| Starting from o-phenylenediamine,4-Nitro-o-phenylenediamine,dimethyl malonic acid,oxalyl chloride,diethyl oxalate and Anhydrous metal chlorides etc,8 complex catalysts with transition metal as the central atom and 9 intermediates were synthesized through one or two steps.The influence of the reaction temperature,reaction time,rate of feeding,mode of feeding,control of anhydrous condition as well as the choice of solvent on the formation of product was studied and the synthetic routes were optimized.The intermediates and final product were characterized with NMR,MS and IR.4-Nitro-o-phenylenediamine with two different active amino can react with dimethyl malonyl chloride using DMA and THF as the solvents and target product was formed.The product can be conveniently separated from the reaction solution and the yields increased from 62.7%to 90.1%.12H4L was produced by the reaction of o-phenylenediamine and diethyl oxalate without using chloride.The reaction is simple and the yield is up to 90.1%.Different products were synthesized using different solvents to nitration12H4L.The research found that the two catalysts 14?Fe?and 13?Fe?can degraded the dyeing water using H2O2 as the oxidant.The effect of pH,time and concentration on the catalytic H2O2oxidative degradation of dyes with these efficient catalysts were explored.The degradation of Acid Blue 80 showed that the reaction rate of 14?Fe?and 13?Fe?reached the maximum value at about pH=10.And investigated the minimum required H2O2 degradation of certain dyes,14?Fe?is 10-2M and 13?Fe?is 0.5×10-2M.When the concentration of H2O2,dye and 13?Fe?were 10-2M,10-4M and 10-6M respectively,pH=10,the decolorizations in 10min for five dyes were Acid Blue80 100%,Gold Orange?100%,Alizarin Red S 78.91%,Acid Chrome Yellow GG 87.5%,Reactive Brilliant Red 34.6%;the rate of TOC removal were 49.2%,54.16%,39.0%,43.1%and30.9%respectively.Study the catalytic H2O2 oxidative degradation of the concentration of phenol model were10-4M,5×10-4M,and 10-3M respectively with 13?Fe?as the catalyst,the rate of degradation were 40.5%,37.9%and 33.0%. |
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