Recoverable ligand-free mesoporous polymer palladium catalyst and synthetic method and application thereof

The technology of a palladium catalyst and a synthesis method is applied in the directions of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, catalytic reaction, etc., and can solve the problems of large particle size, low content and uneven distribution of catalyst metal particles. , to achieve the effect of high catalytic activity and stability, high specific surface area, and high catalytic activity

Inactive Publication Date: 2017-01-18
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the following disadvantages: the silica carrier is unstable, easy to decompose under alkaline high-temperature conditions, the introduced functional groups are unevenly distributed, the content is low, time-consuming, and the process is cumbersome, etc.
Since the mesoporous carbon material itself is an inert carrier, the binding force between the noble metal and the precious metal is very weak. The catalyst prepared by the post-loading method adopted in the above-mentioned patent has the problems of large metal particle size, uneven distribution, easy agglomeration, and in the reaction process. Easy to lose and other issues

Method used

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  • Recoverable ligand-free mesoporous polymer palladium catalyst and synthetic method and application thereof
  • Recoverable ligand-free mesoporous polymer palladium catalyst and synthetic method and application thereof
  • Recoverable ligand-free mesoporous polymer palladium catalyst and synthetic method and application thereof

Examples

Experimental program
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Embodiment 1

[0039] Synthesis of phenolic resin precursor solutions. The specific process is as follows: Weigh the mass of the flask and the magnet, accurately add 8.0g of phenol, and heat in a water bath at 42-45°C to completely melt the phenol and become transparent. Add 1.7 g of the prepared 20% NaOH solution dropwise into the phenol solution. Then, 14.2 g of a 37 wt % formaldehyde solution was added dropwise, followed by reflux at 70° C. for 1 hour. After the reflux is completed, cool to room temperature, adjust the solution to neutrality with 2mol / L HCl, distill under reduced pressure under vacuum at 45-50°C to anhydrous state, and cool to room temperature naturally. Weigh the quality of the product, prepare it as a 20wt% ethanol solution, stir evenly and then centrifuge, the obtained supernatant is the phenolic resin precursor, referred to as PF.

Embodiment 2

[0041] Synthesis of a recyclable ligand-free mesoporous polymeric palladium catalyst with a Pd content of 1 wt% and an N content of 8.5 wt%. Dissolve 2.4g P123, 2.0g hydrochloric acid in 10.0g ethanol and stir at 40°C for 15min, 3.74g tetraethyl orthosilicate, 1.65g octadecyldimethyl[3-(trimethoxysilyl)propane Base] (ODDMA) ammonium chloride 5.0g ethanol and stirred at 40°C for 15 minutes, then added 20% PF solution and mixed together and continued to stir for 2 hours. The mixed solution is coated with a film, volatilized at room temperature for 5-8 hours, and then placed in an oven for thermal polymerization at 100°C for 24 hours. Scraped film, calcined at 330°C for 5 hours in a high-purity nitrogen atmosphere to obtain an ordered mesoporous material, marked as 8.5ODDMA-MP (8.5 represents the mass percentage of ODDMA functional groups measured by elemental analysis). 2.0mL 0.05g / mL Na 2 PdCl 4 The ethanol solution and 0.3g 8.5ODDMA-MP were stirred at room temperature for 6...

Embodiment 3

[0045] Synthesis of a recyclable ligand-free mesoporous polymer palladium catalyst with a Pd content of 1 wt% and an N content of 11.5 wt%. Dissolve 2.4g P123, 2.0g hydrochloric acid in 10.0g ethanol and stir at 40°C for 15 minutes, 3.74g tetraethylorthosilicate, 1.87g octadecyldimethyl[3-(trimethoxysilyl) Propyl](ODDMA)ammonium chloride 5.0g ethanol was stirred at 40°C for 45 minutes, and then 20% PF solution was added and mixed together to continue stirring for 2 hours. The mixed solution is coated with a film, volatilized at room temperature for 5-8 hours, and then placed in an oven for thermal polymerization at 100°C for 48 hours. Scraped film, calcined at 275°C for 5 hours in a high-purity nitrogen atmosphere to obtain an ordered mesoporous material, marked as 11.5ODDMA-MP (11.5 represents the mass percentage of ODDMA functional groups measured by elemental analysis). 4.0mL 0.05g / mL Na 2 PdCl 4 The ethanol solution was stirred with 0.3g 11.5ODDMA-MP at room temperature...

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Abstract

The invention relates to a recoverable ligand-free mesoporous polymer palladium catalyst and a synthetic method and application thereof. The catalyst has a two-dimensional hexagonal ordered mesostructure. specific surface area is 250-380 m<2>/g; pore diameter is 3.0-7.0 nm; mass content of a functional phase transfer agent is 8.5-13 wt%; mass content of metal palladium is 1-5 wt%; and particle size of palladium particles is 3-5 nm. The preparation comprises the following steps: adding a surfactant and hydrochloric acid into an organic solvent, stirring and reacting, successively adding a silicon source, quaternary ammonium salt and a carbon source, continuously stirring and reacting; carrying out a thermosetting reaction, and then carrying out high-temperature calcining to prepare a functional mesoporous polymer carrier; and mixing the functional mesoporous polymer carrier and a palladium source, stirring, carrying out suction filtration, washing, carrying out vacuum drying, and carrying out a reduction reaction. The catalyst is applied in aqueous medium catalysis of a Heck reaction between bromobenzene and styrene for generation of stilbene. In comparison with the prior art, the method of the invention is simple; and the catalyst is efficient and stable, can be recycled for many times and has a wide application prospect in the field of industrial catalysis.

Description

technical field [0001] The invention belongs to the technical field of preparation of mesoporous materials, and relates to a catalyst and its synthesis method and application, in particular to a recyclable ligand-free mesoporous polymer palladium catalyst and its synthesis method and application. Background technique [0002] Mesoporous carbon materials have the advantages of large specific surface area, high stability, and uniform pore size. The preparation of metal catalysts using mesoporous carbon as a carrier by post-loading has attracted widespread attention from scientists. However, the mesoporous carbon material itself is an inert carrier, and the binding force between it and the noble metal is very weak. The catalyst prepared therefrom has problems such as large metal particle size, uneven distribution, easy agglomeration, and easy loss during the reaction process. Therefore, it is particularly important to prepare efficient and stable catalysts. [0003] Certain ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06
CPCB01J31/06B01J35/1019B01J35/1061B01J2231/4261
Inventor 万颖段林林张独伊陈尚军
Owner SHANGHAI NORMAL UNIVERSITY
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