Study Of Synthesis Of O-Phenylphenol From Cyclohexanone

o-Phenylphenol (OPP) is widely used in the fields of dyeing, antiseptics, assistantagent in dyeing, surface activator, flame retardant and thermal stabilizator as one of themost important fine chemical industrial products. In the fields of antiseptics, OPP can beused in the preservation of lumber, citrus and cosmetics, which effect can last for manyyears. In the field of dyeing, OPP is mainly used as the carrier assistant agent of dyeingand surface activator. In the aspect of surface activator, OPP, blended with liquidturpentine wood oil, can perform the function as cleanser and deodorant used in woodenfloor and door window. One kind of flame retardant prepared from OPP afterbromination exhibits excellent performance, which even reachs the level of (UV-94)V-O.Furthermore, some kind of varnish prepared from this compound show high stabilityagainst water and base. In addition, OPP can be used as the raw material to producenon-ion emulsifier and composite dyeing.OPP shows prospective future in many fields, including dyeing, lumberpreservation and information dyeing et al. However, the limited output limits theapplications and development in these fields. China's entrance to WTO offers thewonderful opportunity to the industry of textile. Our industry of textile is certain toselect the developing way of large scale and high quality. At the same time, our countryhas become the main country of producing the synthesized fiber in the world. Thesefactors offer a good developing space to OPP in the fields of dyeing as assistant agentwith high performance and high quality. In addition, because of the scarce of lumber inour country, it is very important to reasonably use, preserve lumber and prolong theperiod of using. Most of the lumber in our country has not been dealt with antisepsis. Sothe field of antisepsis using OPP is also a very important market with great developingpotential. Furthermore, one of the latest documents has introduced the wonderful marketprospect of the downstream products prepared with OPP. In this document, one kind offlame retardant prepared from OPP show excellent performance. In present, OPP is mainly obtained from the residue of phenol prepared withsulfonation method and the output is very small. On basis of the statistics, the demand ofOPP of our country is about 5000 ton/year and the output is no more than two hundred,which can't meet the demand of the domestic market greatly. With the development ofpetrol and chemical engineering, the technique of sulfonation method to produce phenol,owing to its low benefit, complicate technique and execrable operating environment, isdefinitely replaced by the technique of cumin method. On the other hand, the output ofcyclohexanone about 200,000 tons/year is far more than the domestic demand, soenlarging the fields of the products from cyclohexanone is very necessary. As one of themain product derived from cycloheanone, carrying out the research and explitation ofOPP, enlarging the application and extending sphere are very prospective. The main work focuses on the following aspects.1. We systematically studied the condensation reaction of cyclohexanone catalyzed by different catalyst. Among all the Br?nsted acid, HCl showed high catalytic performance, reaching 54% conversion and 89% selectivity to Dimer at 5wt.% loading and T = 137°C. of all the Lewis acids, Fe2(SO4)3 and FeCl3 also exhibited high activity. The solid sulfuric acid prepared by sol-gel method showed high activity and stability in the condensation reaction. The higher stability may be due to the presence of the relatively strong interaction between H2SO4 and the matrix of SiO2 in the catalyst synthesized by sol-gel method.2. We studied the influence of the synthesis conditions on the surface and structural properties of Al2O3 prepared by sol-gel method. The material showed higher specific surface area, better-defined pore size distribution and higher thermal stability compared with Al2O3 prepared by conventional precipitation method, which obtained high BET of 325 m2/g even calcined at 600°C. For Al2O3 prepared by the assistance of citric acid, the material showed higher homogeneity and thermal stability than that prepared by precipitation method. High specific surfacearea as 308 m2/g was achieved even after calcined at 700°C for 2 h.3. The effect of preparation conditions on the structural and catalytic properties of Pt/Al2O3 prepared by impregnation method was investigated by different methods. The synthesis and reaction condition greatly affected the activity and stability in the dehydrogenation reaction. The catalyst showed the highest performance as the following treatment: the catalyst was impregnated and aged in vacuum, then calcined at 600°C, and then reduced at 400°C for 2 h. 99.8% conversion of Dimer and 95.8% selectivity to OPP were obtained at the reaction condition: T = 350°C, Pd loading = 0.5% and LHSV = 0.33 h-1. Furthermore, the acetone conversion only declined from 99.8% to 92.5% and the selectivity to OPP decreased from 95.8% to 87.2% after 2000 h of time on stream, which was inferior to the best results in all the papers. This indicated that the 0.5%Pt/Al2O3 was effective and very stable for the synthesis of OPP from Dimer.4. We systematically studied the influence of synthesis conditions on the structural parameters of Pt/Al2O3 prepared by sol-gel methods. Some interesting results were found in the study of the reduced properties by TPR technique. Different from the catalyst prepared by impregnation method, the particles size was not increased obviously after the material was reduced, which can be attributed to the Pt-Al alloy during the reduction process. The catalyst showed higher thermal stability in the dehydrogenation reaction compared with Pt/Al2O3 prepared by impregnation method. This may be related to the special synthesis theory for this material.5. In the thesis, Hydrotalcites were synthesized by different methods at different conditions. Hydrotalcites synthesized by low supersaturation method showed higher crystallinity than those synthesized by high supersaturation method. The crystallinity was also affected by the crystallinity time and temperature. Hydrotalcites showed poorer crystallinity with the increment of crystallinity time and temperature. We also synthesized hydrotalcites with high crystallinity by using the decomposing property of urea at high temperature. The crystallinity and the regular degree of the samples were much preferable to those synthesized with other methods. HT lost its structure and transformed to Mg(O)Al compound after...