| m-Aminophenol(MAP), who played an important role in arylamine derivatives. It has a widely applications in dye, medicine and farm chemical field as the synthetic intermediates, also in carbon, printer paper and photographic industry. With the rapid developed of chemical technology, it has been concerned that MAP's application in composite of super capacitor by international and domestic academics. Now dominating rote of preparing MAP is nitrobenzene sulfonated alkali fusion in China and India. But this rote caused serious waste and environment that restricted it cannot been produced in enormous quantities,even faced been eliminated. Based on domestic and foreign literatures, this paper proposed a rote of Bucherer catalytic aminolysis reaction of resorcinol, which had only water of by-product that can be used as cooling liquid, and focused on how to raise conversion ratio of resorcinol, selectivity of MAP and separate of the product.Influencing factors of resorcinol conversion ratio, selectivity of MAP was studied by single factor experiment. Results demonstrated that optimized conditions were:toluene as solvent, synthesis zeolite ZSM-5 as catalyst and the usage amount was 12.5g(100/8,8 times used repeatedly) per 110g resorcinol, optimum molar ration of ammonia and resorcinol was 2.4, optimum reaction temperature range was 210-220?and reactor pressure maintain 2.0 approximately as the time, 6 hours was the optimal process time. At this process condition, the conversion ratio of resorcinol can reach above 85% and selectivity of MAP can reach 83%.Research on main factors that affected product separating of resorcinol ammonolysis by stimulating the mixture in a scale proportion of resorcinol, MAP and m-phenylenediamine. Drawn a diagram of solubility in water of MAP in low temperature area(5?-25?). Determined UV detection wavelength that was 275nm by mensurating absorption wavelength of the pure product of the above three. Studied firstly on the extractant of resorcinol,as a result that the optimum extractant was butyl-acetate and the usage amount was three to four times of resorcinol. Than research on separating technology of MAP and m-phenylenediamine, in view of industry production cost and pollution, we determined the optimum conditions were:crystallization temperature as 15?, agitation speed in the range of 400-600 r/min, and crystallization for 40 min. At this crystallizing condition, the content of MAP in aqueous was low as 12.611ug/mL and had high purity of MAP.Macro reaction kinetic equation gave technical foundation to determine process parameter, select plant model selection, estimate and analysis energy consumption, etc. Therefore, the article explored and figure out kinetic equation of resorcinol ammonolysis in chapter forth. The result was that the macro kinetic equation was:rB= 20.905cA1.50918-3.8993cB 0.97733 at 210?,and rB=28.276cA 1.30947-4.5374cB0.94055 at 220?,than found the activation energy and pre-exponential factor of resorcinol ammonolysis according to Arrhenius equation,they were Ea?59.74kJ/mol and A?0.685 ×105.In the end of paper, drawn technological equipment flow chart and economic assessment of resorcinol ammonolysis process. During the production process,catalyst circulation using by added 20% catalyst in each charge, and surplus ammonia can be recycled through distillation tower. Finally, calculated that for a production line of 1000t MAP annually can gain profit 8.3 million yearly. |
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