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Preparation method of trace oxygen modified Pd-coated CNFs catalyst

A catalyst and trace oxygen technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problems of small specific surface area, metal leaching loss, etc., and achieve improvement Selectivity, enhanced ability to activate hydrogen, and improved loading effect

Active Publication Date: 2022-06-24
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention proposes a novel preparation method of trace oxygen-modified Pd@CNFs catalyst for the problems of small specific surface area and metal leaching loss in traditional CNFs

Method used

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  • Preparation method of trace oxygen modified Pd-coated CNFs catalyst
  • Preparation method of trace oxygen modified Pd-coated CNFs catalyst
  • Preparation method of trace oxygen modified Pd-coated CNFs catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Pd@CNFs catalyst preparation

[0038] (1) Preparation of electrospun PAN nanofibers

[0039] Disperse 1 g of PAN in 10 mL of DMF o Stir at C for 12 h until the solution turns into a yellow transparent viscous liquid, and prepare an electrospinning solution. Then, the electrospinning solution was injected into a syringe with a 22-gauge stainless steel needle. The electrospinning operating conditions were set as follows: the working voltage was 14 kV, the syringe bolus was 1 mL / h, the translation distance was 60 mm, the receiver receiving distance was 15 cm, and the receiving speed was 80 rpm. Thus, a white PAN nanofiber membrane was prepared and cut into a 10*10cm sheet for use.

[0040] (2) Preparation of ZIF-L-Co / PAN nanofibers

[0041] The Co(NO 3 ) 2 ·6H 2 O-methanol solution (0.1 mol / L, 20 mL) was quickly poured into 2-methylimidazole-methanol solution (0.8 mol / L, 20 mL), at 30 o C, magnetic stirring at 100 rev / min for 60s to obtain ZIFs mother liquor. T...

Embodiment 2

[0067] (1) Preparation of electrospun PAN nanofibers

[0068] Disperse 0.8g PAN evenly in 10mL DMF, and put it at 60 o Stir at C for 12 h until the solution turns into a yellow transparent viscous liquid, and prepare an electrospinning solution. Then, the electrospinning solution was injected into a syringe with a 22-gauge stainless steel needle. The electrospinning operating conditions were set as follows: working voltage 13kV, syringe bolus 0.75mL / h, translation distance 100mm, receiver receiving distance 17cm, and receiving speed 100rpm. Thus, a white PAN nanofiber membrane was prepared and cut into a 10*10cm sheet for use.

[0069] (2) Preparation of ZIF-L-Co / PAN nanofibers

[0070] The Co(NO 3 ) 2 ·6H 2 O-methanol solution (0.05mol / L, 20mL) was quickly poured into 2-methylimidazole-methanol solution (0.24mol / L, 20mL), and at 40 o C, magnetic stirring at 80 rpm for 50 s. The trimmed PAN nanofiber membranes were then immersed in ZIFs mother solution for 8 h. After ...

Embodiment 3

[0079] (1) Preparation of electrospun PAN nanofibers

[0080] 1.4g PAN was uniformly dispersed in 10mL DMF, and the o Stir at C for 12 h until the solution turns into a yellow transparent viscous liquid, and prepare an electrospinning solution. Then, the electrospinning solution was injected into a syringe with a 21-gauge stainless steel needle. The electrospinning operating conditions were set as follows: working voltage 16 kV, syringe bolus 1.5 mL / h, translation distance 80 mm, receiver receiving distance 13 cm, and receiving speed 85 rpm. Thus, a white PAN nanofiber membrane was prepared and cut into a 10*10cm sheet for use.

[0081] (2) Preparation of ZIF-L-Co / PAN nanofibers

[0082] The Co(NO 3 ) 2 ·6H 2 The O-methanol solution (0.2mol / L, 20mL) was quickly poured into 2-methylimidazole-methanol solution (4.8mol / L, 20mL), and the solution was heated at 20 o C, magnetic stirring at 150 rpm for 80 s. The trimmed PAN nanofiber membranes were then immersed in ZIFs moth...

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Abstract

The invention relates to a preparation method of a trace oxygen modified Pd-coated CNFs catalyst, and belongs to the technical field of catalysis. The preparation method of the material comprises the following steps: growing ZIF-67 on electrostatic spinning PAN nanofibers in situ through an impregnation method, carrying out oxygen activation on the ZIF67 / PAN composite nanofibers in a high-temperature pyrolysis process by taking oxygen as an oxidant, then carrying out acid pickling, and loading an active component Pd to obtain the trace oxygen modified Pd-coated CNFs catalyst. The preparation method has the advantages that etching with a proper initial oxygen concentration is beneficial to preparation of a hierarchical porous material with a high non-micropore ratio and formation of high-content ether-type oxygen on the surface of the catalyst, so that adsorption, dispersion and anchoring of active components are enhanced; the basic strength of the catalyst and the dispersity of the catalyst in reaction liquid can be enhanced by introducing ether oxygen; the prepared Pd-coated CNFs catalyst shows excellent catalytic performance, and has relatively good reusability. In addition, due to the characteristic of easy solid-liquid separation of the catalyst after the reaction, the separation operation cost is remarkably reduced.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to a preparation method of a trace oxygen-modified Pd@CNFs catalyst. Background technique [0002] As an important chemical raw material for the synthesis of nylon 6, the preparation of cyclohexanone has received extensive attention. At present, the widely used cyclohexane oxidation method has problems such as high energy consumption, post-treatment of acid-base waste liquid, complicated process, and many by-products, which does not conform to the concept of green development. Therefore, the liquid-phase hydrogenation method of phenol with mild reaction conditions, few by-products and simple operation process is favored by researchers. The design and preparation of catalysts for the liquid-phase hydrogenation of phenol with high activity and selectivity have become a research hotspot. [0003] Pd-based catalysts have become one of the most widely studied catalysts becau...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/10
CPCB01J23/8913B01J35/61B01J35/60Y02P20/52
Inventor 陈日志朱心如屈正炎姜红邢卫红
Owner NANJING UNIV OF TECH