环戊二烯合成甲基环戊二烯的放大试验技术研究

在有关资料的基础上,对以环戊二烯、金属钠和一氯甲烷为原料合成甲基环戊二烯放大试验过程进行了研究,包括环戊二烯钠的制备和环戊二烯甲基化两步反应。放大试验表明,反应温度、搅拌和甲基化试剂滴加方式等因素是影响甲基环戊二烯收率的主要条件。环戊二烯钠的制备初期应严格控制温度条件在0~5℃,缓解环戊二烯二聚体的生产;后期逐渐升温至40℃左右,以加快反应速率。结合放大试验中出现的问题,寻找到了较佳的搅拌、加料等其他条件。在此条件下,甲基环戊二烯的收率为85%,和文献资料基本一致;二甲基环戊二烯的收率仅为2.0%。

Amplification Test Technology Research of Synthesizing Methyl-Cyclopentadiene from Cyclopentadiene

Based on the relevant data, we studied the amplification test progress of synthesizing methyl - cyclo- pentadiene with cyclopentadiene, metallic sodium and methyl chloride as original materials, including two reactions： the preparation of eyelopentadiene sodium and the methylation of cyclopentadiene, in this paper. The amplification test indicates that, the factors such as the reaction temperature, the way of stirring and dropping with the methylating agent were the primary conditions to effect on the methyl - cyclopentadiene yield. The initial the temperature condition should strictly controlled in 0 - 5 ℃ to ease the production of the cyclopentadiene dimer; then gradually heated to a- bout 40 ℃ to accelerate the reaction rate. Combined with the problems found in the amplification test progress, we discovered the best conditions of stirring, dropping with original materials, etc. Under these conditions, the methyl - eyclopentadiene yield of 85%, which is basically the same as the literature; dimethyl- cyclopentadienyl yield of only 2.0%.