CHINESE JOURNAL OF ENERGETIC MATERIALS
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液相连续制备挂式四氢双环戊二烯
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(北京理工大学化工与环境学院, 北京 100081)

作者简介:

陈华祥(1989-),男,硕士研究生,主要从事高能燃料挂式四氢双环戊二烯的合成研究。e-mail: 2120121292@bit.edu.cn 通信联系人: 史大昕(1975-),男,讲师,主要从事有机合成新试剂新方法研究。e-mail: shidaxin@bit.edu.cn

通讯作者:

史大昕(1975-),男,讲师,主要从事有机合成新试剂新方法研究。e-mail: shidaxin@bit.edu.cn

基金项目:

国家国际科技合作项目基金资助(2012DFR40240)


Liquid-phase Continuous-flow Preparation of High Energy Fuel Exo-THDCPD
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(School of Chemical Engineering & Environment,Beijing Institute of Technology, Beijing 100081,China)

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    摘要:

    挂式四氢双环戊二烯(exo-THDCPD)是重要的高密度液体烃类燃料。为提高exo-THDCPD的合成效率, 研究了连续制备exo-THDCPD的新工艺, 包括两个反应器(鼓泡式连续流加氢反应器和连续流异构化釜式反应器)的串联, 即两个过程(Pd/C催化环戊二烯二聚体(DCPD)加氢制备桥式四氢双环戊二烯(endo-THDCPD)和AlCl3催化endo-THDCPD异构合成exo-THDCPD)的串联。结果表明, 液相连续制备exo-THDCPD的较佳工艺条件为:重时空速2.4 h-1, 加氢压力0.1 MPa, 氢气流速80 mL·min-1, DCPD浓度0.76 mol·L-1, 加氢反应温度30 ℃, 异构化反应温度70 ℃; DCPD转化率100%, exo-THDCPD收率92.5%。

    Abstract:

    Exo-tetrahydrodicyclopentadiene (exo-THDCPD) is an important high density liquid hydrocarbon fuel. To improve the synthesis efficiency of exo-THDCPD, a new process of continuous preparation of exo-THDCPD, including the cascade of two reactors (continuous-flow bubbling hydrogenation reactor and continuous-flow isomerization tank reactor), namely the cascade of two processes (dicyclopentadiene (DCPD) was hydrogenated to endo-THDCPD over Pd/C catalyst and the endo-THDCPD was isomerized to exo-THDCPD over AlCl3 catalyst) was studied. The liquid-phase continuous-flow preparation of exo-THDCPD was realized. Results show that the optimum liquid-phase continuous-flow process conditions of preparing exo-THDCPD are determined as: weight hourly space velocity(WHSV), 2.4 h-1; hydrogenation pressure(pH), 0.1 MPa; H2 gas flow rate, 80 mL·min-1; DCPD concentration (CDCPD), 0.76 mol·L-1; hydrogenation reaction temperature: 30 ℃; isomerization; reaction temperature, 70 ℃; conversion of DCPD, 100% and yield of exo-THDCPD, 92.5%.

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引用本文

陈华祥,李加荣,黎汉生,等.液相连续制备挂式四氢双环戊二烯[J].含能材料, 2015, 23(10):964-970. DOI:10.11943/j. issn.1006-9941.2015.10.009.
CHEN Hua-xiang, LI Jia-rong, LI Han-sheng, et al. Liquid-phase Continuous-flow Preparation of High Energy Fuel Exo-THDCPD[J]. Chinese Journal of Energetic Materials, 2015, 23(10):964-970. DOI:10.11943/j. issn.1006-9941.2015.10.009.

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  • 收稿日期: 2014-10-29
  • 最后修改日期: 2014-01-16
  • 录用日期: 2015-01-22
  • 在线发布日期: 2015-09-01
  • 出版日期: 2015-09-10