Preparation method and application of bipyridine functionalized COF loaded palladium nanoparticles

A technology of palladium nanoparticles and bipyridine is applied in the field of preparation of bipyridine functionalized COF-supported palladium nanoparticles, which can solve the problems of low ethylene selectivity and easy deactivation of catalysts, and achieve the effects of long service life and high catalytic performance.

Inactive Publication Date: 2020-04-21
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Supported palladium-based catalysts are widely used due to their excellent low-temperature catalytic activity for acetylene, but there are also problems such as low ethylene selectivity and easy deactivation of the catalyst.

Method used

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  • Preparation method and application of bipyridine functionalized COF loaded palladium nanoparticles
  • Preparation method and application of bipyridine functionalized COF loaded palladium nanoparticles

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: The preparation method of bipyridyl functionalized COF loaded palladium nanoparticles, the specific steps are as follows:

[0023] (1) Dissolve tritylaldehyde and 5,5'-diamino-2,2'-bipyridine in an organic solvent in a high borosilicate glass tube to obtain a mixed solution A, drop by drop in the mixed solution A Add acetic acid aqueous solution to obtain mixed solution B; wherein the organic solvent is a mixed solvent of ethanol and mesitylene; wherein the concentration of tritylaldehyde in mixed solution A is 0.10mol / L, 5,5'-diamino-2,2 The concentration of '-bipyridyl is 0.150mol / L, the volume ratio of ethanol and mesitylene in the organic solvent is 4:1, the concentration of acetic acid aqueous solution is 6.0mol / L, and the volume ratio of acetic acid aqueous solution and organic solvent is 1:5 ;

[0024] (2) Freeze the mixed solution B in the high borosilicate glass tube in step (1) sequentially with liquid nitrogen and vacuumize it with a mechanical...

Embodiment 2

[0030] Embodiment 2: the preparation method of bipyridyl functionalized COF loaded palladium nanoparticles, the specific steps are as follows:

[0031] (1) Dissolve tritylaldehyde and 5,5'-diamino-2,2'-bipyridine in an organic solvent in a high borosilicate glass tube to obtain a mixed solution A, drop by drop in the mixed solution A Add acetic acid aqueous solution to obtain mixed solution B; wherein the organic solvent is a mixed solvent of ethanol and mesitylene; wherein the concentration of tritylaldehyde in mixed solution A is 0.11mol / L, 5,5'-diamino-2,2 The concentration of '-bipyridine is 0.165mol / L, the volume ratio of ethanol and mesitylene in the organic solvent is 3:1, the concentration of acetic acid aqueous solution is 6.0mol / L, and the volume ratio of acetic acid aqueous solution and organic solvent is 1:5 ;

[0032] (2) Freeze the mixed solution B in the high borosilicate glass tube in step (1) sequentially with liquid nitrogen and vacuumize it with a mechanica...

Embodiment 3

[0037] Embodiment 3: The preparation method of bipyridyl functionalized COF loaded palladium nanoparticles, the specific steps are as follows:

[0038] (1) Dissolve tritylaldehyde and 5,5'-diamino-2,2'-bipyridine in an organic solvent in a high borosilicate glass tube to obtain a mixed solution A, drop by drop in the mixed solution A Add acetic acid aqueous solution to obtain mixed solution B; wherein the organic solvent is a mixed solvent of ethanol and mesitylene; wherein the concentration of mesitylaldehyde in mixed solution A is 0.12mol / L, 5,5'-diamino-2,2 The concentration of '-bipyridine is 0.180mol / L, the volume ratio of ethanol and mesitylene in the organic solvent is 2:1, the concentration of acetic acid aqueous solution is 5.0mol / L, and the volume ratio of acetic acid aqueous solution and organic solvent is 1:5.5 ;

[0039] (2) Freeze the mixed solution B in the high borosilicate glass tube in step (1) sequentially with liquid nitrogen and vacuumize it with a mechan...

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Abstract

The invention relates to a preparation method and an application of bipyridine functionalized COF loaded palladium nanoparticles. The preparation method comprises the following steps: adding 1,3,5-benzenetricarboxaldehyde and 5,5'-diamino-2,2'-dipyridyl in an organic solvent to obtain a mixed solution A, dropwise adding an aqueous acetic acid solution into the mixed solution A, sequentially carrying out liquid nitrogen freezing-vacuumizing-thawing cycle operation, performing vacuum sealing, thawing to room temperature, and carrying out a constant-temperature reaction at 120-150 DEG C for 3-6 d; carrying out unsealing, dropwise adding tetrahydrofuran to carry out a quenching reaction, carrying out solid-liquid separation, washing the solid, and carrying out vacuum drying to obtain a solid powder D; and carrying out wet grinding on the solid powder D to obtain a micropowder, sequentially adding ethanol and a palladium salt solution into the micropowder, carrying out a stirring reaction for 2-4 h, dropwise adding a NaBH4 solution until the mixed solution is brown yellow, continuously carrying out a reaction for 1-2 h under a stirring condition, carrying out solid-liquid separation, washing the solid, and carrying out vacuum drying to obtain the bipyridine functionalized COF supported palladium nanoparticles. The bipyridine functionalized COF loaded palladium nanoparticles are usedas a catalyst for catalyzing a semi-hydrogenation reaction of acetylene.

Description

technical field [0001] The invention relates to a preparation method and application of bipyridyl functionalized COF-loaded palladium nanoparticles, belonging to the technical field of catalysts. Background technique [0002] Ethylene is one of the chemical products with the largest output and the core raw material of the petrochemical industry. Its output is an important symbol to measure the development level of a country's oil industry. The development of ethylene industry also drives the development of fine chemicals, light industry textiles, automobile manufacturing, building materials industry, mechanical electronics and modern agriculture, and plays an important role in the economic field. Ethylene is generally produced by cracking naphtha in the industry, but 0.1%-0.5% of acetylene is often produced in this process. The presence of acetylene will poison and deactivate the Ziegler-Natta catalyst used to produce polyethylene. Add acetylene to remove. In industry, ace...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C5/05C07C11/04
CPCB01J31/183B01J2231/645B01J2531/0213B01J2531/0238B01J2531/824C07C5/05C07C2531/22C07C11/04Y02P20/52
Inventor 关清卿张关印施宇震宁平朱远蹠
Owner KUNMING UNIV OF SCI & TECH
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