柠康酸酐的最佳合成工艺研究

摘要

Citraconic anhydride ( CTA) was synthesized using itaconic acid. The effects of different factors on the synthesis process, dehydrating agent type and dosage, catalyst dosage and type, etc. , were analyzed, the orthogonal test was adopted. The results of orthogonal test showed that the best formulation and process conditions were as follows: the catalyst was N,N-dimethylformamide( DMF) , the amount was 0. 47 times of the itaconic acid ( w/w) , dehydration agent was o-dichlorobenzene, 3. 8 times dosage of itaconic acid ( w/w) , the yield was 95. 56%. The synthetic products were analyzed by IR and 1 H NMR, analysis results showed that the product was the target product.%以衣康酸为原料合成了柠康酸酐。对合成过程中的各种影响因素进行了详细的分析,对脱水剂类型及用量、催化剂类型及用量等进行了正交试验。正交试验结果显示：最佳配方及工艺条件为催化剂为N,N-二甲基甲酰胺( DMF),用量为衣康酸的0.47倍( w/w),脱水剂为邻二氯苯,用量为衣康酸的3.8倍( w/w),气相收率为95.56%。对合成产物进行了红外光谱和核磁氢谱分析,分析结果显示产品为目标产物。