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[方法]利用中孔分子筛Al-MCM-41作催化剂,直接用反应物乙醇作带水剂,以乙醇和异戊烯酸为原料,采用分批补充乙醇的工艺方法合成农药异戊烯酸乙酯。考察了催化剂用量、反应物物质的量比、反应温度和反应时间对反应转化率和选择性的影响。[结果]该反应最佳的合成条件:异戊烯酸和乙醇的物质的量比为1∶8,催化剂的量为异戊烯酸质量的1.8%,反应时间为6 h,反应在剧烈回流温度下进行。在此条件下,异戊烯酸转化率可达89.9%,产品纯度大于99.7%。[结论]中孔分子筛Al-MCM-41可作为合成异戊烯酸乙酯高效而环保的固体酸催化剂。
[Method] The mesoporous molecular sieve Al-MCM-41 was used as the catalyst, the reactant ethanol was directly used as water-carrying agent, ethanol and isoprenoic acid were used as raw materials, ester. The effect of catalyst dosage, reactant mass ratio, reaction temperature and reaction time on the reaction conversion and selectivity was investigated. [Result] The optimal reaction conditions were as follows: the ratio of substance of pentenoic acid to ethanol was 1: 8, the amount of catalyst was 1.8% of the amount of pentenoic acid, the reaction time was 6 h, the reaction was under vigorous reflux Temperature. Under these conditions, the conversion of iso-pentenoic acid is up to 89.9% and the purity of the product is over 99.7%. [Conclusion] The mesoporous molecular sieve Al-MCM-41 can be used as an efficient and environmentally friendly solid acid catalyst for the synthesis of ethyl isoprenoidate.