Rhodium-calix[4]pyrrole and rhodium-tetraphenyl porphyrin: preparation, surface grafting and their catalytic application in nitro-benzene reduction†,Dalton Transactions

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Rhodium-calix[4]pyrrole and rhodium-tetraphenyl porphyrin: preparation, surface grafting and their catalytic application in nitro-benzene reduction†
Dalton Transactions ( IF 3.5 ) Pub Date : 2018-08-09 00:00:00 , DOI: 10.1039/c8dt02151a
K. Anjali _{1,

2,

3,

4} , M. Ahmed _{1,

4,

5,

6} , J. Christopher _{4,

7,

8,

9} , A. Sakthivel _{1,

2,

3,

4}

Affiliation

Rhodium containing macromolecules calix[4]pyrrole (RhCP) and tetraphenyl porphyrin (RhTPP) were prepared and grafted on the surface of functionalised molecular sieve materials. ¹H and ¹³C NMR, CHNS and mass spectral analyses were used for the structural elucidation of homogeneous organometallic complexes.¹H NMR and CHNS analyses confirm the formation of calix[4]pyrrole (CP) and tetraphenyl porphyrin (TPP). The introduction of rhodium ions into the macromolecule is well evident from the disappearance of the ¹H NMR signal characteristic of N–H proton (7.1 ppm in CP and −2.74 ppm in TPP). Furthermore the formation of RhCP and RhTPP complexes is confirmed using CHNS and mass spectral analysis; the data are in line with theoretically calculated values. The grafting of RhCP and RhTPP on a diamino functionalised SBA-15 support was confirmed through low angle XRD, ¹³C MAS-NMR and SEM-EDAX analysis. Both homogeneous and heterogeneous catalysts were utilized for nitrobenzene reduction. RhCP and RhTPP heterogenized on SBA-15-F showed complete conversion of nitrobenzene with exclusive formation of aniline as a product. The catalytic activities were retained in both the systems even after several runs.

中文翻译：

铑杯[4]吡咯和铑四苯基卟啉：制备，表面接枝及其在硝基苯还原中的催化应用†

制备了含铑大分子杯[4]吡咯（RhCP）和四苯基卟啉（RhTPP），并将其接枝到功能化分子筛材料的表面。¹ H和¹³ C NMR，CHNS和质谱分析用于均相有机金属配合物的结构阐明。¹ H NMR和CHNS分析证实了杯[4]吡咯（CP）和四苯基卟啉（TPP）的形成。引入铑离子进入高分子从消失是井明显¹NH质子的H NMR信号特征（CP中为7.1 ppm，TPP中为-2.74 ppm）。此外，使用CHNS和质谱分析证实了RhCP和RhTPP配合物的形成。数据与理论计算值一致。通过低角度XRD，¹³ C MAS-NMR和SEM-EDAX分析证实了RhCP和RhTPP在二氨基官能化的SBA-15载体上的接枝。均相和非均相催化剂均用于硝基苯还原。在SBA-15-F上杂化的RhCP和RhTPP显示硝基苯完全转化，而仅形成苯胺产物。即使经过几次运行，催化活性仍保留在两个系统中。

更新日期：2018-08-09

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