Nitrate-intercalated Mg/Cu/Al-layered double hydroxides (LDHs) were successfully synthesized by the co-precipitation method under ultrasonic irradiation as a fast, simple, and low-cost technique. The LDHs were synthesized with six different molar ratios of Cu2+/Mg2+, and then they were characterized by FT-IR, XRD, TGA, ICP, BET, TEM, and FE-SEM analyses. The results showed that the nitrate ions were well intercalated between layers without any carbonate ions. According to the XRD and TGA results, increasing of Cu ions in the LDHs lowered the crystallization and improved the thermal stability of samples at the same time. The morphological studies carried out by FE-SEM and TEM analyses showed the morphological structure similar to the lamellar structure and plate-like shape particles. However, the surface property of binary LDHs, including Al and only one of Cu or Mg elements, was better than ternary ones. Furthermore, this catalyst was used for the phenol hydroxylation using H2O2 as oxidant and water as a solvent. The results exhibit that the CuMg32Al-NO3− catalyst had the best catalytic activity, as well as it was found that the catalyst is active under mild reaction conditions such as the temperature of 65 °C, phenol: oxidant ratio of 2:1, phenol/catalyst = 100, and reaction time of 1 h. Thus, these conditions gave better activity with the conversion of 27%, the selectivity of 92.05% for catechol and hydroquinone, and CAT/HQ ratio of 1.5.
在超声波辐照下采用共沉淀法成功合成了
硝酸盐夹杂
镁/
铜/铝层双氢氧化物(LDHs),这是一种快速、简单、低成本的技术。合成了六种不同摩尔比的 Cu2+/Mg2+ 双氢氧化物,并对其进行了 FT-IR、XRD、TGA、ICP、BET、
TEM 和 FE-
SEM 分析。结果表明,
硝酸根离子在层间插层良好,没有
碳酸根离子。XRD 和 TGA 结果表明,增加 LDHs 中的
铜离子含量可降低结晶度,同时提高样品的热稳定性。通过 FE-
SEM 和
TEM 分析进行的形态学研究表明,LDHs 的形态结构类似于片状结构和板状颗粒。然而,二元 LDH(包括 Al 和仅含一种
铜或
镁元素)的表面性质优于三元 LDH。此外,该催化剂还被用于以
H2O2 为氧化剂、
水为溶剂的
苯酚羟基化反应。结果表明,CuMg32Al-
NO3- 催化剂的催化活性最好,而且在温和的反应条件下,如温度为 65 °C、
苯酚与氧化剂的比例为 2:1、
苯酚/催化剂=100、反应时间为 1 h,该催化剂也很活跃。因此,在这些条件下,催化剂具有较好的活性,转化率为 27%,对
儿茶酚和
对苯二酚的选择性为 92.05%,CAT/HQ 比率为 1.5。