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氟碳聚醚单体——1,1,5-三氢八氟戊基缩水甘油醚合成研究——特种聚氨酯预聚体端羟基氟碳聚醚研究Ⅲ
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Synthesis of 1,1,5-Trihydro-octafluoro Pentyl Glycidylether—A Monomer for Fluoro-carbonic Polyether —An Investigation of Hydroxy-terminated Fluoro-carbonic Polyether for Special Polyurethane Prepolymer Ⅲ
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    摘要:

    在合成氟碳聚醚单体1,1,5-三氢八氟戊基缩水甘油醚(FGE-2)的过程中,用气液色谱跟踪研究1,1,5-三氢八氟戊醇(FOH-2)与环氧氯丙烷(ECH)在 NaOH存在下的缩合反应进程,发现该反应是一个可逆反应; 反应温度较低(30℃)时反应速度太慢,反应温度过高(80℃)时平衡逆向移动,较适合的反应温度为50℃。当反应物摩尔比为: FOH-2/ECH/NaOH=1/3/1~1.2时,在无水介质中,采用FOH-2后加法,反应4~5h即达平衡; 若NaOH过量5%~20%,转化率达90%以上,产率可达82%。采用ECH后加法,也得到良好结果。反应物经减压精密分馏,分离回收ECH和FOH-2后,收集在266.6Pa真空度下b.p. 68℃的馏分,得到FGE-2产品,环氧值为0.3440~0.3471mol/100g,纯度达99%以上。

    Abstract:

    The condensation reaction of 1,1,5-trihydro-octafluoro-pentanol (FOH-2) with epichlorohydrin (ECH) under the presence of NaOH to form 1,1,5-trihydro-octafluoro pentyl glycidylether(FGE-2) was investigated by using gas-liquid chromatograph. The reaction was found to be reversible and reach into equilibrium under the conditions of non-aqueous medium,mole ratio of reactants FOH-2/ECH/NaOH=1/3/1~1.2,post addition of FOH-2, reaction temperature of 50℃ and reaction time 4 to 5h.If the excess of NaOH was in the range of 5%~20%,the conversion of FOH-2 into FGE-2 would be higher than 90%. A satisfied result was also obtained in the case of post-adding ECH. The raw product was fractionated under reduced pressure and collected the fine FGE-2 at 68℃ and 266.6Pa with yield of 82% and epoxy value 0.3440~0.3470mol/100g.

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陈世武,李开罢,徐志宏,等.氟碳聚醚单体——1,1,5-三氢八氟戊基缩水甘油醚合成研究——特种聚氨酯预聚体端羟基氟碳聚醚研究Ⅲ[J].含能材料, 1999, 7(1):5-10.
CHEN Shi-wu, LI Kai-ba, XU Zhi-hong, et al. Synthesis of 1,1,5-Trihydro-octafluoro Pentyl Glycidylether—A Monomer for Fluoro-carbonic Polyether —An Investigation of Hydroxy-terminated Fluoro-carbonic Polyether for Special Polyurethane Prepolymer Ⅲ[J]. Chinese Journal of Energetic Materials, 1999, 7(1):5-10.

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  • 收稿日期: 1998-04-29
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  • 在线发布日期: 2011-11-02
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