CHINESE JOURNAL OF ENERGETIC MATERIALS
+高级检索
3,4-二氨基呋咱的两种催化合成新方法
作者:
作者单位:

西安近代化学研究所 七部

作者简介:

李春迎(1979-),女,博士,从事催化合成方面的研究

通讯作者:

基金项目:

国家重点基础研究发展计划(973计划)


Two New Synthesis Method of 3,4-Diaminofurazan
Author:
Affiliation:

Xi’an Modern Chemistry Research Institute

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
    摘要:

    研究了胶束催化和负载型固体碱催化的3, 4-二氨基乙二肟分子内脱水合成3, 4-二氨基呋咱的两种新方法。负载型固体碱催化下,考察了反应温度、压力、物料配比等对反应收率的影响,较佳的反应条件为:150 ℃,0.7 MPa,3, 4-二氨基乙二肟(DAG)与负载型固体碱催化剂(cat.)和H2O的质量比为1:3.5:12.5,反应时间4 h,该条件下收率为91.2%。催化剂分离后重复使用五次以上,催化活性无明显下降。与氢氧化钾催化的反应相比,催化剂用量少,反应温度及压力低,收率高,易分离。胶束催化下,阴、阳离子表面活性剂在大于临界胶束浓度下均具有良好的催化效果,升高压力不利于反应进行。110 ℃,DAG与KOH、H2O及十二烷基苯磺酸钠(SDBS)的质量比为1:1.3:7.1:0.02条件下,常压反应10 h,反应收率为46.0%。

    Abstract:

    3, 4-Diaminofurazan was prepared from 3, 4-diaminoglyoxime by two new methods. Supported solid alkali or micelle was used as catalysts in the reaction first time. When the reaction catalyzed by supported solid alkali, the optimal conditions are: 150 ℃, 3, 4-diaminoglyoxime:supported solid alkali:H2O(mass)=1:3.5:12.5, 4 h. Under those conditions, the yield could be improved to 91.2%. The temperature, pressure and catalyst amount are lower and yield is higher than the reaction catalyzed by KOH. Moreover, the catalyst can be reused at least five times without decreasing of catalyst activity. Then, 3, 4-diaminofurazan synthesis catalyzed by micelle was explored. Anionic and cationic surfactants both possessed well catalytic activity when the mass ratio of surfactant and 3, 4-diaminoglyoxime was 0.02. On the condition of 110 ℃, DAG:KOH:H2O:sodium dodecyl benzene sulfonate(mass)=1:1.3:7.1:0.02, when the reaction time was 10 h, the yield was 46.0%. Compared with the reaction without catalyzed by micelle, the cite reaction could react at lower temperature and pressure.

    参考文献
    相似文献
    引证文献
文章指标
  • PDF下载次数:
  • HTML阅读次数:
  • 摘要点击次数:
  • 引用次数:
引用本文

李春迎,马洋博,薛云娜,等.3,4-二氨基呋咱的两种催化合成新方法[J].含能材料, 2012, 20(2):151-154. DOI:10.3969/j. issn.1006-9941.2012.02.003.
LI Chun-ying, MA Yang-bo, XUE Yun-na, et al. Two New Synthesis Method of 3,4-Diaminofurazan[J]. Chinese Journal of Energetic Materials, 2012, 20(2):151-154. DOI:10.3969/j. issn.1006-9941.2012.02.003.

复制
历史
  • 收稿日期: 2011-04-26
  • 最后修改日期: 2011-07-11
  • 录用日期: 2011-08-25
  • 在线发布日期: 2012-04-23
  • 出版日期: