摘要
该文以4,4′-二苯甲烷二胺(MDA)与碳酸二甲酯(DMC)为原料合成4,4′-双(二甲氨基)二苯甲烷(MBDMA)。用不同类型催化剂对反应过程中甲氧羰基化和甲基化反应进行了调控。NaY分子筛催化剂促进甲基化反应的发生,适宜的反应条件为:催化剂用量m(NaY)∶m(DMC)=0.07∶1,反应物配比n(DMC)∶n(MDA)=30∶1,反应温度190℃,反应时间6 h,此时MDA完全转化,MBDMA选择性达97%。相反,乙酸锌催化剂则促进甲氧羰基化反应的进行。用高效液相色谱/质谱联用技术(HPLC/MS)对NaY催化下反应副产物的结构进行了分析,发现生成的副产物主要为3种不同程度的N-甲基化产物,表明MBDMA生成是经过逐步甲基化完成的。
4,4′-Methylene bis（N,N-dimethylanline）（MBDMA） was synthesized from 4,4′-methylenedianiline（MDA） and dimethyl carbonate（DMC）.The methylation and methoxycarbonylation reactions between MDA and DMC can be regulated by using catalysts of different types.NaY zeolite promoted the methylation reaction and the optimum reaction conditions were：m（NaY）∶m（DMC）=0.07∶1,n（DMC）∶n（MDA）=30∶1,reaction temperature 190 ℃ and reaction time 6 h.MDA was totally converted while the selectivity to MBDMA reached 97%.In contrast,zinc acetate promoted the methoxycarbonylation reaction.The by-products formed during the reaction catalyzed by NaY were analyzed by HPLC/MS.It was found that the by-products mainly consisted of three N-methylated derivatives with different degrees of N-methylation,indicating that MBDMA was produced by stepwise N-methylation.
出处
《精细化工》
CAS
CSCD
北大核心
2008年第8期821-824,共4页
Fine Chemicals
基金
中国科学院知识创新工程青年人才领域前沿项目(2007YQNRC04)资助~~
