节点文献
FeCl3·6H2O/C催化水合肼还原制备2,2-二(4-羟基-3-氨基)苯基丙烷
Synthesis of 2.2-Bis(4-hydroxy-3-amido-phenyl)-propane Catalyzed by the FeCl3·6H2O/C Catalyst with Hydrazine Hydration
【摘要】 以ω(Fe)=5%的FeCl3·6H2O/C为催化剂,用ω(NH2NH2)=80%的水合肼,在乙醇溶剂中将2,2-二(4-羟基-3-硝基)苯基丙烷还原成为阻燃剂的中间体2,2-二(4-羟基-3-氨基)苯基丙烷.实验条件:用0.3g的催化剂(每10mmol反应物),反应物与水合肼的摩尔比为1∶4.5,控制反应温度为70℃,反应时间为3.5h,目标产物的产率为93.0%,纯度为98.5%,考察9种金属离子对催化活性的影响.结果表明:Pb2+会引起催化剂中毒;Mg2+、Cu2+和Zn2+钝化了催化剂的催化活性;Ba2+和Cr3+对反应几乎不影响;只有Al3+、Ni2+、Ti4+3种离子能活化催化剂,从而使反应速度加快,但这3种金属离子单独作为催化剂时都没有催化活性.
【Abstract】 Catalyzed by the FeCl3·6H2O/C catalyst [w(Fe)=5%] with hydrazine hydration [w(NH2NH2)=80%], 2.2-Bis(4-hydroxy-3-nitro-phenyl)-propane was reduced in the alcohol solvent to 2.2-Bis(4-hydroxy-3-amido-phenyl)-propane which is an intermediate of fire-retardants. The results show that the best condition of the reduction is that the catalyst is 0.3 g (10 mmol reactant), the mole scale of reactant and hydrazine hydration is 1∶4.5, the temperature should be 70℃, the test hour is 3.5 h , the yield is 93.0% and the purity is 98.5%. We have even made a study of the nine kinds of metal ions to learn what influence they could make on catalyst activity. The results show that Pb2+ can cause the catalyst to be poisoned; that Mg2+, Cu2+ and Zn2+ blunt the activity of catalyst; that Ba2+ and Cr3+ can hardly affect the activity of catalyst; and that Ni2+, Al3+ and Ti4+ can activate the activity of catalyst and quicken the reaction rapidly. But none of Ni2+, Al3+ and Ti4+ has any catalytic activity to the reaction when they are used as catalyst alone.
- 【文献出处】 中南林学院学报 ,Journal of Central South Forestry University , 编辑部邮箱 ,2004年04期
- 【分类号】O625
- 【被引频次】12
- 【下载频次】400