摘要
以邻二氯苄为原料,在乙醇/水体系中经过Na_2CO_3水解,合成了邻苯二甲醇。考察了水醇体积比、反应原料摩尔比、反应时间以及反应温度对产品收率的影响,确定了最佳反应条件。通过红外光谱对产物进行了结构表征,利用高效液相色谱测定了产品的纯度。结果表明:在水醇体积比5∶1的体系中,在反应时间8 h、反应温度90℃、邻二氯苄与无水碳酸钠摩尔比为1∶1.3的最佳反应条件下,合成的邻苯二甲醇收率可达86%,纯度(w)达98%。该工艺操作简单、反应条件温和、成本低,有利于工业化生产。
O-benzenedimethanol is synthesized by hydrolysis of 1,2-bis( chloromethyl) benzene through Na_2CO_3 in ethanol and water system. The effects of the volume ratio of water and anhydrous ethanol,the mole ratio of reaction materials,the reaction time and the reaction temperature on the product yield are investigated and the optimum reaction conditions are determined. The structure of product is characterized by IR,and the purity is detected by HPLC. The results show that the yield of the o-benzenedimethanol can be up to 86% under the optimum conditions: the volume ratio of water and anhydrous ethanol is 5 ∶1,the reaction time is 8 h,the reaction temperature is 90 ℃,the molar ratio of o-dichlorobenzyl and anhydrous sodium carbonate is 1 ∶1. 3. The purity of the product is 98%.The synthetic process has advantages of simple operation,moderate reaction conditions and low cost,which is in favor of commercial process.
出处
《能源化工》
2016年第3期72-74,共3页
Energy Chemical Industry
关键词
邻二氯苄
水解
邻苯二甲醇
1
2-bis(chloromethyl) benzene
hydrolysis
o-benzenedimethanol