以间苯二胺为原料,与酰化剂甲酸反应制得中间体N,N'-二甲酰基间苯二胺,再以NABH4-I2为还原剂合成得到产品N,N'-二甲基间苯二胺,对合成工艺进行了优化,并分析了还原机理,化合物的结构经IR,1 H NMR和MS分析确定.该法原料易得,反...以间苯二胺为原料,与酰化剂甲酸反应制得中间体N,N'-二甲酰基间苯二胺,再以NABH4-I2为还原剂合成得到产品N,N'-二甲基间苯二胺,对合成工艺进行了优化,并分析了还原机理,化合物的结构经IR,1 H NMR和MS分析确定.该法原料易得,反应条件要求低,收率高且成本更低.展开更多
以Cu/Ni为主活性组分,γ-Al2O3球为载体,考察了Mn助剂对N,N-二甲基乙醇胺(DMEA)固定床连续催化胺化制备N,N,N',N'-四甲基乙二胺(TMEDA)催化剂性能的影响,并通过XRD、BET/BJH、H2-TPR、H2-TPD等对催化剂结构进行表征,结果表明,M...以Cu/Ni为主活性组分,γ-Al2O3球为载体,考察了Mn助剂对N,N-二甲基乙醇胺(DMEA)固定床连续催化胺化制备N,N,N',N'-四甲基乙二胺(TMEDA)催化剂性能的影响,并通过XRD、BET/BJH、H2-TPR、H2-TPD等对催化剂结构进行表征,结果表明,Mn能够抑制脱氢而促进加氢反应的发生,随着Mn含量的增加,选择性会提高,而活性相对会受到抑制,当n(Cu)∶n(Ni)∶n(Mn)=4∶1∶0.2时催化剂性能较佳。采用4Cu-1Ni-0.2Mn/γ-Al2O3球作为催化胺化催化剂,在反应温度为240℃,DMEA空速为0.15 h-1,胺醇摩尔比为1∶1,常压,氢速为30 m L/min时,DMEA转化率和TMEDA选择性分别达到92%和83%左右。展开更多
3,5-dimethyl phenyl isocyanate was prepared by the method of trichloromethyl chloroformate in 70% yield.New compound N,N′-di-(3,5-dimethyl)phenyl-3,6-dimethyl-1,4-dihydro-1,2,4,5-tetrazine-1,4-dicarboamide was synthe...3,5-dimethyl phenyl isocyanate was prepared by the method of trichloromethyl chloroformate in 70% yield.New compound N,N′-di-(3,5-dimethyl)phenyl-3,6-dimethyl-1,4-dihydro-1,2,4,5-tetrazine-1,4-dicarboamide was synthesized by reacting 3,5-dimethyl phenyl isocyanate and 3,6-dimethyl-1,6-dihydro-1,2,4,5-tetrazine.Its post-disposal method had been improved.yield being 30.8%.Byproduct 1,3-bis-(3,5-dimethyphenyl)-1,3-diazetidine-2,4-dione have not been reported,too.Their structures were conformed by IR, 1HNMR and elemental analysis.展开更多
文摘以Cu/Ni为主活性组分,γ-Al2O3球为载体,考察了Mn助剂对N,N-二甲基乙醇胺(DMEA)固定床连续催化胺化制备N,N,N',N'-四甲基乙二胺(TMEDA)催化剂性能的影响,并通过XRD、BET/BJH、H2-TPR、H2-TPD等对催化剂结构进行表征,结果表明,Mn能够抑制脱氢而促进加氢反应的发生,随着Mn含量的增加,选择性会提高,而活性相对会受到抑制,当n(Cu)∶n(Ni)∶n(Mn)=4∶1∶0.2时催化剂性能较佳。采用4Cu-1Ni-0.2Mn/γ-Al2O3球作为催化胺化催化剂,在反应温度为240℃,DMEA空速为0.15 h-1,胺醇摩尔比为1∶1,常压,氢速为30 m L/min时,DMEA转化率和TMEDA选择性分别达到92%和83%左右。
文摘3,5-dimethyl phenyl isocyanate was prepared by the method of trichloromethyl chloroformate in 70% yield.New compound N,N′-di-(3,5-dimethyl)phenyl-3,6-dimethyl-1,4-dihydro-1,2,4,5-tetrazine-1,4-dicarboamide was synthesized by reacting 3,5-dimethyl phenyl isocyanate and 3,6-dimethyl-1,6-dihydro-1,2,4,5-tetrazine.Its post-disposal method had been improved.yield being 30.8%.Byproduct 1,3-bis-(3,5-dimethyphenyl)-1,3-diazetidine-2,4-dione have not been reported,too.Their structures were conformed by IR, 1HNMR and elemental analysis.
