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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。
With hexafluoropropylene trimer and sodium p-hydroxybenzenesulfonate as main raw materials, sodium perfluorononenoxy benzene sulfonate was synthesized. The effects of reaction temperature, catalyst and feeding method on the yield of sodium perfluorononenoxybenzenesulfonate were investigated. The optimum technological conditions were determined by orthogonal experiments: the reaction temperature was 66 ℃, the reaction time was 4 h, and the catalyst triethylamine was fed into the solution of sodium p-hydroxybenzenesulfonate in N, N-dimethylformamide (DMF) After completely dissolved, the catalyst was added, then the hexafluoropropylene trimer was added dropwise, yielding 80.15%. The structure of the product was confirmed by FTIR and 19F NMR. The thermal decomposition temperature was measured by TG at 350-360 ℃. The results of surface activity measurement showed that the critical micelle concentration was 9.26 × 10-4mol / L and γCMC was 18.95 mN / m 20 ° C). Rubber demoulding application experiments found that when the mold release agent of sodium perfluorononethoxy benzene sulfonate mass fraction of 4%, the number of demoulding 43 times.