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MOF-based transition metal monatomic catalyst for carbon-carbon triple bond selective hydrogenation and preparation method of MOF-based transition metal monatomic catalyst

A transition metal, selective technology, applied in catalyst activation/preparation, physical/chemical process catalysts, hydrogenation to hydrocarbons, etc., can solve the problems of easy agglomeration coupling, no relevant reports, affecting catalytic activity and stability, etc. Achieve the effect of outstanding catalytic performance, simple process, easy recovery and reuse

Active Publication Date: 2021-02-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are no related reports on improving the performance of catalysts in the selective hydrogenation of carbon-carbon triple bonds by adjusting the local electronic structure of single atoms.
[0005] In summary, the construction of electron-rich single-atom catalytic sites is an effective means to improve the catalytic performance of supported catalysts in hydrogenation reactions. Surface energy, the cohesion between metal atoms makes the chemical bonds in a non-localized state, and agglomeration coupling is very easy to occur during high temperature treatment, which seriously affects the catalytic activity and stability

Method used

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  • MOF-based transition metal monatomic catalyst for carbon-carbon triple bond selective hydrogenation and preparation method of MOF-based transition metal monatomic catalyst
  • MOF-based transition metal monatomic catalyst for carbon-carbon triple bond selective hydrogenation and preparation method of MOF-based transition metal monatomic catalyst
  • MOF-based transition metal monatomic catalyst for carbon-carbon triple bond selective hydrogenation and preparation method of MOF-based transition metal monatomic catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A. 1.18g soluble ZrCl 4 and 0.9g of 2-aminoterephthalic acid were dissolved in 60mLN, N-dimethylformamide for ultrasonic dissolution;

[0036] B. Uniformly mix the mixed solution in step A with the glacial acetic acid solution at a volume ratio of 6:1, transfer to a reaction kettle, crystallize at 120°C for 24 hours, cool to room temperature naturally, filter the precipitate, and use N, N-dimethylformamide solution and absolute ethanol were washed until the pH value was neutral, and the solid was dried at 60 °C for 12 h to obtain a metal-organic framework material with an average pore size of 1.0 nm, expressed as UiO-66-NH 2 ;

[0037] C. The soluble transition metal salt PdCl 2 Soluble in deionized water to make Na with a concentration of 50mmol / L 2 PdCl 4 solution; take 1mL Na 2 PdCl 4 The solution was added to anhydrous methanol containing 2-pyridinecarbaldehyde, and stirred continuously at room temperature for 1 h;

[0038] D. At room temperature, according t...

Embodiment 2

[0043] A, B are with embodiment 1;

[0044] C. The soluble transition metal salt PdCl 2 Soluble in deionized water to make Na with a concentration of 50mmol / L 2 PdCl 4 solution; take 1mL Na 2 PdCl 4 The solution was added to anhydrous methanol containing 2-pyridinecarbaldehyde, and stirred continuously at room temperature for 1 h;

[0045] D. At room temperature, according to the fact that the transition metal accounts for 0.1wt.% of the mass of the carrier, fully disperse the carrier in step B into the impregnation solution of step C, keep stirring for 72h, filter, and wash with anhydrous methanol and dichloroethane , and dried at 60°C for 12 hours to obtain Pd 1 / UiO-66-NH 2 ;

[0046] E. Pd obtained in step D 1 / UiO-66-NH 2 Placed in the reactor, passing H 2 / C 2 h 2 / C2 h 4 atmosphere, wherein the molar ratio of alkynes to alkenes is 0.01, alkynes and H 2 The molar ratio is 0, the flow rate is 10mL / min, and at 10℃·min -1 The temperature is raised to 150 ° C ...

Embodiment 3

[0048] A. 1.18g soluble ZrCl 4 and 1.28g of 2-amino-4,4'-biphenyldicarboxylic acid were dissolved in 60mL of N,N-dimethylformamide for ultrasonic dissolution;

[0049] B. Uniformly mix the mixed solution in step A with the glacial acetic acid solution at a volume ratio of 6:1, transfer to a reaction kettle, crystallize at 120°C for 24 hours, cool to room temperature naturally, filter the precipitate, and use N, N-dimethylformamide solution and absolute ethanol were washed until the pH value was neutral, and the solid was dried at 60 °C for 12 h to obtain a metal-organic framework material with an average pore size of 1.5 nm, expressed as UiO-67-NH 2 ;

[0050] C. The soluble transition metal salt PtCl 2 Soluble in deionized water to make Na with a concentration of 50mmol / L 2 PtCl 4 solution; take 1mL Na 2 PtCl 4 The solution was added to anhydrous methanol containing 2-pyridinecarbaldehyde, and stirred continuously at room temperature for 1 h;

[0051] D. At room temper...

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Abstract

The invention provides an MOF-based transition metal monatomic catalyst for carbon-carbon triple bond selective hydrogenation and a preparation method of the MOF-based transition metal monatomic catalyst. The MOF-based transition metal monatomic catalyst is represented as M1 <[delta]+> / UiO-A-NH2, the catalyst is structurally characterized in that transition metal M is loaded on a UiO-A-NH2 carrier, atomic-scale uniform dispersion is realized, and the dispersion degree of active metal is 100%; carrier lattice strain induced by atmosphere treatment enables transition metal single atoms to be inan electron-enriched positive valence state, and meanwhile, the transition metal single atoms have good stability. The preparation method comprises the steps of dissolving a transition metal salt in deionized water to prepare a mixed salt solution, mixing the mixed salt solution with a carrier, anchoring an active metal single atom on the surface of the carrier through an organic ligand, and obtaining the M1 / UiO-A-NH2-R transition metal monatomic catalyst with an optimal local electronic structure and good stability through reaction atmosphere retreatment. The catalyst can be applied to various carbon-carbon triple bond selective hydrogenation reaction processes in the fields of petrochemical engineering, fine chemical engineering and the like, has outstanding catalytic performance, and has high activity and C=C double bond selectivity. The catalyst also has good recyclability, and is easy to recycle and reuse.

Description

technical field [0001] The invention belongs to the field of petrochemical industry and fine chemical industry, and in particular relates to a carbon-carbon triple bond selective hydrogenation catalyst and a preparation method thereof. Background technique [0002] Selective hydrogenation of carbon-carbon triple bonds is an extremely important and challenging reaction in the chemical industry. Supported Pd-based catalysts are widely used in industrial production due to their excellent activity, but they are prone to form subsurface H species and carbon deposits during the reaction process, greatly reducing their olefin selectivity and stability. Therefore, it is extremely urgent to develop catalysts with high activity, high selectivity and stability. Earlier, in order to improve the selectivity, researchers used lead acetate and quinoline to modify single metal Pd catalysts (Lindlar catalysts). However, the toxic lead species not only caused great damage to the environment,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/00B01J35/10B01J37/02B01J37/08B01J37/18C07C5/09C07C11/04
CPCB01J31/1691B01J31/1815B01J31/2239B01J37/0201B01J37/08B01J37/18C07C5/09B01J2231/645B01J2531/847B01J2531/842B01J2531/824B01J2531/828B01J2531/48B01J35/394B01J35/643C07C11/04Y02P20/52Y02P20/584
Inventor 刘雅楠茹威李殿卿冯俊婷贺宇飞
Owner BEIJING UNIV OF CHEM TECH
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