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Facile preparation of nanostructured Pd-Sch-δ-FeOOH particles: A highly effective and easily retrievable catalyst for aryl halide cyanation and p-nitrophenol reduction
Journal of Physics and Chemistry of Solids ( IF 4.3 ) Pub Date : 2021-01-25 , DOI: 10.1016/j.jpcs.2021.109968
Melike Çalışkan , Talat Baran , Mahmoud Nasrollahzadeh

Iron based compounds are good candidates as supports to immobilize different transition metals due to their eco-friendly nature, capability of facilitating chemical modifications, inexpensiveness, high stability and easy recoverability. In this study, palladium nanoparticles (Pd NPs) were successfully stabilized on designed Schiff base modified δ-FeOOH particles as a highly effective and readily recoverable heterogeneous catalyst (Pd-Sch-δ-FeOOH nanocatalyst). The catalyst was fabricated via a facile multi-step approach without utilizing any additional reducing agents. The Pd-Sch-δ-FeOOH was characterized by Fourier transforms infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET). Characterization studies confirmed that the prepared small sized Pd NPs were spherically shaped and well dispersed on the surface of Schiff base modified δ-FeOOH. The catalytic efficiency of Pd-Sch-δ-FeOOH nanocatalyst was then tested in the preparation of benzonitriles through cyanation of aryl halides using K4[Fe(CN)6] has been utilized as a cyanation agent and also reduction of p-nitrophenol (p-NP) using NaBH4 as the reducing agent. Benzonitriles were characterized using GC-MS. Catalytic studies showed that benzonitriles were obtained in good reaction yields in the presence of heterogeneous Pd-Sch-δ-FeOOH nanocatalyst (87–98%). It was found that Pd-Sch-δ-FeOOH was also a useful nanocatalyst for p-NP reduction at ambient temperature in eco-friendly media within 2 min. The reduction rate for p-NP with Pd-Sch-δ-FeOOH was measured via UV–Vis spectroscopy from 250 nm to 550 nm. Furthermore, Pd-Sch-δ-FeOOH nanocatalyst was able to remain active for six successive runs due to its recyclable/reusable nature.



中文翻译:

简便地制备纳米结构的Pd-Sch-δ-FeOOH颗粒:一种高效且易于回收的芳基卤化物氰化和硝基苯酚还原的催化剂

铁基化合物由于其生态友好的性质,促进化学修饰的能力,廉价,高稳定性和易回收性,因此是固定不同过渡金属的良好候选载体。在这项研究中,钯纳米颗粒(Pd NPs)成功地稳定在设计的席夫碱改性δ-FeOOH颗粒上,作为高效且易于回收的多相催化剂(Pd-Sch-δ-FeOOH纳米催化剂)。催化剂是通过一种简便的多步骤方法,无需使用任何其他还原剂。通过傅立叶变换红外光谱(FT-IR),X射线衍射(XRD),扫描电子显微镜(SEM),能量色散X射线光谱(EDS),透射电子显微镜对Pd-Sch-δ-FeOOH进行表征(TEM)和Brunauer-Emmett-Teller(BET)。表征研究证实,所制备的小尺寸Pd NP为球形,并良好地分散在席夫碱改性的δ-FeOOH表面上。然后测试了Pd-Sch-δ-FeOOH纳米催化剂在使用K 4 [Fe(CN)6 ]进行芳基卤化物氰化制备苄腈中的催化效率,该催化剂已被用作氰化剂,还还原了硝基苯酚(p-NP),使用NaBH 4作为还原剂。使用GC-MS对苯甲腈进行表征。催化研究表明,在非均相Pd-Sch-δ-FeOOH纳米催化剂(87-98%)的存在下,苯甲腈以良好的反应收率获得。已经发现,Pd-Sch-δ-FeOOH还是在环境友好的介质中于2分钟内在环境温度下还原p- NP的有用的纳米催化剂。通过UV-Vis光谱从250 nm至550 nm测量了Pd-Sch-δ-FeOOH对p -NP的还原率。此外,Pd-Sch-δ-FeOOH纳米催化剂由于其可循环/可重复使用的性质,因此能够连续六次保持活性。

更新日期:2021-02-10
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