高等学校化学学报

高等学校化学学报 ›› 2011, Vol. 32 ›› Issue (7): 1541.

• 研究论文 • 上一篇    下一篇

N,N'-二乙氧羰基-O,O'-烷基二硫氨酯的合成及表征

袁露, 钟宏, 刘广义, 夏柳荫, 李立清   

  1. 中南大学化学化工学院, 长沙410083
  • 收稿日期:2010-08-27 修回日期:2010-10-12 出版日期:2011-07-10 发布日期:2011-06-02
  • 通讯作者: 钟宏 E-mail:zhongh@mail.csu.edu.cn
  • 基金资助:

    国家“九七三”计划项目(批准号: 2007CB613602-3),  国家“八六三”计划项目(批准号: 2007AA06Z122)和国家自然科学基金(批准号: 51074183, 50604016)资助.

Synthesis and Characterization of N,N'-Diethoxycarbonyl-O,O'-alkyl-dithiocarbamates

YUAN Lu, ZHONG Hong*, LIU Guang-Yi, XIA Liu-Yin, LI Li-Qing   

  1. School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China
  • Received:2010-08-27 Revised:2010-10-12 Online:2011-07-10 Published:2011-06-02
  • Contact: ZHONG Hong E-mail:zhongh@mail.csu.edu.cn
  • Supported by:

    国家“九七三”计划项目(批准号: 2007CB613602-3),  国家“八六三”计划项目(批准号: 2007AA06Z122)和国家自然科学基金(批准号: 51074183, 50604016)资助.

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被引次数

13

摘要： 关于含有一个酯基和一个硫代酰胺基团的硫氨酯的合成研究已有大量报道，但含有两个酯基和两个硫代酰胺基团的硫氨酯的合成研究尚未见报道。由氯甲酸乙酯和硫氰酸钠经亲核取代反应和异构化合成N-烃氧羰基异硫氰酸酯中间体，再将该中间体与二醇经亲核加成反应，合成出了3种未见报道的N,N’-二乙氧羰基-O,O’-烷基二硫氨酯。经元素分析、红外光谱、核磁共振氢谱及碳谱分析，证实所合成的化合物即为目标产物。小型浮选实验表明，仅使用6 g/t的目标化合物a~c，铜的品位即可分别达到6.12%、6.35%、5.92%，回收率分别达到75.31%、76.50%、76.35%，用量远低于丁基黄药，且铜的品位和回收率都有不同程度的提高，可作为一种新型捕收剂应用到硫化铜类的矿物浮选中。

关键词: 二乙氧羰基, 二硫氨酯, 合成

Abstract: The synthesis and research of thiocarbamate which contains two eater group and two acylamide group was reported. The intermediate N-ethoxylcarbonyl isothiocyanate was synthesized from ethyl chloroformate and sodium thiocyanate by nucleophilic substitution reaction and isomerization. Then using this intermediate with diols as raw materials, the target products N,N’-diethoxycarbonyl-O,O’-alkyl-dithionocarbamates were obtained by nucleophilic addition reaction. The compounds were characterized by elemental analysis, infrared spectrum, 1HNMR and 13CNMR. Small scale flotation experiments showed that, when the dosage of target compounds a~c was 6 g/t, the grade of Cu can reached to 6.12%, 6.35% and 5.92% respectively, the recovery of Cu can reached to 75.31%, 76.50% and 76.35% respectively, the dosage of each collector was far lower than butyl xanthate, while the grade and recovery were higher. So this kind of dithionocarbamates is suggested to be applied in the flotation of sulfur copper as a new collector.

Key words: Diethoxycarbonyl, dithiocarbamate, synthesis

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