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Metal organic framework based on Cd (II), composite catalyst and preparation method and application thereof

A technology of metal-organic frameworks and composite catalysts, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, preparation of amino hydroxyl compounds, etc. It can solve the problem of unstable catalytic performance and poor dispersion of precious metals in composite catalysts. Uniformity and other issues, to achieve the effect of less catalyst consumption, uniform size, and improved utilization

Active Publication Date: 2022-03-01
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inventors found that the common loading methods in the prior art, such as wet mixing, solid phase grinding, etc., resulted in uneven dispersion of precious metals in the obtained composite catalyst and unstable catalytic performance.

Method used

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  • Metal organic framework based on Cd (II), composite catalyst and preparation method and application thereof
  • Metal organic framework based on Cd (II), composite catalyst and preparation method and application thereof
  • Metal organic framework based on Cd (II), composite catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Preparation of organic ligand L

[0045] Concrete preparation steps are as follows:

[0046]

[0047] Weigh 3.0g (8.6mmol) of intermediate X into a 100ml round bottom flask, add 6.12g (30mmol) of intermediate Y and 20mL of anhydrous pyridine, and react at 120°C for 2-4 hours. After the system was cooled, 60ml of water was added, the dark crude product was obtained by suction filtration, dried, and column chromatography (ethyl acetate) gave 6.5g of light yellow powder Z with a yield of 56%. The above-mentioned Z was dissolved in 50 mL of ethanol, 2 g of NaOH was added, the reaction was refluxed for 5-7 hours, acidified with dilute hydrochloric acid until the pH was 1, and the white solid of L was filtered with suction, and the yield was 90%. HNMR of ligand L as figure 1 shown.

Embodiment 2

[0048] Example 2 Preparation of Cd-MOF

[0049] Concrete preparation steps are as follows:

[0050] Ligand L (70mg, 0.096mmol) and CdBr 2(87mg, 0.32mmol) was dissolved in 4mL of methanol, and reacted in a 23mL polytetrafluoroethylene reactor for 72h. Cool naturally to room temperature to obtain colorless crystals, centrifuge, wash with a small amount of methanol, and dry under infrared light to obtain Cd-MOF, whose stacking structure is figure 2 . From figure 2 It can be seen that the Cd-MOF has a regular framework structure and channel arrangement.

Embodiment 3

[0051] Example 3 Preparation of Composite Catalyst Pd@Cd-MOF

[0052] With 33mg K 2 PdCl 4 Dissolve in 5mL water, add 30mg Cd-MOF, stir at room temperature, reach adsorption saturation, and centrifuge to obtain the adsorption of Pd precursor (PdCl 4 )x@Cd-MOF. The above powder was washed with NaBH 4 The obtained methanol solution was reduced to obtain a brown Cd(II) metal-organic framework-supported palladium nanoparticle composite catalyst Pd@Cd-MOF.

[0053] The compound was characterized by XPS, TEM, X-ray powder diffraction, etc., the results are shown in the attached image 3 , 4 , 5; attached image 3 , 4 , 5 It can be seen that: Pd is reduced to zero valence, and ultra-small particles of about 2nm are uniformly dispersed inside the MOF, and in the above process, the structure of the MOF remains intact.

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PUM

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Abstract

The invention discloses a Cd (II)-based metal organic framework, a composite catalyst and a preparation method and application of the Cd (II)-based metal organic framework and the composite catalyst. The preparation method comprises the following steps: firstly, preparing an organic ligand L through an organic synthesis method, and secondly, reacting the ligand with CdBr2 under a solvothermal condition to obtain Cd (II)-MOF. The preparation method comprises the following steps: synthesizing an MClx-Cd-MOF intermediate from a metal organic framework and a noble metal precursor salt, and then reducing MClx-Cd-MOF through sodium borohydride to obtain the novel metal organic framework loaded noble metal nanoparticle M-Cd-MOF composite catalyst of Cd (II). The catalyst can effectively catalyze the reduction reaction of nitrobenzene compounds and the coupling reaction of phenylboronic acid and iodobenzene at the same time, the reaction condition is mild, the reaction time is short, the dosage of the catalyst is small, no other additive is added, and compared with free precious metal salt, the catalyst can be repeatedly used for more than five times.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to Cd(II)-based metal-organic frameworks, composite catalysts, preparation methods and applications thereof. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Metal-organic framework (Metal-organic Framework, MOF) is a research hotspot in recent years. Compared with traditional porous materials, MOF has porosity, larger specific surface area and pore volume in the framework. As a porous functional material in Applications in catalysis present great advantages. Noble metal nanoparticles often have excellent catalytic performance, but they are difficult to recycle and cannot be re...

Claims

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Application Information

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IPC IPC(8): C07D271/10C08G83/00B01J31/22C07C213/02C07C215/76
CPCC07D271/10C08G83/008B01J31/1815B01J31/2208C07C213/02B01J2531/824B01J2231/641C07C215/76
Inventor 赵朝委张月凤方洁游胜勇晏南富李韦伟
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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