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采用热分解法制备的SnO2+Sb2O3/Ti作为阳极材料,以联二脲为原料,电化学氧化法合成出偶氮二甲酰胺。通过单因素实验和正交实验研究了电流密度、电量、NaBr的质量浓度和H2SO4的浓度以及反应温度对偶氮二甲酰胺的产率和电流效率的影响。得出最佳工艺条件:电流密度2 300 A/m2,电量12 350 C,NaBr的质量浓度和H2SO4的浓度分别为8 g/L和1.47 mol/L,温度40℃。在最佳条件下,偶氮二甲酰胺的产率达94%,质量分数97%,电流效率89%。此外,SnO2+Sb2O3/Ti电极在NaBr和H2SO4的溶液中的循环伏安测试结果表明,吸附溴原子Brad复合成溴的步骤控制电合成偶氮二甲酰胺的反应速度。整个电极过程包括电子转移及后续的化学反应(EC机理)。
Thermal decomposition method was used to prepare SnO2 + Sb2O3 / Ti as the anode material, and the biuret was used as the raw material to synthesize azodicarbonamide by electrochemical oxidation. The effects of the current density, the amount of electricity, the concentration of NaBr, the concentration of H2SO4 and the reaction temperature on the yield and current efficiency of azodicarbonamide were investigated by single factor experiments and orthogonal experiments. The optimum technological conditions were as follows: current density 2 300 A / m2, power 12 350 C, concentration of NaBr and H2SO4 concentration of 8 g / L and 1.47 mol / L, respectively. Under the optimal conditions, the yield of azodicarbonamide is 94%, the mass fraction is 97% and the current efficiency is 89%. In addition, the cyclic voltammetry results of SnO2 + Sb2O3 / Ti electrode in NaBr and H2SO4 solution show that the step of adsorbing bromine atom Brad into bromine can control the reaction rate of azodicarbonamide. The entire electrode process includes electron transfer and subsequent chemical reaction (EC mechanism).