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SYNTHESIS AND SOLUBILITIES OF 3,9-DIPYROLIDINO-2,4,8,10-TETRAOXA-3,9-DIPHOSPHASPIRO[5.5]UNDECANE-3,9-DIOXIDE IN SELECTED SOLVENTS
Chemical Engineering Communications ( IF 1.9 ) Pub Date : 2014-08-21 , DOI: 10.1080/00986445.2013.818985 R. L. Fan , L. Guo , P. Z. Wang , S. F. Chen , Z. X. Bian
Chemical Engineering Communications ( IF 1.9 ) Pub Date : 2014-08-21 , DOI: 10.1080/00986445.2013.818985 R. L. Fan , L. Guo , P. Z. Wang , S. F. Chen , Z. X. Bian
A flame retardant with enhanced phosphorus-nitrogen content, 3,9-dipyrolidino-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane-3,9-dioxide (DTDP) was synthesized by the reaction of 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5,5]undecane (SPDPC) with pyrrole. The structure and the thermal stability of the compound were characterized by infrared spectroscopy (IR), nuclear magnetic resonance (1H NMR and 13C NMR), mass spectroscopy (MS), elemental analysis, and thermogravimetric analysis (TGA). Using a static analytical method, the solubilities of DTDP in N,N-dimethylformamide (DMF) in the temperature range from 302.80 to 362.05 K and in water in the temperature range from 303.65 to 360.75 K were determined. The solubilities of DTDP in ethanol, acetonitrile, acetone, acetic ester, and DMF + water binary mixtures were also measured for comparison. The solubility data were correlated with an empirical equation.
中文翻译:
3,9-DIPYROLIDINO-2,4,8,10-TETRAOXA-3,9-DIPHASPIRO[5.5]UNDECANE-3,9-DIOXIDE在选定溶剂中的合成和溶解度
通过以下反应合成了一种提高磷氮含量的阻燃剂 3,9-dipyrolidino-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane-3,9-dioxide (DTDP) 3,9-二氯-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5,5]undecane (SPDPC) 与吡咯。该化合物的结构和热稳定性通过红外光谱(IR)、核磁共振(1H NMR和13C NMR)、质谱(MS)、元素分析和热重分析(TGA)表征。使用静态分析方法,测定了 DTDP 在 302.80 至 362.05 K 温度范围内的 N,N-二甲基甲酰胺 (DMF) 和 303.65 至 360.75 K 温度范围内的水中溶解度。DTDP 在乙醇、乙腈、丙酮、醋酸酯中的溶解度 还测量了 DMF + 水二元混合物以进行比较。溶解度数据与经验方程相关。
更新日期:2014-08-21
中文翻译:
3,9-DIPYROLIDINO-2,4,8,10-TETRAOXA-3,9-DIPHASPIRO[5.5]UNDECANE-3,9-DIOXIDE在选定溶剂中的合成和溶解度
通过以下反应合成了一种提高磷氮含量的阻燃剂 3,9-dipyrolidino-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane-3,9-dioxide (DTDP) 3,9-二氯-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5,5]undecane (SPDPC) 与吡咯。该化合物的结构和热稳定性通过红外光谱(IR)、核磁共振(1H NMR和13C NMR)、质谱(MS)、元素分析和热重分析(TGA)表征。使用静态分析方法,测定了 DTDP 在 302.80 至 362.05 K 温度范围内的 N,N-二甲基甲酰胺 (DMF) 和 303.65 至 360.75 K 温度范围内的水中溶解度。DTDP 在乙醇、乙腈、丙酮、醋酸酯中的溶解度 还测量了 DMF + 水二元混合物以进行比较。溶解度数据与经验方程相关。