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Load type palladium/polyvinyl alcohol fibre membrane catalyst, and preparation method and application thereof

A polyvinyl alcohol fiber, supported palladium technology, applied in physical/chemical process catalysts, fiber chemical characteristics, chemical instruments and methods, etc., can solve problems such as insufficient specific surface area of ​​activated carbon, insufficient structural stability, and low catalyst activity. , to achieve the effect of unique crystal structure and surface characteristics, controllable fiber structure and high specific surface area

Inactive Publication Date: 2011-09-14
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the commonly used metal palladium carrier activated carbon has insufficient specific surface area and unstable structure, resulting in low catalyst activity and short service life.

Method used

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  • Load type palladium/polyvinyl alcohol fibre membrane catalyst, and preparation method and application thereof
  • Load type palladium/polyvinyl alcohol fibre membrane catalyst, and preparation method and application thereof
  • Load type palladium/polyvinyl alcohol fibre membrane catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: The preparation of 2.5% palladium / polyvinyl alcohol fiber membrane catalyst is divided into three steps:

[0024] The first step is to prepare Na 2 PdCl 4 / polyvinyl alcohol solution; the second step, electrospinning Na 2 PdCl 4 / polyvinyl alcohol solution to prepare fiber membranes; the third step is thermal crosslinking and activation of palladium / polyvinyl alcohol fiber membrane catalysts.

[0025] The first step, Na 2 PdCl 4 Preparation of polyvinyl alcohol solution: weigh 0.100g PdCl 2 , 0.070g NaCl, then add 1 mL of 80 wt.% acetic acid aqueous solution, shake it to completely dissolve to obtain PdCl 2 Uniform, transparent, orange-red Na at a concentration of 0.01 g / ml 2 [PdCl 4 ] complex solution; 2.28 g of polyvinyl alcohol with a molecular weight of 80,000 was dissolved in 28.5 mL of 80 wt.% acetic acid aqueous solution to prepare a polyvinyl alcohol solution with a mass concentration of 8 wt.%. Finally, the above-mentioned Na 2 PdCl 4 so...

Embodiment 2

[0028] Example 2: Application of supported palladium / polyvinyl alcohol fiber membrane catalyst in Ullmann reaction.

[0029] Reactant R-X (for Ex. 1-7, X is I; For Ex. 10, X is I, C 5 h 4 N is pyridine) 1 mmol, palladium / polyvinyl alcohol fiber membrane catalyst 0.05 mmol, potassium acetate 7.5 mmol, DMSO 5 ml at 130 ° C for a certain period of time, poured into water, extracted with ethyl acetate, processed to obtain the product.

[0030]

[0031] Ex.

Embodiment 3

[0032] Embodiment 3: the recycling of catalyst.

[0033]The catalyst recovered by the Ex 1 reaction in Example 2 was washed with ethanol, dried and activated and then reused 5 times, and the catalytic efficiency was not substantially reduced.

[0034] usage count

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Abstract

The invention discloses a load type palladium / polyvinyl alcohol fibre membrane catalyst, and a preparation method and application thereof, belonging to the technical field of chemical catalyst preparation processes. The preparation method comprises the following steps of: 1, preparing a Na2PdCl4 solution and preparing a polyvinyl alcohol solution; 2, preparing a Na2PdCl4 / polyvinyl alcohol fibre membrane; and 3, cross-linking and activating. The Na2PdCl4 / polyvinyl alcohol fibre membrane prepared by electrostatic spinning has the advantages of high specific surface area, large porosity, controllable fibre structure and suitability for micromachining of a high polymer material; and the load type palladium / polyvinyl alcohol fibre membrane catalyst still has high catalytic efficiency after being used for several times.

Description

Technical field: [0001] The invention belongs to the technical field of chemical catalyst preparation technology, and specifically relates to a supported palladium / polyvinyl alcohol fiber membrane catalyst, a preparation method and an application thereof. Background technique: [0002] Supported palladium catalysts can overcome the disadvantages of homogeneous palladium catalysts, such as difficult separation and recovery, severe palladium loss, and generation of palladium black pollution reaction products, etc., occupying an extremely important position in petrochemical and organic synthesis. However, the commonly used metal palladium carrier activated carbon has insufficient specific surface area and insufficient structure stability, resulting in low catalyst activity and short service life. [0003] Based on this, make the present invention. Invention content: [0004] The purpose of the first aspect of the present invention is to provide a supported palladium / polyviny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30D01F6/50D01F1/10D04H1/72D01D5/00C07B37/04C07C15/14C07C1/26C07C25/18C07C17/269C07C69/618C07C69/65C07C67/343C07C255/34C07C253/30C07C15/54C07C2/86C07C25/24C07C17/266
Inventor 齐陈泽邵林军季伟鑫曾敏峰
Owner SHAOXING UNIVERSITY
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