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Y2 O3 nanometer carrier Ag catalyst, its synthesis and use

A synthesis method and catalyst technology, which are applied in the field of new high-efficiency catalysts for in-situ supported Ag nanocrystals on single crystal Y2O3 nanobelts, can solve the problems of easy accumulation of hydroxylamine, potential safety hazards, low activity and selectivity, etc. The effect of shortened time, simple and safe operation process

Inactive Publication Date: 2007-09-05
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the invention is to design the solid-liquid phase chemical reaction route thermal decomposition Y (NO 3 ) 3 .6H 2 O solid preparation Y 2 o 3 single crystal nanoribbons while utilizing AgNO 3 The thermal decomposition reaction of the solid, in the resulting Y 2 o 3 In-situ loading of Ag nanocrystals on single crystal nanobelts, constructing a new Ag nanocrystal-supported catalyst for catalytic hydrogenation of various aromatic nitro compounds to prepare various amine-based compounds, solving the current catalytic hydrogenation catalysts for aromatic nitro compounds There are three thorny problems: (1) the activity and selectivity are not high; (2) hydroxylamine is easy to accumulate, and there are potential safety hazards; (3) it is easy to dechlorinate or hydrogenate other active functional groups at the same time

Method used

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  • Y2 O3 nanometer carrier Ag catalyst, its synthesis and use
  • Y2 O3 nanometer carrier Ag catalyst, its synthesis and use
  • Y2 O3 nanometer carrier Ag catalyst, its synthesis and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a clean and dry 250 ml round bottom flask or three-necked flask, add 2.05 g of yttrium nitrate hexahydrate (Y(NO 3 ) 3 .6H 2 O) solid, 10 milliliters of dodecylamine and 10 milliliters of octadecene, then rise to 320 ℃ with the rate of 8 ℃ per minute from room temperature, after reacting for 20 minutes, add 100 milligrams of silver nitrate (AgNO 3 ) solid, after continuing to react for 10 minutes, turn off the heating source and cool down to room temperature naturally. Disperse the product with 20 milliliters of n-heptane or n-hexane, then add 10 milliliters of absolute ethanol for precipitation, and finally centrifuge, repeat this operation 3-7 times, and vacuum-dry the final product at 60°C for 4 hours for use in Analysis and Characterization.

[0029] The components and phase structure of the product were analyzed by X-Ray powder diffraction (Fig. 1), which proved that there was Y in the product. 2 o 3 and Ag two components. X-Ray photoelectron spectroscopy ...

Embodiment 2

[0034] In a clean and dry 250 ml round bottom flask or three-necked flask, add 1.58 g of yttrium nitrate hexahydrate (Y(NO 3 ) 3 .6H 2 O) solid, 6 milliliters of dodecylamine and 8 milliliters of octadecene liquid, then the reactor was raised to 310 DEG C at a rate of 12 DEG C per minute from room temperature, and after 15 minutes of reaction, 30 milligrams of silver nitrate (AgNO 3 ) solid, after continuing to react for 10 minutes, turn off the heating source and cool down to room temperature naturally. Disperse the product with 20 milliliters of n-heptane or n-hexane, then add 10 milliliters of absolute ethanol for precipitation, and finally centrifuge, repeat this operation 3-7 times, and vacuum-dry the final product at 60°C for 4 hours for use in Analysis and Characterization.

[0035] The products were analyzed and characterized by X-Ray powder diffraction, X-Ray photoelectron spectroscopy and transmission electron microscopy. Using the catalytic hydrogenation reactio...

Embodiment 3

[0037] In a clean and dry 250 ml round bottom flask or three-necked flask, add 5.0 g of yttrium nitrate hexahydrate (Y(NO 3 ) 3 ) solid, 12 milliliters of dodecylamine and 15 milliliters of octadecene liquid, then raise the reactor from room temperature to 320 degrees Celsius at a rate of 6 degrees per minute in a sand bath, and after 25 minutes of reaction, quickly add 160 milligrams of nitric acid Silver (AgNO 3 ) solid, after continuing to react for 10 minutes, turn off the heating source and cool down to room temperature naturally. Disperse the product with 20 milliliters of n-heptane or n-hexane, then add 10 milliliters of absolute ethanol for precipitation, and finally centrifuge, repeat this operation 3-7 times, and vacuum-dry the final product at 60°C for 4 hours for use in Analysis and Characterization.

[0038] The products were analyzed and characterized by X-Ray powder diffraction, X-Ray photoelectron spectroscopy and transmission electron microscopy. Using the...

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Abstract

A Y2O3 nanobelt carried Ag catalyst for catalytic hydrogenation reaction with high activity, selectivity and safety is prepared through proportionally adding hexahydrated yttrium nitrate solid, dodecylamine and octadecene into reactor, heating to 300-320 deg.C at the speed of 5-15 deg.C per min, reacting, quickly adding AgNO3, continuous reacting, natural cooling, washing with heptane and alcohol 5-7 times, and vacuum drying.

Description

1. Technical field [0001] The present invention relates to a kind of single crystal Y 2 o 3 A new type of high-efficiency catalyst supported by nanobelts in situ supporting Ag nanocrystals, a gram-scale preparation method of the catalyst and its application in catalytic hydrogenation reactions of various aromatic nitro compounds. 2. Background technology [0002] Efficient and selective catalytic hydrogenation of aromatic nitro compounds is of great significance in the industrial field, because its product aromatic amine is an important class of chemical intermediates, and has important roles in the fields of dyes, polyurethane rubber, agrochemicals and pharmaceuticals. application. Pt, Pd, Ru, Rh, Ir and Raney Ni are commonly used catalysts to catalyze the hydrogenation of aromatic nitro compounds. Although the activity is high, the selectivity is not high, and there are three thorny problems: 1. Halogenated aromatic nitro compounds 2. Other active groups are easy to be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63C07C209/32
Inventor 徐正韩敏李保军
Owner NANJING UNIV
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