利用二级管式反应器耦合渗透分离装置,以对苯二甲酸(PTA)和正丁醇为原料,在高温、高压条件下不使用催化剂实现对苯二甲酸二丁酯(DBT)的连续制备。考察了反应温度、压力、停留时间、醇酸摩尔比等对最终二级酯化产物收率的影响。结果表明,当反应温度为360℃、反应压力为16 MPa、反应停留时间为25 min、醇酸摩尔比为30∶1时,原料PTA一级酯化转化率达到90.06%,目标产物DBT收率达到66.14%;二级酯化原料转化率达到99.03%,目标产物DBT收率达到84.18%。

The continuous preparation of dibutyl terephthalate (DBT) is realized by using a two-stage tubular reactor coupled with a permeation separation unit,using terephthalic acid (PTA) and n-butanol as raw materials,not using a catalyst under high temperature and high pressure conditions.The influences of reaction temperature,pressure,residence time and alkyd-acid ratio on the yield of the final secondary esterification product are investigated.Results show that the first-order esterification conversion rate of PTA reaches 90.06%,and the yield of DBT reaches 66.14% when reaction temperature is 360°C,reaction pressure is 16 MPa,reaction residence time is 25 min,and alkyd-acid ratio is 30∶1.The conversion rate of secondary esterification raw materials reaches 99.03%,and the yield of DBT reaches 84.18%.

张宝忠(1971-),男,博士,高级工程师,研究方向为精细化工,通讯联系人,zhangbaozhong.tjsh@sinopec.com。