TBAB催化碳酸乙烯酯与苯酚合成苯氧乙醇

TBAB Catalyzed Synthesis of Phenoxyethanol From Ethylene Carbonate and Phenol

开发一种无溶剂、催化剂用量低、原料转化率高和产品选择性好的苯氧乙醇合成工艺具有重要意义。研究了以四丁基溴化铵(TBAB)为催化剂,用苯酚和碳酸乙烯酯为原料合成苯氧乙醇,考察了碳酸乙烯酯和苯酚的物料比、催化剂用量、反应温度和反应时间等工艺参数对合成苯氧乙醇的影响,得出最优工艺条件:碳酸乙烯酯和苯酚的物质的量之比为1.05、TBAB用量为苯酚质量的1%、反应温度为145℃、反应时间为4.5 h。在此条件下,苯酚的转化率为99.77%、苯氧乙醇的选择性为99.08%,对反应液进行分离纯化,可得到高纯度苯氧乙醇。采用GC-MS对反应液定性分析,发现除产物外只产生了4种副产物,GC内标法对反应液中苯酚和产物进行定量测定。

Developing a solvent-free,low catalyst usage,high raw material conversion rate,and good product selectivity synthesis process for benzyl alcohol is of great significance.The synthesis of phenoxyethanol from phenol and ethylene carbonate using TBAB as a catalyst was studied.The effects of material ratios of ethylene carbonate and phenol,catalyst dosage,reaction temperature,and reaction time on the synthesis of phenoxyethanol were studied.The optimal process conditions were obtained as follows:the molar ratio of ethylene carbonate to phenol was 1.05,the amount of TBAB was 1%of phenol mass,the reaction temperature was 145℃,and the reaction time was 4.5 hours.Under these conditions,the conversion rate of phenol is 99.77%and the selectivity of phenoxyethanol is 99.08%.By separating and purifying the reaction solution,high-purity phenoxyethanol can be obtained.Qualitative analysis of the reaction solution was conducted using GC-MS,and it was found that only four by-products were produced except for the products.The GC internal standard method was used to quantitatively determine phenol and products in the reaction solution.