Study On Catalyst's Preparation And Properties For Synthesis O-Phenylphenol

Cyclohexenylcyclohexanone was prepared from cyclohexanone. o-Phenylphenol was made from cyclohexenyl cyclohexanone by dehydrogenation reaction. The noble metal (Pd or Pt) supported on HZSM-5 and r -Al2O3 or CCA respectively using as dehydrogenation catalysts were prepared. The factors that could influence catalysts' properties were studied by the numbers.Pd/HZSM-5 was prepared by method of iron-exchanged reaction, Pd could be dispersed better on the catalyst after deoxidizing. The cyclohexenylcyclohexanone conversion rate and the selectivity of OPP were more 95% and 90% respectively, while Pd/HZSM-5 catalyst in an amount of w(Pd) = 0.9%. K2SO4 or K2O as assistant agent were used for Pt supported by Y -Al2O3 catalyst. The results showed that: catalyst consist as [w(Pt)=0.3% w(K.2SO4)=2%], the initiative conversion rate of cyclohexenylcyclohexanone is more 96% and the yield of OPP is as high as 90% in a certain reaction condition ,which temperature is 350 C and flux of H2 is 50mL/min,adding rate is 7mL/h.CCA carrier was prepared by cyclohexene cracked to carbon compound over the r -Al2O3 under higher temperature 400C-650C. The amount of carbon-covered has linear relation with time when temperature is determined. With temperature rising, the total amounts of carbon-covered has exponential relation with temperature. Through BET surface structure analysis ,CCA has more SSA than that of Y -AI2O3 and it's pore diameter distributing is tend to equality. When the catalyst Pt/CCA [w(Pt)=0.5% w(K2O)=l%] was lasted used 100h,the dehydrogenation convert of rate for cyclohexenylcyclohexanone is 95%,and the selectivity of OPP keep stabilization. When the catalyst was pre-poisoned by CS2 which amount of CS2 be controlled under [m(CS2): m(Pt)=1:10] the yield of OPP is more 90% after lasted using 200h. The results of XPS analysis showed that the S 2P3 electron bring energy rose to 169ev from normal 165ev, it is possible that S has play participate to restrain H transfer in the process of dehydrogenation so as to reduce hydrogenolysis and promoteselectivity of OPP.OPP was refined by rectify and recrystal technology and purity add to 99.8%. DOPO and HPPA are synthesized with phosphorous trichloride and o-phenylphenol by an "one-pot" method without isolating intermediate products and avoiding a distillation step.