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Preparation method and application of nanopd1.6au1.0 alloy @mn(ii)mof

A pd1.6au1.0, MOF technology, applied in the preparation of imino compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. The problems of less amines, etc., to achieve the effect of simple preparation method, easy recovery, and improved utilization rate

Inactive Publication Date: 2018-07-24
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few relatively specific catalysts for directly generating N-benzylamine from the reaction of benzyl alcohol and benzyl ammonia, and the selectivity is not high.

Method used

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  • Preparation method and application of nanopd1.6au1.0 alloy @mn(ii)mof
  • Preparation method and application of nanopd1.6au1.0 alloy @mn(ii)mof
  • Preparation method and application of nanopd1.6au1.0 alloy @mn(ii)mof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: the synthesis of ligand L

[0050] in N 2 Under the protection of 4-bromoacetophenone (2.00g, 10.0mmol), pyridine-4-boronic acid (1.48g, 12.0mmol), tetrakistriphenylphosphine palladium (0.34g, 0.30mmol), anhydrous phosphoric acid Potassium (4.14g, 30.0mmol), 40ml of ethanol and 20ml of water were placed in a three-necked flask (50ml), and stirred at a constant temperature of 80°C for 36h. After the reaction was completed, the liquid was separated while it was hot, and the upper organic layer was taken, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain a yellow solid. Perform column chromatography (CH 2 Cl 2 :CH 3 OH=20:1), a white intermediate was obtained. in N 2 Under the protection of , the intermediate (1.00g, 5.0mmol), sodium amide (0.39g, 5mmol), ethyl trifluoroacetate (3.6ml, 25mmol) and anhydrous tetrahydrofuran (30ml) were placed in a 100ml three-necked flask at room temperature Stir ...

Embodiment 2

[0051] Embodiment 2: the synthesis of Mn (II)-MOF

[0052] Dissolve 3 mg of organic ligand L in 2 ml of ethyl acetate, 5 mg of manganese acetate in 2 ml of methanol, put it in a 10 ml test tube, add a mixture of ethyl acetate and methanol between the two solutions, and leave it at room temperature after 5 days Light red crystals were obtained with a yield of 82% (based on L).

[0053] We passed TGA, CO 2 The compound was characterized by adsorption and XRD, and the results are shown in Figure 5 , 7 ,9.

Embodiment 3

[0054] Embodiment 3: Nano Pd 1.6 Au 1.0 Synthesis of Alloy@Mn(II)-MOF

[0055] Weigh 5 mg of potassium tetrachloroalloy and 5 mg of palladium chloride and dissolve them in 5 ml of ethanol, and perform ultrasonic treatment to dissolve completely to obtain a dark brown solution. After weighing 5 mg MOFs and mixing with the above solution, it was placed on a magnetic stirrer and stirred for 1 h at a speed of 130 r / min. Then carry out centrifugation, firstly wash twice with ethanol, then wash twice with acetonitrile, and finally wash once with ether, and finally the solution is colorless, which proves that the washing is clean. The obtained product is baked under an infrared lamp for about 5 minutes to make it dry. Weigh 2mg of sodium borohydride and dissolve it in 2ml of secondary water, shake it slightly to dissolve completely, then slowly add the solution drop by drop to the dried product, a large number of bubbles will be observed, and the product will quickly turn black. ...

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Abstract

The invention discloses a preparation method and application of nano-Pd1.6Au1.0 alloy@Mn(II)MOF. The Mn(II)-MOF is crystallized in the triclinic system, belongs to the P-1 space group, and has a node The Mn(II) metal center is in a coordination environment of a deformed octahedron {MnN2O4}. The octahedral coordination plane is occupied by four O atoms from diketone and one N atom from pyridine in the axial direction. Mn(II)-MOF is soaked in PdCl2 and K2AuCl4 solutions and reduced with sodium borohydride to obtain a nano-Pd1.6Au1.0 alloy@Mn(II)-MOF catalyst. The catalyst can effectively catalyze the series reaction of benzyl alcohol and benzyl ammonia. The reaction temperature is mild, the reaction time is short, the catalyst dosage is small, there are no other additives, and it can be reused more than five times.

Description

technical field [0001] The present invention relates to a kind of nanometer Pd 1.6 Au 1.0 The preparation method and application of alloy@Mn(II)MOF belong to the technical field of catalyst preparation. Background technique [0002] Nanomaterials are a research hotspot in recent years. Compared with traditional porous materials, nanomaterials have large specific surface area and high activity, and show great advantages in the application of organic catalysis, but they are easy to aggregate and their The catalytic activity will be greatly reduced after aggregation. Metal-organic frameworks (Metal-organic Frameworks, MOFs), as a material with holes, the size of the holes can be better regulated, and the loading of nanoparticles into metal-organic frameworks can limit the aggregation of nanomaterials, while maintaining the high catalytic activity of the material. [0003] As an important chemical raw material, N-benzylamine is mainly prepared by reacting aldehyde and corres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C249/02C07C251/16
CPCC07C249/02B01J31/2217B01J2231/4283B01J2531/72B01J2531/0241B01J35/40C07C251/16Y02P20/584
Inventor 董育斌马慧超陈功军
Owner SHANDONG NORMAL UNIV
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