全氟代壬烯氧基苯磺酸钠的合成、表征与应用
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Synthesis,characterization and application of Sodium p-perfluorous nonenoxybenzene sulfonate
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    摘要:

    摘要:以六氟丙烯三聚体和苯酚磺酸钠为主要原料,合成了全氟代壬烯氧基苯磺酸钠。考察了反应温度、催化剂和投料方式对全氟代壬烯氧基苯磺酸钠收率的影响;通过正交试验确定了最佳的实验反应条件:反应温度65℃、反应时间4h、催化剂三乙胺,投料方式为待苯酚磺酸钠在DMF中完全溶解后加入催化剂,再滴加六氟丙烯三聚体。在此条件下合成产物的最高收率可达80.15%。红外光谱(FTIR)和19F NMR表征结果显示,产物与全氟代壬烯氧基苯磺酸钠的结构完全符合,TG测出它的热分解温度为350~360℃;表面活性测定的结果表明,产物临界胶束浓度为0.058kg/m3,γcmc为18.95 mN/m(20℃)。橡胶脱模应用实验结果发现,当脱模剂中添加少量的全氟代壬烯氧基苯磺酸钠时,能很好地改善其脱模效果,脱模次数最大达到43次。

    Abstract:

    Abstract: Sodium p-perfluorous nonenoxybenzene sulfonate was synthesized by the reaction of hexafluoropropylene trimer and sodium phenolsulfonate. The effects of reaction temperature,catalysts and the way of feeding was investigated.The experimental scheme was optimized by means of orthogonal test. The best reaction conditions was that it reacts four hours at 66℃ in the presence of Et3N, adding catalyst after sodium phenolsulfonate was completely dissolved in DMF,then adding drops of hexafluoropropylene trimer. The yield of the product reached maximum at this condition .The maximum value was 80.15%. The molecular structure of the product was identified by IR and 19NMR spectra,which show that it was in accord with sodium p-perfluorous nonenoxybenzene sulfonate. Its decomposition temperature was 350~360℃,which was provide by TG. The results of the surface activity determination show that the surface tension(γcmc)of the product at critical micelle concentration (CMC)was18.95 mN/m(20℃) and the value of CMC was 0.058kg/m3.In the end,it was added in to releasing agent to do stripping experiment. The results found that adding a little bit of sodium p-perfluorous nonenoxybenzene sulfonate can well improve its stripping effect. The biggest number of stripping reached to 43 times.

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曹友桂.全氟代壬烯氧基苯磺酸钠的合成、表征与应用[J].精细化工,2012,29(2):

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  • 收稿日期:2011-11-07
  • 最后修改日期:2011-12-08
  • 录用日期:2011-12-15
  • 在线发布日期: 2012-01-09
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