应用化学

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二硅烷表面活性剂的合成与表面性能测定

王春光,于丽,张培龙,庞立飞,贾寿华*   

  1. (山东农业大学化学与材料科学学院 泰安 271018)
  • 收稿日期:2011-11-23 修回日期:2012-03-23 出版日期:2012-10-10 发布日期:2012-10-10
  • 通讯作者: 贾寿华,副教授; Tel:0538-8241570; Fax:0538-8242251; E-mail:shjia@sdau.edu.cn; 研究方向:精细化工产品开发

Synthesis and Property Determination of Disilane surfactant

WANG Chunguang, YU Li, ZHANG Peilong, PANG Lifei, JIA Shouhua*   

  1. (College of Chemistry and Material Science,Shandong Agricultural University,Taian 271018,China)
  • Received:2011-11-23 Revised:2012-03-23 Published:2012-10-10 Online:2012-10-10
  • Contact: jiashouhua

摘要: 合成了一种新型有机硅表面活性剂——聚醚改性二硅烷。 首先以(CH3)3SiCl和(CH3)2HSiCl为原料,金属钠作还原偶合剂,二甲苯作溶剂,用Wurtz偶合法合成了含氢二硅烷,对其结构进行了红外光谱、紫外吸收光谱和气相色谱表征,并确定了合成最佳反应条件:n((CH3)3SiCl)∶n((CH3)2HSiCl)=1.2∶1,反应物浓度为1.8 mol/L,助剂15-冠醚-5用量为总反应原料质量的2%,反应温度为80 ℃,反应时间为11 h。 再以合成的含氢二硅烷和甲基封端烯丙基聚醚(Mr=400)为原料,在Karstedt铂催化剂作用下进行硅氢加成反应,合成了聚醚改性二硅烷表面活性剂,确定的合成反应最佳温度为95 ℃,时间为4 h;该表面活性剂的表面张力为22.49 mN/m,临界胶束浓度为0.9 g/L,在pH值为6.94和4.12的水溶液中,具有良好的水解稳定性。

关键词: 有机硅表面活性剂, 含氢二硅烷, 聚醚, 水解稳定性

Abstract: A novel organic silicon surfactant, polyether modified disilane, was prepared via a two-step reaction. The hydrogen-containing disilane was first prepared by (CH3)3SiCl and (CH3)2HSiCl based on Wurtz coupling method using sodium as the reductive coupling agent and xylene as the dissolvant, and the obtained product was characterized by IR, UV and GC. The optimum experiment conditions of the synthesis were as follows:n((CH3)3SiCl)∶n((CH3)2HSiCl)=1.2∶1, the concentration of reactants with 1.8 mol/L, 15-crown-5 dosage with 2% of the reaction materials, the reaction temperature and time were 80 ℃ and 11 h, respectively. The polyether modified disilane surfactant was then synthesized via hydrosilation of the obtained hydrogen-containing disilane and methoxy-terminated polyether polyols using Karstedt Pt as catalysts, the experiment conditions of the synthesis were as follows: the reaction temperature was 95 ℃ and the reaction time was 4 h. Experimental results showed that the critical micelle concentration(CMC) was 0.9 g/L and the surface tension was 22.49 mN/m. The hydrolytic stability of product was good under pH=6.94 and pH=4.12 conditions.

Key words: organosilicone surfactant, hydrogen-containing disilane, polyether, hydrolytic stability

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