草酸二丁酯的催化合成

Synthesis of dibutyl oxalate by catalyst

以草酸和正丁醇为原料,分别采用不同催化剂——对甲苯磺酸和强酸性阳离子交换树脂合成草酸二丁酯,用正交实验法研究了两种催化剂对该反应的催化性能;确定了各自的最佳合成条件。以对甲苯磺酸为催化剂,在醇酸比为4:1,催化剂用量15％,回流分水1h,以苯为带水剂的反应条件下,酯收率达 83．6％;以强酸性阳离子交换树脂为催化剂,在醇酸比3:1,催化剂用量10%,回流分水1．5h,以甲苯为带水剂的反应条件下,酯收率达89．5％,且催化剂可重复使用。

In this paper, with oxalic acid and n - butyl alcohol, dibutyl oxalate was synthesized by using p - toluene sulfonic acid and strong acid ionic exchange resin as catalysts. The catalytic activities and each optimal conditions were decided by orthogonal experiments. The yield of dibutyl oxalate was 83.6 % when the material ratio（acid/alcohol） 4： 1, p - toluene sulfonic acid content 15 %, reaction time 1 h and benzene as water taker. The yield of dibutyl oxalate was 89.5 % when the material ratio（acid/alcohol） 3：1, strong acid ionic exchange resin content 10%, reaction time 1.5h and toluene as water taker.The result showed that strong acid ionic exchange resin had higher catalytic activity and can be reused.