Catalyst Preparation For Ammoxidation Of 3-Piconline & Pilot Process Research

3-cyanopyridine is an important intermediate in the synthesis of pesticide, medicine, fodder etc. At present the main synthesis method of 3-cyanopyridine is 3-picoline ammoxidation on the industrial. The key technologies include catalyst preparation, equipment design and production process.This thesis aims at achieving industrialization of 3-picoline ammoxidation, and targeting on above three technologies, including preparation of catalyst suitable for industaialization, building pilot plant, optimum production process.Preparation of catalyst includes choosing catalyst carrier, loading appropriate active component and characterization for catalysts etc. The result shows:when the catalyst made by the catalyst scarrier containing 18.5% Si, particle size (5 mm), a specific surface area (less than 50 m2/g), pore diameter (10-120 nm) and vanadium pentoxide(10.1%), the yield of 3-cyanopyridine is above 60%.In the pilot plant, reactor is fixed bed reactor, absorption tower is packed tower, and pipelines were made by stainless steel and carbon steel. This pilot plant is stable and similar with the equipment used in industrial, and the flow rate of 3-picoline reached 200 g/h. Many kinds of catalysts have been evaluating with this pilot plant. At last No.6 catalyst was found to be best.The 3-piclone ammoxidation can be influenced by several factores including material concentration, catalyst load, residence time, temperature of the molten salt, absorption time etc. The result showed that when the flow rate of 3-picoline was 171 g/h, total flow of material was 3080 g/h, the temperature of molten salt was 370 ℃, the concentration of ammonia, oxygen, water was 2%,6% and 3.4% respectively, residence time was 2.4 s and absorption time was 2 h, the conversion of 3-picoline achieved 98.1% and the yield of 3-cyanopyridine achieved 83%.The process of manufacturing 3-cyanopyridine was designed on the basis of pilot experimental reslut. Some facilities were designed simply. And material balance was also carried on.