摘要
以阳离子交换树脂-FeCl3络合物为催化剂、丁二酸和正丁醇为原料,采用负压酯化技术合成丁二酸二丁酯。考察了反应温度、原料配比、催化剂用量和反应时间等因素对酯化反应的影响,通过正交试验得到了最佳酯化反应工艺条件:n(正丁醇)∶n(丁二酸)为3.0∶1、w(催化剂)为1.5%、反应温度<125℃、反应时间3h;在该条件下丁二酸的转化率达到98.6%。催化剂重复使用6次后,丁二酸的转化率达到97.6%。利用红外光谱、色谱-质谱对产品进行分析。
Dibutyl succinate was synthesized from succinic acid and n-butyl alcohol using a complex of cation exchange resin with ferric chloride as catalyst, and a negative-pressure esterification technique. The effects of reaction conditions were investigated, including reaction temperature, mole ratio of n-butyl alcohol to succinic acid, catalyst content, and reaction time. Using an orthogonal experimental design, optimum reaction conditions were identified as an n-butyl alcohol to succinic acid ratio of 3.0：1, catalyst content of 1.5% of the total mass of succinic acid and n-butyl alcohol, reaction temperature of 398°K, and reaction time of 3.0 h. Conversion of succinic acid reached 98.6%, and activity of the catalyst remained at 97.6% even after six uses. The product was analyzed by FTIR and GC-MS.
出处
《农药》
CAS
北大核心
2006年第6期399-401,共3页
Agrochemicals
