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阴离子表面活性剂聚二硫二丙烷磺酸钠的合成
引用本文:杨永,张敏,刘鸿雁,干建群,区菊花.阴离子表面活性剂聚二硫二丙烷磺酸钠的合成[J].广州化学,2013,38(1):7-13.
作者姓名:杨永  张敏  刘鸿雁  干建群  区菊花
作者单位:1. 中国科学院广州化学研究所,广东广州510650;中国科学院大学,北京100049
2. 中国科学院广州化学研究所,广东广州,510650
基金项目:广东省中科院全面战略合作项目(2011B090300003);广东省科技计划项目(2012B020308006)
摘    要:利用硫化钠与硫磺反应制备二硫化钠,然后将二硫化钠与1,3-丙磺酸内酯反应,合成了一种可作为电镀添加剂的阴离子表面活性剂——聚二硫二丙烷磺酸钠(SPS)。采用核磁共振氢谱对合成产物进行结构表征,确认了产物结构及产率。通过正交试验研究了产物产率与反应物配比、反应温度、溶剂加入量等因素之间的关系,找出了最优合成条件:第一步合成二硫化钠的反应中,硫化钠/硫磺物质的量比为1∶1.3,温度55℃,加水量18 mL;第二步合成SPS的反应中,1,3-丙磺酸内酯/硫化钠物质的量比为1.7∶1,温度40℃,溶剂量75 mL,产物的最高产率可达到95.8%。

关 键 词:阴离子表面活性剂  1  3-丙磺酸内酯  聚二硫二丙烷磺酸钠  正交试验  电镀添加剂

Synthesis of Anionic Surfactant Sodium 3,3’-Dithiodipropane Sulfonate
YANG Yong , ZHANG Min , LIU Hong-yan , GAN Jian-qun , OU Ju-hua.Synthesis of Anionic Surfactant Sodium 3,3’-Dithiodipropane Sulfonate[J].Guangzhou Chemistry,2013,38(1):7-13.
Authors:YANG Yong  ZHANG Min  LIU Hong-yan  GAN Jian-qun  OU Ju-hua
Institution:1,2(1.Guangzhou Institute of Chemistry,Chinese Academy of Sciences,Guangzhou 510650,China;2.University of Chinese Academy of Sciences,Beijing 100049,China)
Abstract:Anionic surfactants sodium 3,3'-dithiodipropane sulfonate (SPS) was prepared by reacting 1,3-propane sultone and sodium disulfide deriving from reaction sodium sulfide and sulfur. IH-NMR was applied to confirm the structure of product and calculate the yield. Effect of reaction conditions such as material ratio, temperature, and solvent amount etc on yield of SPS was investigated in detail. The optimum reaction conditions were as follows: the molar ratio of sodium sulfide and sulfur was 1 : 1.3, reaction temperature was 55℃ and water addition was 18 mL in first step. 1,3-propane sultone and sodium disulfide was 1.7 ; 1, reaction temperature was 40℃ and solvent quantity was 75 mL in second step. The yield of SPS as high as 95.8% was obtained by orthogonal experiment test.
Keywords:anionic surfactant  1  3-propane sultone  sodium 3  3'-dithiodipropane sulfonate  orthogonal experiment test  electroplating additive
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