应用化学

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室温合成二硫化二正丁基黄原酸酯及其表征

曾燕飞,周元林*   

  1. (四川省非金属复合与功能材料重点实验室-省部共建国家重点实验室培育基地,
    [JZ]西南科技大学材料科学与工程学院 绵阳 621010)
  • 收稿日期:2013-11-27 修回日期:2014-04-16 出版日期:2014-09-03 发布日期:2014-09-03
  • 通讯作者: 周元林,教授; Tel:0816-2419631; E-mail:zyl603@163.com; 研究方向:高分子复合材料
  • 基金资助:
    国家自然科学基金委员会-中国工程物理研究院联合基金(11176026)资助项目

Room Temperature Synthesis and Characterization of Dibutyl Xanthate Disulfide

ZENG Yanfei, ZHOU Yuanlin*   

  1. (State Key Laboratory Cultivation Base for Nonmetal Composite and Functional Materials;
    School of Materials Science and Engineering,
    Southwest University of Science and Technology,Mianyang 621010,China)
  • Received:2013-11-27 Revised:2014-04-16 Published:2014-09-03 Online:2014-09-03
  • Contact: yuanlin zhou

摘要: 以正丁醇、氢氧化钠和二硫化碳为原料,水作溶剂合成正丁基黄原酸钠,再与一氯化硫反应,室温条件下合成对称的二硫化二正丁基黄原酸酯,并探讨了反应条件对合成正丁基黄原酸钠和二硫化二正丁基黄原酸酯产率的影响。 通过红外(FT-IR)、核磁(1H NMR)、质谱(MS)及元素分析等技术手段确定了产物的结构。 优化的合成条件为:n(正丁基黄原酸钠)∶n(S2Cl2)=2∶1.1,温度为室温,溶剂为THF,反应时间为2 min,产率可达83.2%,反应条件温和,反应迅速、收率高。

关键词: 正丁基黄原酸钠, 二硫化二正丁基黄原酸酯, 促进剂, 合成, 表征

Abstract: Sodium n-butylxanthate obtained from n-butyl alcohol, sodium hydroxide and carbon disulfide in water was converted to symmetrical dibutyl xanthate disulfide by reacting with disulfur dichloride(S2Cl2) at room temperature. The effects of reaction conditions on the yields of the sodium nbutylxanthate and dibutyl xanthate disulfide were investigated respectively. Characterizations of dibutyl xanthate disulfide were done using Fourier transform infrared(FT-IR) spectroscopy, 1H nuclear magnetic resonance(1H NMR)spectroscopy, mass spectroscopy(MS) and elemental analysis techniques. In optimized reaction conditions, the molar ratio of sodium n-butylxanthate to S2Cl2 is 1∶1.1 in THF solvent. The reaction completes within 2 min at room temperature to give up to 83.2% yield.

Key words: sodium n-butyxanthate, dibutyl xanthate disulfide, accelerant, synthesis, structure characterization

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