Normal-pressure preparation method and application of block nanometer silver loading silica aerogel catalyst

A technology of silica and airgel, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problem of not meeting the requirements of green chemistry, the high price of silver nanoparticles, and the impact of agglomeration on catalytic performance and other problems, to achieve the effect of completely pollution-free synthesis process, good catalyst stability and good catalytic effect

Inactive Publication Date: 2017-02-15
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods mainly have the following problems: Although the iron / acid chemical reduction method is simple in process and mature in technology, the consumption of iron powder and acid in production is relatively large, and a large amount of iron sludge and waste water are produced, which pollutes the environment and does not meet the requirements of green chemistry.
However, the direct use of silver nanoparticles is not only expensive and costly, but also prone to agglomeration under the influence of intermolecular forces affecting its catalytic performance, easy to sinter under high temperature conditions to deactivate the catalyst, and low reuse rate

Method used

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  • Normal-pressure preparation method and application of block nanometer silver loading silica aerogel catalyst
  • Normal-pressure preparation method and application of block nanometer silver loading silica aerogel catalyst
  • Normal-pressure preparation method and application of block nanometer silver loading silica aerogel catalyst

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Experimental program
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Effect test

Embodiment 1

[0043] (1) At room temperature, measure 3mL of tetraethylorthosilicate, 4.5mL of acetonitrile, 2mL of deionized water in a beaker and stir it evenly, mark it as A; Measure 4.5mL of acetonitrile and 1mL of aminopropyltriethyl Stir the oxysilane in a beaker and mark it as B. The stirring time is 10 minutes. The mixed solution in beaker B is quickly added to beaker A and stirred for 10 minutes. When the solution has a turbid color, stop the stirring, take it out and let it stand until it returns to room temperature, and a wet gel will form. After aging at room temperature for 2 hours, 20 mL of acetonitrile was added for aging for 10 hours.

[0044] (2) Prepare 20 mL of acetonitrile solution of trimethylhexamethylene diisocyanate with a mass fraction of 10%, soak the wet gel with the prepared 20 mL solution, and place it in a water bath at 40°C for 24 hours.

[0045] (3) Take out the cross-linked gel, add 20 mL of acetonitrile, leave it at room temperature for 24 hours, seal it with a...

Embodiment 2

[0056] (1) Measure 3mL of tetraethylorthosilicate, 4.5mL of acetonitrile, 2mL of deionized water in a beaker and stir evenly, place in a mixture of ice and water, labeled A; Measure 4.5mL of acetonitrile and 1mL of aminopropyl Triethoxysilane was stirred evenly in a beaker and marked as B. The stirring time is 10 minutes. The mixed solution in beaker B is quickly added to beaker A and stirred for 10 minutes. When the solution has a turbid color, stop the stirring, take it out and let it stand until it returns to room temperature, and a wet gel will form. After aging at room temperature for 2 hours, 20 mL of acetonitrile was added for aging for 11 hours.

[0057] (2) Prepare 20 mL of acetonitrile solution of trimethylhexamethylene diisocyanate with a mass fraction of 10%, soak the wet gel with the prepared 20 mL solution, and place it in a water bath at 40°C for 24 hours.

[0058] (3) Take out the cross-linked gel, add 20 mL of acetonitrile, leave it at room temperature for 24 hour...

Embodiment 3

[0063] (1) Measure 3mL of tetraethylorthosilicate, 4.5mL of acetonitrile, 2mL of deionized water in a beaker and stir evenly, place in a mixture of ice and water, labeled A; Measure 4.5mL of acetonitrile and 1mL of aminopropyl Triethoxysilane was stirred evenly in a beaker and marked as B. The stirring time is 10 minutes. The mixed solution in beaker B is quickly added to beaker A and stirred for 10 minutes. When the solution has a turbid color, stop the stirring, take it out and let it stand until it returns to room temperature, and a wet gel will form. After aging at room temperature for 2 hours, 18 mL of acetonitrile was added for aging for 10 hours.

[0064] (2) Prepare 18 mL of a 10% mass fraction of trimethylhexamethylene diisocyanate in acetonitrile solution, soak the wet gel with the prepared 18 mL solution, and place it in a 40°C water bath for 24 hours.

[0065] (3) Take out the cross-linked gel, add 18 mL of acetonitrile, leave it at room temperature for 24 hours, seal ...

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Abstract

The invention discloses a preparation method of a block nanometer silver loading silica aerogel catalyst, and an application of the catalyst to preparation of 4-aminophenol from 4-nitrophenol through catalytic hydrogenation. A sol-gel method is adopted, and trimethylhexamethylene diisocyanate is used for cross-linking to obtain enhanced silica-based wet gel, which is dried at a normal pressure to prepare silica-based aerogel with the block shape well kept. The impregnation method is used to prepare the nanometer silver loading silica aerogel catalyst. The catalyst can have the block shape well kept. Silver is loaded on silica aerogel having a three-dimensional network porous structure, so that the dispersity of silver is increased. The chemical stability of the catalyst and the catalytic activity of the catalyst are improved. Further, the block is convenient to recycle and reuse. The catalyst is adopted to catalyze 4-nitrophenol to prepare 4-aminophenol through hydrogenation and is high in catalytic activity and good in stability.

Description

[0001] Technical neighborhood [0002] The invention belongs to the field of catalysts, and relates to a preparation method of a massive silica aerogel supported nano silver catalyst and its application in the preparation of 4-aminophenol by the catalytic hydrogenation of 4-nitrophenol. Background technique [0003] 4-nitrophenol is a non-biodegradable and toxic environmental pollutant, but 4-aminophenol is an important chemical raw material and pharmaceutical intermediate, which is widely used in the synthesis of pesticides, dyes, rubber additives, photoelectric functional molecules, etc. Fine chemicals and antipyretic and analgesic drugs. There are currently three methods for preparing 4-aminophenol: iron / acid chemical reduction method, electrochemical reduction method and catalytic hydrogenation method. These methods mainly have the following problems: although the process of iron / acid chemical reduction is simple and the technology is mature, the consumption of iron powder and...

Claims

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Application Information

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IPC IPC(8): B01J23/50C07C213/00C07C215/76
CPCY02P20/584B01J23/50B01J37/0201C07C213/00C07C215/76
Inventor 马丽蓉朱建军冯金汪强谢吉民
Owner JIANGSU UNIV
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