摘要
以顺丁烯二酸酐和苯胺为原料,研究在催化剂作用下合成N-苯基马来酰亚胺(N-PMI)的新工艺,在N-苯基马来酰胺酸合成时采用乙酸已酯作溶剂,在N-PMI合成时采用乙二胺四乙酸(ED-TA)钠盐作为催化剂、醋酐作为脱水剂、丙酮作为溶剂,考察了原料配比、催化剂的选择及用量、反应温度与反应时间等因素对反应结果的影响,合成N-PMI的最佳工艺条件为:顺酐与苯胺质量比为1.06∶1.00,催化剂用量为0.35g/g中间体,反应温度为55℃,反应时间为4h。在最佳工艺下产品收率可达92%以上,产品纯度可达99%(质量分数)以上,并通过气相色谱检测了产品纯度,通过红外光谱对产品结构进行了表征。
The novel technology of the synthesis of N-phenylmaleimide under catalyst was studied by using maleic anhydride and aniline as starting materials. In the investigation, ethyl acetate was se- lected as solvent when the N-phenylmaleamic acid was synthesized. In addition, during the process of the synthesis of N-phenylmaleimide,edetate disodium,acetic anhydride and acetone were used as cata- lyst, dehydration reagent and solvent, respectively. The ratio of starting materials, the selection and dosage of catalysts,reaction temperature as well as the rection time were investigated in order to un- derstand their influences on the results. The optimized technological condition was that the mass ratio of maleic anhydride and aniline was 1.06 : 1, catalyst dosage was 0. 35 (g/g intermediates), the reac- tion temperature was 55 ℃ and the reaction time was 4 hours. Under such conditions, the yield and the purity were 92% and 99%, respectively. Besides, the purity was detected by GC, and the structure of product was identified by IR.
出处
《弹性体》
CAS
2013年第1期37-39,共3页
China Elastomerics
基金
吉林省科技厅科技发展计划基金项目(200705C12)