摘要
巯丙基三乙氧基硅烷作为一种重要的硅偶联剂,主要有溶剂法和水相法两种合成工艺。针对现有工艺中存在的有机溶剂用量大、产物易水解等不足,以γ-氯丙基三乙氧基硅烷和硫氢化钠的结晶水合物为原料,采用微水法合成γ-巯丙基三乙氧基硅烷。通过控制变量的方法分别考察了两种原料的投料比、熔融温度、反应时间和相转移催化剂对反应的影响。优化后的微水法合成工艺条件为:γ-氯丙基三乙氧基硅烷与硫氢化钠的结晶水合物的物质的量之比为1.0∶1.6,加入2%(质量分数,相对于γ-氯丙基三乙氧基硅烷)的四丁基溴化铵,在75℃下反应2 h,能以94%的收率分离得到γ-巯丙基三乙氧基硅烷。通过红外光谱、核磁共振氢谱和核磁共振硅谱对产物进行了表征,产物的核磁纯度可达99%以上。
The presence of water leading to deactivation of copper based catalysts is a prominent issue that limits the development of industrial applications for carbon dioxide hydrogenation to methanol.The solution for developing hydrophobic catalysts has the advantages of low cost and simple industrial operation.A series of hydrophobic catalysts with a maximum hydrophobic angle of 119°were synthesized by introducing different amounts of hydrophobic material(stearic acid)into the catalyst system.By XRD,TEM,adsorption and desorption of N2,H2-TPR,CO_(2)-TPD,in situ infrared spectroscopy and other characterization methods were used to analyze and characterize the catalyst,and the data showed that the introduction of an appropriate amount of stearic acid did not have a significant effect on the crystal structure of the catalyst.On the contrary,the introduction of an appropriate amount of stearic acid not only increased the hydrophobicity of the catalyst,but also enhanced its specific surface area and hydrogen adsorption capacity.The result of activity evaluation showed a significant improvement in the conversion rate of carbon dioxide,and the structure of the heat-resistant catalyst remained unchanged.This work provides an idea and direction for the development of hydrophobic catalysts.
作者
齐官军
乐治平
YU Yang(Sinopec Nanjing Chemical Industry Research Institute Co.,Ltd.,Nanjing 210048,China)
出处
《合成化学》
2025年第6期417-422,共6页
Chinese Journal of Synthetic Chemistry
作者简介
第一作者:齐官军(1986-),男,汉族,江西上饶人,硕士研究生,主要从事有机硅材料的开发和运用研究,E-mail:qiguanjun2008@126.com;通讯作者:乐治平,博士,教授,E-mail:zple@ncu.edu.cn。
