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Preparation method and application of fixed bed framework metal catalyst

A framework metal and catalyst technology, which is applied in the field of hydrogenation of organic unsaturated compounds, can solve the problems of unfavorable alloy activation and catalyst activity improvement, catalyst strength is difficult to guarantee, and is not suitable for hydrogenation reaction, etc., to achieve excellent flame retardancy Sexuality and chemical inertness, saving active metal resources, solving the effect of high calcination temperature

Inactive Publication Date: 2013-07-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that only part of the catalyst has a macroporous structure, so it is not suitable for the hydrogenation reaction of larger molecules
[0008] Based on the above patent reports, after the active metal aluminum alloy is formed, it needs to be roasted at a high temperature of 700-900°C to improve the strength. If α-Al is formed during the roasting process 2 o 3 , it is not conducive to the activation of the alloy and the improvement of the catalyst activity, if the α-Al cannot be generated during the roasting process 2 o 3 , then only surface activation can be carried out, otherwise the catalyst strength is difficult to guarantee

Method used

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  • Preparation method and application of fixed bed framework metal catalyst
  • Preparation method and application of fixed bed framework metal catalyst
  • Preparation method and application of fixed bed framework metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: preparation of catalyst A

[0018] Weigh 16.7g of polytetrafluoroethylene concentrate and 2g of polyacrylamide to prepare a slurry, then add 90g of nickel-aluminum alloy powder with a particle size of 200-240 mesh (mass content: nickel 47.3%, aluminum 48.2%, iron and other elements 4.5%), fully kneaded, extruded into a cylindrical strip with a diameter of 1.8mm, dried under an infrared lamp, dried at 120°C for 3h, and then heat-treated at 250°C for 3h under an argon atmosphere. The activation conditions are: put 50g of the above particles into 250ml of NaOH solution with a mass percentage concentration of 20%, raise the temperature to 70°C for 2h, wash with deoxygenated deionized water until the pH value is 7-8, and then wash with absolute ethanol Replace deionized water to prepare catalyst A, which is stored in absolute ethanol.

Embodiment 2

[0019] Embodiment 2: preparation of catalyst B

[0020] Weigh 12.5g of polytetrafluoroethylene concentrate and 2.5g of carboxymethyl cellulose to prepare a slurry, then add 90g of nickel-aluminum alloy powder with a particle size of 200-240 mesh (mass content: nickel 52.1%, aluminum 43.8%, molybdenum and other elements 4.1%), fully ground and evaporated to dryness, pressed into a cylindrical sheet with a diameter of 3.0mm and a height of 2.0mm, dried at 120°C for 3h, and then heat-treated at 300°C for 2h under an argon atmosphere. The activation conditions are: put 50g of the above particles into 350ml of a solution with a mass percent concentration of 15% NaOH, raise the temperature to 80°C for 2 hours, wash with deoxygenated and deionized water until the pH value is 7-9, and then wash with absolute ethanol Replace deionized water to prepare catalyst B, which is stored in absolute ethanol.

Embodiment 3

[0021] Embodiment 3: preparation of catalyst C

[0022] Prepare 50g of nickel-aluminum alloy powder with a particle size of 200-240 mesh (mass content: nickel 47.3%, aluminum 48.2%, iron and other elements 4.5%), 10g of polytetrafluoroethylene concentrate and 2.5g of carboxymethyl cellulose Slurry, and then smear the slurry on nickel foam (area density 320g / m 2 ) surface, the viscosity of the slurry should enter the interior of the nickel foam network structure. Dry at room temperature, dry at 120°C for 3 hours, then heat-treat at 250°C for 2 hours in a tube furnace under an argon atmosphere, and cut the nickel foam into 2-3mm square particles. The activation conditions are: 20g foamed nickel coated nickel-aluminum alloy particles, 30g NaOH to prepare a solution with a mass percentage of 20%, activate at 80°C for 2h, then wash with deoxygenated and deionized water until the pH value is 7-8, and then wash with absolute ethanol Replace deionized water to prepare catalyst C, wh...

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Abstract

The invention discloses a preparation method and the application of a fixed bed framework metal catalyst. The method includes: adopting a halogen substituted organic polymer as a coupling agent of active metal aluminum alloy powder, preparing aluminum alloy powder containing transition metal in VIII class, IB class or VB class into particles in certain shapes, adopting forming methods like direct kneading method for band extrusion or tabletting or coating method for attaching the alloy powder on the surface of a carrier with certain strength, subjecting the formed particles to heat treatment under certain atmosphere for improving strength, and activating with an inorganic alkaline solution to obtain the fixed bed framework metal catalyst. The catalyst prepared by the method can be used for fixed bed hydrogenation reaction of unsaturated organic compounds like aldehyde, ketone, ester, nitrile, olefine, aromatic and nitro compounds. The aluminum alloy particles are low in heat treatment temperature, the strength of the carrier can be fully utilized by the coating method, and the aluminum alloy particles after being activated have excellent hydrogenation activity and stability.

Description

Technical field: [0001] The invention relates to a preparation method of a skeleton metal catalyst used for hydrogenation of a fixed bed, and the application of the catalyst in the field of hydrogenation of organic unsaturated compounds. Background technique: [0002] In order to solve the various shortcomings in the use of traditional powdered skeleton (Raney) metal catalysts, such as only used in suspended bed or batch operation, it is easy to be deactivated due to oxidation or pulverization loss during operation, and it is difficult to separate from the reaction system Recycle for reuse. Researchers are trying to make skeleton metal catalysts into granular catalysts with certain mechanical strength, which can be applied to fixed bed continuous operation. [0003] The preparation methods of US4826799 and US4895994 are: after kneading and molding the active metal aluminum alloy, aluminum, organic polymer binder and channel template agent, roasting in air at a temperature h...

Claims

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Application Information

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IPC IPC(8): B01J25/02C07C211/12C07C209/48C07D307/12C07D307/44C07C13/61C07C5/03
Inventor 赵会吉刘亚文刘晓彤路兴禄刘晨光
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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