A new approach (microwave-hydrothermal plus oxidation) was proposed for the preparation of the Zn-based sorbents supported on the ordered mesoporous Si-based material. The hydrothermal synthesis and oxidation conditions of the sorbent precursor (ZnS/MCM41 mesophase) with Zn(AC)₂ and thioacetamide (TAA) as the Zn and S sources, respectively, were optimized. The sorbents were evaluated in a fixed bed using the simulate gas of 2000 ppm H₂S, 39% H₂, 27% CO, 12% CO₂, and N₂ as balance gas. The structure of the sorbents was characterized by means of XRD, N₂ adsoprtion, SEM, EDX, and TEM analysis. The results indicate that the optimal microwave-hydrothermal conditions are 400 W, 2.5 h, and 1:3 (the mole ratio of the Zn(AC)₂ to TAA). The oxidation of ZnS in the sorbent precursor to ZnO is invalid at 550 °C due to unfavorable reaction kinetics. Both the fresh and used sorbents show ordered hexagonal mesoporous structure. It is confirmed that Zn₂SiO₄ present in the fresh and regenerated sorbents could be consumed during the desulfurization process via the reaction (Zn₂SiO₄ + 2H₂S → 2ZnS + SiO₂ + 2H₂O), giving a positive effect on the desulfurization of the sorbents. The optimized Zn-based mesoporous sorbent (actual Zn content: 20.3%) exhibits superior (high breakthrough sulfur capacity: 5.4–5.7%) and stable desulfurization ability during five sulfidation/regeneration cycles. In addition, sulifidation reaction only leads to low-degree plugging of the pore structure of the regenerated sorbents, and the regeneration reaction could restore (at least mostly) the aforementioned changes in the pore properties.

提出了一种新的方法（微波水热加氧化法）来制备有序介孔Si基材料上负载的Zn基吸附剂。优化了分别以Zn（AC）₂和硫代乙酰胺（TAA）为Zn和S源的吸附剂前体（ZnS / MCM41中间相）的水热合成和氧化条件。吸附剂使用2000ppm的H的模拟气体中的固定床评价₂ S，39％H ₂，27％CO，12％CO ₂和N ₂作为平衡气体。吸附剂的结构通过XRD，N ₂表征吸附，SEM，EDX和TEM分析。结果表明，最佳微波水热条件为400 W，2.5 h和1：3（Zn（AC）₂与TAA的摩尔比）。由于不利的反应动力学，吸附剂前体中的ZnS氧化为ZnO在550°C时是无效的。新鲜的和用过的吸附剂均显示出有序的六角形介孔结构。可以确认，在脱硫过程中，新鲜的和再生的吸附剂中存在的Zn ₂ SiO ₄可以通过反应（Zn ₂ SiO ₄  + 2H ₂ S→2ZnS + SiO ₂  + 2H _2）被消耗掉。O），对吸附剂的脱硫有积极作用。经过优化的基于Zn的中孔吸附剂（实际Zn含量：20.3％）在五个硫化/再生循环中均表现出优异的（高突破硫容量：5.4-5.7％）和稳定的脱硫能力。另外，硫化反应仅导致再生吸附剂的孔结构的低度堵塞，并且再生反应可以（至少大部分）恢复上述孔特性的变化。