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以草酸和异戊醇为原料,环己烷为带水剂,采用酸性化合物作为催化剂,合成草酸二异戊酯。考察了酸醇比、反应时间、催化剂用量和带水剂用量等因素对于酯化反应产率的影响。以对甲苯磺酸为催化剂的最佳反应条件为:草酸和异戊醇的物质的量比为1∶3,催化剂用量为草酸质量的2.5%,带水剂环己烷的用量为30mL/0.1mol草酸,反应时间为120min,反应的酯化率在95%以上。以硫酸氢钠为催化剂的最佳反应条件为:草酸和异戊醇的物质的量比为1∶2.5,催化剂用量为1.2g/0.1mol草酸,带水剂环己烷的用量为30mL/0.1mol草酸,反应时间为90min,反应的酯化产率可达93%。由该方法得到的草酸二异戊酯的酯化率和产品的纯度均较高,具有广泛的应用前景。
Using oxalic acid and isoamyl alcohol as raw materials, cyclohexane is a water-carrying agent, and acidic compounds are used as a catalyst to synthesize diisopentyl oxalate. The effects of acid-alcohol ratio, reaction time, the amount of catalyst and the amount of water-carrying agent on the yield of esterification reaction were investigated. The optimal reaction conditions for p-toluenesulfonic acid as catalyst are as follows: the molar ratio of oxalic acid to isoamyl alcohol is 1: 3, the amount of catalyst is 2.5% of oxalic acid, the amount of cyclohexane of water-carrying agent is 30mL / 0.1 mol oxalic acid, the reaction time is 120min, the esterification rate of the reaction is above 95%. The optimal reaction conditions of sodium bisulfate as catalyst are as follows: the molar ratio of oxalic acid to isoamyl alcohol is 1: 2.5, the amount of catalyst is 1.2g / 0.1mol oxalic acid, the amount of cyclohexane with water-entraining agent is 30mL / 0.1 mol oxalic acid, the reaction time is 90min, the reaction yield of esterification up to 93%. The esterification rate of diisoamyl oxalate obtained by the method and the purity of the product are high, and have wide application prospect.