Key Laboratory of Eco-functional Polymer Materials of the Ministry of Education, Key Laboratory of Eco-environmental Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, 967 Anning Road, Lanzhou, Gansu, 730070, China.
Lanzhou Fire and Rescue Division, Lanzhou, Gansu, China.
Chemosphere. 2021 Jun;273:129658. doi: 10.1016/j.chemosphere.2021.129658. Epub 2021 Jan 18.
In this study, a novel organic-inorganic hybrid flame retardant 10-(1,4-dicarboxylic acid magnesium salt)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DMMH) was synthesized via neutralization and addition reaction of maleic acid, magnesium hydroxide and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), and subsequently used in an intrinsic flame retardant epoxy resin. The chemical structure and morphology of DMMH were analyzed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Further, the prepared DMMH was combined with ammonium polyphosphate (APP) to form an intumescent flame retardant system. The thermal stability and flame retardance were evaluated by thermogravimetric analysis (TG), UL-94 vertical burning test, limiting oxygen index (LOI) and cone calorimetry. It was observed that the addition of 1.7% DMMH and 5.3% APP led EP-7 to acquire UL-94 V-0 rating, with the limiting oxygen index of 26.0%. As compared with pure EP, the peak heat release rate, total heat release, smoke production rate and total smoke production of the sample was noted to decrease by 54.5%, 35.1%, 43.6% and 38.1%, respectively. In addition, the introduction of DMMH did not negatively impact the mechanical properties of the epoxy resin.
在这项研究中，通过马来酸、氢氧化镁和 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO）的中和加成反应，合成了一种新型的有机-无机杂化阻燃剂 10-（1,4-二羧酸镁盐）-9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物（DMMH），并随后将其用于本征阻燃环氧树脂中。通过傅里叶变换红外光谱（FTIR）、X 射线光电子能谱（XPS）和扫描电子显微镜（SEM）分析了 DMMH 的化学结构和形态。此外，将制备的 DMMH 与聚磷酸铵（APP）结合形成膨胀型阻燃体系。通过热重分析（TG）、UL-94 垂直燃烧试验、极限氧指数（LOI）和锥形量热法评估了热稳定性和阻燃性。结果表明，添加 1.7%的 DMMH 和 5.3%的 APP 使 EP-7 获得 UL-94 V-0 等级，其极限氧指数为 26.0%。与纯 EP 相比，该样品的峰值放热率、总放热量、生烟率和总生烟量分别降低了 54.5%、35.1%、43.6%和 38.1%。此外，DMMH 的引入并没有对环氧树脂的力学性能产生负面影响。
