西南石油大学学报(自然科学版) ›› 2011, Vol. 33 ›› Issue (3): 154-158.

• 油气化学工程 • 上一篇    下一篇

Dawson 型磷钼钒过渡金属盐催化氧化苯制苯酚

李贵贤1 陈光1,2 高云艳1 马建军2 张雪梅1
  

  1. 1. 兰州理工大学石油化工学院,甘肃兰州730050
    2. 甘肃银光聚银化工有限公司,甘肃白银730900
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2011-06-20 发布日期:2011-06-20

The Catalytic Oxidation of Benzene to Phenol over Transition Metallic Molybdovanadophosphoric Heteropoly with Dawson-type

LI Gui-xian 1 CHEN Guang 1,2 GAO Yun-yan 1 MA Jian-jun 2 ZHANG Xue-mei 1
  

  1. 1. College of Petrochemical Engineering, Lanzhou University of Technology,Lanzhou, Gansu 730050, China;
    2. Gansu Yinguang Juyin Chemical Company Limited, Baiyin, Gansu 730900, China
  • Received:1900-01-01 Revised:1900-01-01 Online:2011-06-20 Published:2011-06-20

摘要:

摘要:采用酸碱中和法制备了一系列Dawson 型磷钼钒过渡金属盐MH6P2Mo16V2O62(M=Mn、Co、Ni、Zn),用IR、TG、XRD 对杂多酸盐进行结构物相分析,并将其用于苯氧化制苯酚的反应中,系统考察了反应介质、反应温度、反应时间、氧化剂用量、催化剂类型及用量对苯羟基化反应的影响。实验结果表明:4.395 g(5 mL)苯在催化剂NiH6P2Mo16V2O62 用量0.176 g,溶剂乙腈25 mL,10 mL30% H2O2,65 ℃条件下回流反应6 h,经气相色谱定性定量分析,苯的转化率达到47.3%,苯酚选择性为91.69%。

关键词:

苯, 苯酚, 过渡金属, 杂多酸, 羟基化

Abstract: A series of MH6P2Mo16V2O62(M=Mn, Co, Ni, Zn)are produced by the principle of acid alkali neutralization. Structure phase for heteropoly acid salt is analyzed by way of Fourier transform infrared spect roscopy (FT-IR), X-ray diffraction(XRD), thermal analysis(TG), and is put into practice in the reaction in which Benzene oxidation produces phenol. The reaction medium, reaction temperature, reaction time, the amount of the oxidizer, the kind and dosage of catalyst, and the influences of Benzene hydroxylation on reaction are studied systemically. Experimental results show that 4.395 g(5 mL)benzene in catalyst NiH6P2Mo16V2O62 is 0.176 g, solvent acetonitrile 25 ml, 30 percent of H2O2 10 mL, and that under the condition of 65 ℃reflux reacts after six hours. Percent conversion of benzene up to 47.3 percent, and selectivity of phenol is up to 91.69 percent, according to the analysis of qualitative and quantitative gas chromatography.

Key words: benzene, phenol, transition metal, heteropoly acid salt, hydroxylation

中图分类号: