压热法合成甲基偶联双(烷基酚)  

Synthesis of Methylene Bisalkylphenols by Autoclave Process

作　　者：何志强[1] 朱宗利[1] 方云[1] 孙守双[1] 

机构地区：[1]江南大学化学与材料工程学院食品胶体与生物技术教育部重点实验室,江苏无锡214122

出　　处：《精细化工》2013年第2期144-148,共5页Fine Chemicals

基　　金："十一五"国家科技支撑计划项目(2007BAE52B01);江苏省精细石油化工重点实验室开放基金项目(KF0903);江南大学博士研究生科学研究基金(JUDCF09007)~~

摘　　要：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.

关 键 词：烷基酚 甲醛 草酸 缩合反应 压热法 GEMINI表面活性剂 

分 类 号：TQ423[化学工程]