【正文】 aw materials created two intermediate of intumescent flame retardant, Synthesis of intermediate for flame retardant caged bicyclic ,6,7trioxa1phosphabicyc lo[2,2,2]octane(pound Ⅰ ) , and bis(2,6,7trioxa1phosphabicyclo[2,2,2]octane4methanol) chlorophosphate (poundⅡ ) is synthetic study. In the first step, the effects of molar ratio, reaction temperature, time and other factors on the product yields are discussed. The conclusion shows that n(POCI3):n(pentaerythritol) is 1:, temperature rise, react time is 7 hours, and alcohol as solvent for post treatment, the yield was attained up to 86%. In the second step, The conclusion shows that n(POCI3):n(poundⅠ )is 1:, the reaction temperature is 75~80℃ , production rate is 78%. The products were characterized by FTIR. Reaction conditions were also discussed. The result of thermal analysis showed that of they all have high thermal stability and execent charforming ability, deposition temperatures of poundⅠ ~Ⅱ were 300℃ and 340℃ .and residual carbon under 500℃ were % and %. Key words： Intumescent flame retardant。第二步討論了 分批加入 化合物 Ⅰ 和原料配比 對 化合物 Ⅱ 的影響 ，結果表明：乙腈作溶劑，反應的摩爾比 n(化合物 Ⅰ )： n(POCI3)=:1， 反應溫度是 75~80℃ ， 產(chǎn)率 78%。膨脹型阻燃劑中間體的合成研究 Study on Synthesis of Intumescent Flame Retardant Intermediates 目 錄 中文摘要、關鍵詞 ..................................................................................................................... I 英文摘要、關鍵詞 ....................................................................................................................II 引 言 ......................................................................................................................................... 1 第 1章綜 述 ............................................................................................................................. 2 阻燃劑的簡介 ................................................................................................................... 2 阻燃劑的分類 ............................................................................................................... 2 阻燃劑阻燃機理 ........................................................................................................... 4 阻燃劑的發(fā)展現(xiàn)狀及方向 ........................................................................................... 5 膨脹型阻燃劑 簡介 ........................................................................................................... 6 膨脹型阻燃劑的阻燃機理 ........................................................................................... 6 膨脹型阻燃劑的 種類及應用 ....................................................................................... 7 膨脹型阻燃劑的優(yōu)點、存在的問題和改進 ............................................................... 9 本課題研究的內(nèi)容及意義 ..............................................................................................11 第 2章 實驗部分 .................................................................................................................... 12 實驗主要原料與儀器 ..................................................................................................... 12 主要實 驗原料 ............................................................................................................. 12 實驗 主要 儀器 ............................................................................................................. 12 合成路線 ......................................................................................................................... 13 1氧基磷雜 4羥甲基 2,6,7三氧雜雙環(huán) [2,2,2]辛烷（化合物Ⅰ）的合成路線 .................................................................................................................................. 13 二（ 2,6,7三氧雜 1氧基磷雜雙環(huán) [2,2,2]辛烷 4亞甲基） 磷 酰氯（ 化合物Ⅱ ）的 合成路線 .............................................................................................................. 13 合成步驟 ......................................................................................................................... 13 化合物 Ⅰ 的制備 ......................................................................................................... 13 化合物 Ⅱ 的制備 ......................................................................................................... 13 紅外光譜分析 .................................................................................................................. 14 熱失重分析 ...................................................................................................................... 14 第 3章結果與討論 .................................................................................................................. 15 4羥甲基 2,6,7三氧雜雙環(huán) [2,2,2]辛烷（化合物Ⅰ）的影響分析 15 反應溫度的影響 ......................................................................................................... 15 反應時間的影響 ......................................................................................................... 15 原料配比的影響 ......................................................................................................... 16 二（ 2,6,7三氧雜 1氧基磷雜雙環(huán) [2,2,2]辛烷 4亞甲基） 磷 酰氯（ 化合物Ⅱ ）影響分析 .................................................................................................................. 16 加料方式對 化合物Ⅱ的產(chǎn)率的影響 ......................................................................... 16 原料配比對產(chǎn)率的影響 ............................................................................................. 17 季戊四醇磷酸酯紅外光譜圖的表征 ............................................................................. 17 季戊四醇磷酸酯化合物Ⅰ的紅外光譜圖表征 ......................................................... 17 季戊四醇磷酸酯 化合物Ⅱ的紅外光譜的表征 ......................................................... 18 季戊四醇磷酸酯的熱重分析 ......................................................................................... 19 季戊四醇磷酸酯化合物 Ⅰ 的熱失重圖 ..................................................................... 19 季戊四醇磷酸酯化合物 Ⅱ 的熱失重圖 .................