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Synthesis of a phosphorus-nitrogen-containing flame retardant and its application in epoxy resin

机译：合成含磷 - 氮的阻燃剂及其在环氧树脂中的应用

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In this article, a phosphorus-nitrogen-containing flame retardant (DOPO-T) was successfully synthesized by nucleophilic substitution reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and cyanuric chloride. The chemical structure of DOPO-T was characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance (NMR) and phosphorous-31 NMR, and elemental analysis. DOPO-T was then blended with diglycidyl ether of bisphenol-A to prepare flame-retardant epoxy resins. Thermal properties, flame retardancy, and combustion behavior of the cured epoxy resins were evaluated by differential scanning calorimetry, thermogravimetric analysis, limited oxygen index (LOI) measurement, UL94 vertical burning test, and cone calorimeter test. The results indicated that the glass transition temperature (T-g) and temperature at 5% weight loss of epoxy resin (EP)/DOPO-T thermosets were gradually decreased with the increasing content of DOPO-T. DOPO-T catalyzed the decomposition of EP matrix in advance. The flame-retardant performance of EP thermosets was significantly enhanced with the addition of DOPO-T. EP/DOPO-T-0.9 sample had an LOI value of 36.2% and achieved UL94 V-1 rating. In addition, the average of heat release rate, peak of heat release rate, average of effective heat of combustion, and total heat release (THR) of EP/DOPO-T-0.9 sample were decreased by 32%, 48%, 23%, and 31%, respectively, compared with the neat EP sample. Impressively, EP/DOPO-T thermosets acquired excellent flame retardancy under low loading of flame retardant.
机译：在本文中，通过9,10-二羟基-9-氧乙烯-10-磷蒽 - 10-氧化物（DOPO）和氰尿酰氯之间的亲核取代反应成功地合成了含磷 - 氮的阻燃剂（DoPO-T）。 DOPO-T的化学结构的特征在于傅里叶变换红外光谱，质子核磁共振（NMR）和磷-31nMR，以及元素分析。然后将DOPO-T与双酚-A的二缩水甘油醚混合以制备阻燃环氧树脂。通过差示扫描量热法，热重分析，有限的氧指数（LOI）测量，UL94立式燃烧试验和锥形量热计测试评估固化环氧树脂的热性质，阻燃性和燃烧行为。结果表明，随着DOPO-T的含量增加，玻璃化转变温度（T-G）和5％重量损失的温度逐渐降低。 DOPO-T预先催化EP矩阵的分解。通过添加DOPO-T，EP热固性件的阻燃性能显着增强。 EP / DOPO-T-0.9样品的LOI值为36.2％，实现了UL94 V-1等级。此外，热释放速率的平均值，热释放速率的峰值，燃烧的平均热量，以及EP / DOPO-T-0.9样品的总热释放（Thr）的释放率和总热释放（Thr）降低了32％，48％，23％与整齐的EP样品相比，31％分别。令人印象深刻，EP / DOPO-T热固性件在低负载阻燃性下获得了出色的阻燃性。

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