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Palladium-supported mesoporous carbon-silicon dioxide catalyst material as well as preparation method and application

A technology of silica and catalysts, which is applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., and can solve problems such as catalyst performance verification and unused functionalized catalysts , to achieve the effect of high yield, low cost and excellent structure

Active Publication Date: 2019-08-02
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent has not been used in the preparation of amino functionalized carbon-silica supported palladium catalyst, and the prepared functionalized catalyst has not been used in the reaction to verify the performance of the catalyst

Method used

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  • Palladium-supported mesoporous carbon-silicon dioxide catalyst material as well as preparation method and application
  • Palladium-supported mesoporous carbon-silicon dioxide catalyst material as well as preparation method and application
  • Palladium-supported mesoporous carbon-silicon dioxide catalyst material as well as preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Put 6.0g of phenol in a three-necked flask and heat it in a water bath at 50°C to make it a transparent liquid; prepare 3.70g of sodium hydroxide solution with a mass percentage of 20%, and slowly drop it into the liquid. After 10 minutes, 15.0 g of formaldehyde solution with a mass percentage of 37% was added, refluxed at 90° C. for 1 hour, cooled to room temperature, and adjusted to neutral pH. Distill under reduced pressure at 45-50° C. to obtain the residue as the target product phenolic resin. After cooling to room temperature, the ethanol or ether solutions of the phenolic resin prepolymer with a mass percent concentration of 20-45wt% are respectively prepared for use.

Embodiment 2

[0043] At 40-60°C, 2.0g of F127(EO 106 PO 70 EO 106 ) surfactant was dissolved in 10.0 g of dichloromethane solution, then 1 g of 0.4 mol / L hydrochloric acid solution was added, and stirred for pre-hydrolysis for 1 hour to obtain solution A. At the same temperature, 3.0 g of ethyl orthosilicate and 1.2 g of N,N-bis(3-trimethoxysilylpropyl)urea were successively added to 10.0 g of dichloromethane solution, and stirred for 1 hour to obtain solution B. After solution A and solution B were mixed, 20 wt% of the phenolic resin synthesized in step 1 was added, and magnetically stirred for 4 hours. A clear, pale yellow transparent solution was obtained. Spread the above solution evenly on the surface of the glass petri dish, let it stand at room temperature for 2 hours, then raise the temperature to 100°C for 24 hours, and scrape off the light yellow transparent film, which is the prefabricated material.

[0044] The obtained prefabricated material was calcined with an inert prote...

Embodiment 3

[0046] At 40-60°C, 2.0g of P123(EO 20 PO 70 EO 20 ) surfactant was dissolved in 10.0 g of tetrahydrofuran solution, and then 1 g of 1 mol / L hydrochloric acid solution was added, and stirred for pre-hydrolysis for 1 hour to obtain solution A. At the same temperature, 3.6 g of propyl orthosilicate and 1.0 g of 3-ureidopropyltriethoxysilane were successively added to 10.0 g of tetrahydrofuran solution, and stirred for 1 hour to obtain solution B. After solution A and solution B were mixed, 20 wt% of the phenolic resin synthesized in Example 1 was added, and magnetically stirred for 4 hours. A clear, pale yellow transparent solution was obtained. Spread the above solution evenly on the surface of the glass petri dish, let it stand at room temperature for 2 hours, then raise the temperature to 100°C for 24 hours, and scrape off the light yellow transparent film, which is the prefabricated material. The prefabricated material was calcined with an inert protective gas at 400°C fo...

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Abstract

The invention relates to a palladium-supported mesoporous carbon-silicon dioxide catalyst material as well as a preparation method and application. The method comprises the following steps: taking soluble resin as a carbon source, an organic silicon source as a source of organic functional groups, and a surfactant as a template; adding an inorganic silicon source; preparing an amino functionalizedordered mesoporous polymer-silicon oxide composite material according to a multi-component co-assembly method; calcining to obtain an amino functionalized mesoporous carbon-silicon dioxide compositematerial; further, impregnating and supporting Pd; supporting the Pd on a mesoporous composite material; finally, reducing to obtain a product. Compared with the prior art, the preparation method disclosed by the invention is simple and feasible; in addition, the prepared palladium catalyst is used for the reaction of catalyzing 8-methylquinoline and methanol to synthesize 8-methoxymethyl-quinoline and has high yield.

Description

technical field [0001] The invention belongs to the technical field of preparation of mesoporous materials, and in particular relates to a mesoporous carbon-silicon dioxide catalyst material loaded with palladium, a preparation method and application thereof. Background technique [0002] Palladium catalyst is an important reaction catalyst in the process of organic synthesis, and is widely used in the activation of organic C-H bonds and the production of fine chemicals. Palladium on carbon is a widely used industrial catalyst. However, since the carbon material itself is an inert carrier, the binding force between it and palladium is weak, and the catalyst has problems such as metal palladium loss, agglomeration, and easy poisoning and deactivation during the reaction process. Therefore, it is of great significance to invent a structurally stable, low-cost palladium catalyst to replace the traditional palladium-carbon catalyst. [0003] Ordered mesoporous materials have h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J23/44B01J37/02B01J37/08B01J37/16B01J37/18B01J35/10C07D215/26
CPCB01J27/24B01J23/44B01J37/0201B01J37/0018B01J37/16B01J37/18C07D215/26B01J35/617B01J35/638B01J35/633B01J35/635B01J35/647B01J35/615
Inventor 万颖赵小瑞
Owner SHANGHAI NORMAL UNIVERSITY
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