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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

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【作者】 周莹易友宾赵芳何丽芳马锁胡峥荣孙汉洲

【Author】 ZHOU Ying~1, YI You-bing~2, ZHAO Fang~1, HE Li-fang~3, MA Suo~3, HU Zheng-rong~3, SUN Han-zhou~1 (1. Research Institute of Applied Chemistry, CSFU, Zhuzhou 412006, Hunan, China; 2. Xinjiang Tulufan Experiment School, Tulufan 838000, Xinjiang, China; 3. School of Industry, CSFU, Zhuzhou 412006, Hunan, China)

【机构】 中南林学院应用化学研究所新疆吐鲁番实验中学中南林学院工业学院中南林学院应用化学研究所 湖南株洲412006新疆吐鲁番838000湖南株洲412006湖南株洲412006湖南株洲412006

【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
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