Dawson型磷钼钒过渡金属盐催化氧化苯制苯酚

THE CATALYTIC OXIDATION OF BENZENE TO PHENOL OVER TRANSITION METALLIC MOLYBDOVANADOPHOSPHORIC HETEROPOLY WITH DAWSON-TYPE

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%。

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 Benzeneoxidation 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 acetonitrile25 ml,30 percent of H2O2 10 mL,and that under the condition of 65 ℃reflux reacts after six hours.Percentconversion of benzene up to 47.3 percent,and selectivity of phenol is up to 91.69 percent,according to the analysisof qualitative and quantitative gas chromatography.