analyses confirmed a successful optimization of the microencapsulation, showing that these microcapsules are promising for thermal energy storage and other applications that require high thermal stability.
本文介绍了一种两步微胶囊化工艺,该工艺利用pH调节来提高由三聚氰胺 - 甲醛(MF)壳和硬脂酸丁酯芯组成的微胶囊的热稳定性。在第一阶段,pH值在6.0至8.0之间调节。将pH值升至8.0会减慢缩聚速率,使聚合度较低的MF树脂迁移到胶囊表面并形成光滑的壳。将pH值降至6.0会加速缩聚。在第二阶段,将pH值相对快速、持续地降至5.0会导致进一步的MF缩聚,使壳变硬。在100°C下后固化可防止在该过程中芯材的液 - 气相转变导致壳受损。通过将pH值两次升至8.0所制备的微胶囊表现出 improved thermal stability,在300°C时总体重量损失仅为最小的5%。在350至400°C之间观察到显著的重量损失,在此温度下MF壳中的亚甲基桥会发生热降解。差示扫描量热法、电子显微镜和热重分析的结果证实了微胶囊化的成功优化,表明这些微胶囊在热能存储和其他需要高热稳定性的应用中具有前景。 (注:improved thermal stability这里英文原文有误,可能是higher thermal stability,推测应翻译为“更高的热稳定性” )