一种支化取代酚安定剂的合成及表征

    Synthesis and characterization of a branched substituted phenolic stabilizer

    • 针对现有安定剂存在与异氰酸酯发生副反应和潜在致癌性等问题,设计了一种适用于含硝酸酯类推进剂的新型支化取代酚安定剂。以三羟甲基丙烷三缩水甘油醚和2,6-二甲氧基苯酚为主要原料,使用水和乙醇形成的混合溶剂,在碳酸钾的催化条件下,合成了一种三羟甲基丙烷三缩水甘油醚-三-2,6-二甲氧基苯酚开环加成物(AH3),并利用核磁共振氢谱、傅里叶变换红外光谱对其分子结构进行表征;通过差示扫描量热法研究了AH3(质量含量为1%)与聚乙二醇(PEG)/硝酸甘油(NG)/ 1,2,4-丁三醇三硝酸酯(BTTN)胶片的相容性;分别研究了含1%AH3和1%MNA的PEG/NG/BTTN胶片经70 ℃、加热14 d后的阿贝尔实验试纸变色时间。结果表明,合成的AH3分子结构与设计分子结构一致,其纯度为97.2%;AH3与PEG/NG/BTTN组分有较好的相容性,与之相应的阿贝尔试验试纸变色时间大于60 min,表明AH3可以较好地捕获硝酸酯分解放出的氮氧化物,具有进一步研究的价值。

       

      Abstract: To address the issues that existing stabilizers face, such as side reactions with isocyanates and potential carcinogenicity, a novel branched substituted phenolic stabilizer suitable for nitrate ester-containing propellants was designed. A trimethylolpropane triglycidyl ether-tris(2,6-dimethoxyphenol) ring-opening adduct (AH3) was synthesized from trimethylolpropane triglycidyl ether and 2,6-dimethoxyphenol as main raw materials in a mixed solvent of water and ethanol using potassium carbonate as catalyst. Its molecular structure was characterized by ¹H nuclear magnetic resonance (¹H NMR) spectroscopy and Fourier transform infrared (FT-IR) spectroscopy. The compatibility of AH3 (at an addition level of 1%) with a poly(ethylene glycol)(PEG)/nitroglycerin (NG) /1,2,4-butanetriol trinitrate (BTTN) film was investigated by differential scanning calorimetry (DSC). The color-change times in the Abel test for PEG/NG/BTTN films containing 1% AH3 and 1% MNA, respectively, after heating at 70 ℃ for 14 days were measured. The results show that the molecular structure of the synthesized AH3 is consistent with the designed structure, with a purity of 97.2%. AH3 exhibits good compatibility with the PEG/NG/BTTN components. The Abel test color-change time exceeds 60 min, indicating AH3 can effectively capture nitrogen oxides released from nitrate ester decomposition and its potential value for further research.

       

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