Immobilized binuclear rhodium metal complex catalyst and preparation method and application thereof
A technology of metal complexes and catalysts, which is applied in the field of immobilized binuclear rhodium metal complex catalysts and their preparation, can solve problems that have not been reported, and achieve the effects of simple and fast methods, large specific surface area, and stable structure
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[0024] The embodiment of the present invention also provides a preparation method of a solid-supported binuclear rhodium metal complex catalyst, comprising: making the 2 (esp) 2 The mixed system of 2-methylimidazole and solvent reacts at room temperature to form 2-methylimidazole axially modified Rh 2 (esp) 2 , and then add Zn to the mixed system 2+ , react at room temperature to obtain a solid-supported binuclear rhodium metal complex catalyst.
[0025] In some more specific embodiments, the preparation method comprises: at room temperature, to Rh 2 (esp) 2 2-Methylimidazole was added to the methanol solution to react until the color of the solution changed from green to light red, and Rh containing 2-Methylimidazole axial modification was obtained. 2 (esp) 2 The reaction mixture, and then add soluble zinc salt to the reaction mixture for reaction to obtain a solid-supported binuclear rhodium metal complex catalyst.
[0026] Further, wherein the amount of 2-methylimida...
Embodiment 1
[0039] Example 1: Immobilized Rh in one step 2 (esp) 2 Preparation of:
[0040] Step 1: 2-Methylimidazole and Rh 2 (esp) 2 Axial coordination: the Rh 2 (esp) 2 Dissolve in 10mL methanol solution respectively to obtain a clear green solution with a concentration below 3.0mg / mL, then add 4.0mmol of 2-methylimidazole, and wait until the solution changes from green to light red, at this time, the solution containing axial Ligand 2-methylimidazole modified Rh 2 (esp) 2 A reaction mixture in which the axial ligand 2-methylimidazole-modified Rh 2 (esp) 2 The X-ray photoelectron spectrum of figure 2 shown.
[0041] Step 2: Self-assembly to form ZIF-8: Slowly add zinc nitrate aqueous solution dropwise to the aforementioned reaction mixture at room temperature, and magnetically stir for 2 hours to allow self-assembly to prepare Rh 2 (esp) 2 complex with ZIF-8. Then centrifuged and washed with methanol solution to obtain the immobilized Rh 2 (esp) 2 Composite material, pl...
Embodiment 2
[0043] Embodiment 2: the Rh 2 (esp) 2 The process of using @ZIF-8 to catalyze the synthesis of N-H propane ring compounds is as follows:
[0044] The reaction was carried out in a 10mL reaction flask, and 0.55mmol of 2,4-dinitrophenylhydroxylamine, 0.005mmolRh 2 (esp) 2 The @ZIF-8 catalyst was added to the reaction bottle, and then filled with nitrogen gas after vacuuming with an oil pump. This was done three times, and then 5.0 mL of 2,2,2-trifluoroethanol solvent and 0.50 mmol of 2- Methyl-1-phenylpropene was reacted for 3h at room temperature. Take 0.60 μL of the clear liquid of the reaction product, and quantitatively analyze the reaction product with a gas chromatograph, and the results are shown in Table 1:
[0045] Table 1 is the result of quantitative analysis of the reaction product by gas chromatography
[0046] catalyst
Reaction time (h)
Conversion rates(%)
selectivity (%)
Yield(%)
1mol% Rh 2 (esp) 2 @ZIF-8
3
96
82 ...
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