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Hydrogenation catalyst and preparation method and application thereof

A technology for the preparation of catalysts and hydrogen, which is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problems of low yield of cyclohexanone oxime and achieve improved Yield, the effect of excellent hydrogenation catalytic performance

Active Publication Date: 2011-07-20
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are problems such as low yield of cyclohexanone oxime in the above process. Therefore, the preparation of a highly active catalyst is the key to improving its selectivity and yield.

Method used

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  • Hydrogenation catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Put 10 grams of carbon nanotubes into 100 milliliters of 20% hydrochloric acid for ultrasonic vibration for 1 hour, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 35% to reflux for 12 hours, filter, wash with deionized water, dry in vacuum and set aside. 1 g of PdCl 2 Dissolve in 50 ml of 4% hydrochloric acid, add the above carbon nanotubes, and add 1 ml of 1% NaOH solution. Stir and soak for 8 hours and then filter. Dry under vacuum at 110°C for 12 hours. Calcined at 200° C. for 4 hours under the protection of nitrogen, reduced by flowing hydrogen at 250° C. for 4 hours, and lowered the temperature under the protection of nitrogen to obtain the catalyst.

[0033] 80 grams of ethylenediamine are added to the reactor, then 12 grams of nitrocyclohexane (purity in 95%) and the hydrogenation catalyst of 1.5 grams of carbon nanotube supported palladium-sodium are added in the kettle, the air is replaced and t...

Embodiment 2

[0035] Put 10 grams of carbon nanotubes into 100 milliliters of 30% hydrochloric acid for ultrasonic vibration for 1 hour, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 60% to reflux for 12 hours, filter, wash with deionized water, dry in vacuum and set aside. 1.5 g PdCl 2 Dissolve in 50 ml of 4% hydrochloric acid, add the above carbon nanotubes, and add 1 ml of 2% NaOH solution. Stir and soak for 8 hours and then filter. Dry under vacuum at 110°C for 12 hours. Calcined at 200° C. for 4 hours under the protection of nitrogen, reduced by flowing hydrogen at 250° C. for 4 hours, and lowered the temperature under the protection of nitrogen to obtain the catalyst.

[0036] 65 grams of ethylenediamine are added to the reactor, then 10 grams of nitrocyclohexane (purity in 95%) and 1 gram of carbon nanotube supported palladium-sodium hydrogenation catalyst are added in the still, the air is replaced and the gas is ch...

Embodiment 3

[0038] Put 10 grams of carbon nanotubes into 100 milliliters of 40% hydrochloric acid for ultrasonic vibration for 1 hour, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 65% to reflux for 12 hours, filter, wash with deionized water, dry in vacuum and set aside. 2.5 g PdCl 2 Dissolve in 50 ml of 4% hydrochloric acid, add the above carbon nanotubes, and add 1 ml of 4% NaOH solution. Stir and soak for 8 hours and then filter. Dry under vacuum at 110°C for 12 hours. Calcined at 250° C. for 4 hours under the protection of nitrogen, reduced with hydrogen at 250° C. for 4 hours, and lowered the temperature under the protection of nitrogen to obtain a catalyst.

[0039] 50 grams of ethylenediamine are added to the reactor, and then 8 grams of nitrocyclohexane (purity is in terms of 95%) and 0.6 gram of carbon nanotube supported palladium-sodium hydrogenation catalyst are added in the kettle, the air is replaced and the...

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PUM

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Abstract

The invention relates to a nitrocyclohexane hydrogenation catalyst and a preparation method thereof, and relates to a method for nitrocyclohexane hydrogenation by using the catalyst. Carbon nano tubes are used as a carrier in the catalyst and carry the following components: at least one VIII family metal and at least one alkali metal in the element periodic table. The catalyst can be used for preparing cyclohexane oxime by nitrocyclohexane hydrogenation; and according to the method, the preparation flow is short, the yield is high, comprehensive cost is low, resources are saved and no waste slag, waste gas or waste liquid is discharged; and the method is a pollution-free production process.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a preparation method of a nitrocyclohexane hydrogenation catalyst and a method for using the catalyst to carry out nitrocyclohexane hydrogenation. Background technique [0002] Hydrogenation of nitro compounds can obtain amine compounds, ketoxime compounds and amide compounds with wide applications. Cyclohexanone oxime can be obtained by hydrogenation of nitrocyclohexane, and cyclohexanone oxime is further subjected to Beckmann rearrangement reaction to generate caprolactam. As a polyamide monomer, caprolactam is an important petrochemical product and chemical fiber raw material, mainly used in the production of polycaprolactam fiber resin, nylon 6 fiber, nylon 6 fiber and other products. It is widely used in textiles, automobiles, electronics, machinery and other fields, and can also be used in the production of antiplatelet drugs such as 6-aminocaproic a...

Claims

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Application Information

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IPC IPC(8): B01J23/58B01J23/78C07C251/44C07C249/10
Inventor 罗和安刘平乐肖艳娟张海科游奎一艾秋红
Owner XIANGTAN UNIV
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