响应面法优化氧化锌中高温煤气脱硫剂的制备工艺

Optimization of the preparation technology of zinc oxide sorbent by response surface methodology for mid-high temperature coal gas desulfurization

通过优化制备工艺和制备条件,提高氧化锌脱硫剂的脱硫性能。以乙二酸和乙酸锌为原料,采用固相法制备了乙二酸锌前驱体;添加助剂和粘结剂后,通过微波焙烧制备了氧化锌中高温煤气脱硫剂。采用单因素法研究了微波功率、焙烧温度、焙烧时间以及活性组分质量分数对脱硫剂性能的影响,并利用响应面法探讨了各因素及其交互作用对脱硫剂穿透时间和硫容的影响,确定了氧化锌脱硫剂的最佳制备工艺:微波功率1 300 W,焙烧温度550℃,焙烧时间60 min,活性组分质量分数30%。采用回归分析法建立了回归模型,并通过试验验证了模型的可靠性。结果表明:模型预测值与实测值接近;焙烧温度、焙烧时间和活性组分质量分数对脱硫剂穿透时间有显著的影响;焙烧温度和焙烧时间、焙烧温度和活性组分质量分数二者的交互作用均比较显著。

The preparation technology and conditions are optimized to improve the desulfurization performance of zinc oxide desulfurizer. The precursor zinc oxalate is prepared via solid-phase reaction of zinc acetate and oxalic acid,and the sorbent is obtained by microwave calcining of the mixture of precursor,promoter and binder. The effects of microwave power,calcination temperature,calcination time and the mass fraction of active component on the desulfurization performance of the sorbent are studied through single factor experiments,and the interaction effects on the penetration time and sulfur capacity are discussed by response surface methodology. The optimum preparation conditions of the sorbent are determined： microwave power 1 300 W,calcination temperature 550 ℃,calcination time 60 min and the mass fraction of active component 30%. The regression analysis method is used to establish a model and the reliability of this model is examined by the experiments. The results show that the model predicted value is closed to the practical value,and the calcinations temperature,time and mass fraction of active component behave prominent effects on the penetration time. The interactions of calcinations temperature and time,calcinations temperature and mass fraction of active component are more remarkable.