全氟代壬烯氧基苯磺酸钠的合成、表征与应用

以六氟丙烯三聚体和对羟基苯磺酸钠为主要原料,合成了对全氟壬烯氧基苯磺酸钠。考察了反应温度、催化剂和投料方式对对全氟壬烯氧基苯磺酸钠收率的影响。通过正交实验确定了最佳工艺条件:反应温度66℃、反应时间4 h、催化剂三乙胺,投料方式为待对羟基苯磺酸钠在N,N-二甲基甲酰胺(DMF)中完全溶解后加入催化剂,再滴加六氟丙烯三聚体,产物收率达80.15%。经FTIR和19FNMR确证了产物结构,TG测出它的热分解温度为350～360℃;表面活性测定结果表明,产物临界胶束浓度为9.26×10-4mol/L,γCMC为18.95 mN/m(20℃)。橡胶脱模应用实验发现,当脱模剂中对全氟壬烯氧基苯磺酸钠的质量分数为4%时,脱模次数达43次。

Synthesis,characterization and application of Sodium p-perfluorous nonenoxybenzene sulfonate

Sodium p-perfluorous nonenoxybenzene sulfonate was synthesized by the reaction of hexafluoropropylene trimer with sodium p-hydroxybenzene sulfonate.The effects of reaction temperature,catalysts and the way of feeding were investigated.The experimental scheme was optimized by means of orthogonal test.The optimum reaction conditions were ascertained as follows:effecting the reaction for four hours at 66 ℃ in the presence of Et3N,adding catalyst after sodium p-hydroxybenzene sulfonate was completely dissolved in DMF,then adding drops of hexafluoropropylene trimer.The optimum yield of the product reached 80.15%.The molecular structure of the product was identified by means of IR and 19FNMR spectra.TG analysis shows that its decomposition temperature was 350～360 ℃.The results of the surface activity determination show that the surface tension(γCMC) of the product was 18.95 mN/m(20 ℃) at critical micelle concentration(CMC) with a value of 9.26×10-4 mol/L.The application experiments of rubber stripping have found that,when the quality of sodium p-perfluorous nonenoxybenzene sulfonate in releasing agent was 4%,the number of stripping reached 43 times.