压热法合成甲基偶联双(烷基酚)

Synthesis of Methylene Bisalkylphenols by Autoclave Process

在压热条件下以草酸催化烷基酚与甲醛的缩合反应合成甲基偶联双(烷基酚),并采用FTIR,ESI-MS,1HNMR等方法表征了目标产物结构。结果表明,与常压条件相比,压热条件使壬基酚转化率提升20%左右,甲基偶联双(壬基酚)的选择性提升10%左右。以单因素实验方法考察了催化剂用量、反应时间、反应温度及反应物料比对壬基酚与甲醛缩合反应的影响,通过优化进一步提升了壬基酚转化率,同时选择性达到92.1%。类似地,又以正交实验方法优化了甲基偶联双(十二烷基酚)的压热工艺。实验结果表明,压热法可以简便、廉价并高效率地合成甲基偶联双(烷基酚)。

Methylene bisalkylphenols were synthesized by condensation reaction from alkylphenol and formaldehyde through an oxalic acid-catalyzed autoclave process, and the target products were identified by means of IR, ESI - MS and ^1HNMR. The experimental results show that compared with normal pressure process, the autoclave process enabled the conversion of nonylphenol to increase by about 20% and the selectivity of methylene bisnonylphenol to be elevated by approximately 10%. The effects of catalyst dosage, reaction time, temperature and substrate molar ratio on the condensation reaction were investigated and the influence factors were optimized so that the conversion of nonylphenol was further improved and the selectivity of methylene bisnonylphenol was as high as 92. 1%. The condensation conditions for preparing methylene bisdodecylphenol through the autoclave process also were optimized by an orthogonal experiment. The experimental results show that the autoclave process is a facile, low-cost and efficient technology to synthesize methylene bisalkylphenols, the precursor of hydrophobic skeletons of Gemini surfactants.