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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)。
Methyl-coupling bis (alkylphenol) was synthesized by the condensation reaction of alkylphenol and formaldehyde with oxalic acid under an autoclaved condition. The structure of the target product was characterized by FTIR, ESI-MS and 1HNMR. The results showed that under the condition of pressureless heating, the conversion of nonylphenol was increased by about 20% and the selectivity of methyl-coupled bis (nonylphenol) was improved by about 10% compared with that under atmospheric pressure. The effects of catalyst dosage, reaction time, reaction temperature and the ratio of reactants on the condensation reaction of nonylphenol with formaldehyde were investigated by single factor experiment. The conversion of nonylphenol was further improved with the selectivity reaching 92.1%. Similarly, the autoclave process of methyl-conjugated bis (dodecylphenol) was optimized by orthogonal experiment. The experimental results show that the autoclave method can synthesize methyl-conjugated bis (alkylphenol) easily, cheaply and efficiently.