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Preparation method and application of Co and Al2O3 compound nanotube array membrane catalyst

A nanotube array, catalyst technology, applied in the preparation of organic compounds, nanotechnology for materials and surface science, preparation of amino compounds, etc., can solve the problems of long anodizing time, low strength of nanotubes, slow growth, etc. To achieve the effect of controllable pipe diameter and pipe length, smooth pipe wall and fast growth rate

Active Publication Date: 2013-12-25
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The nanotube array prepared by this method has uniform pore size, smooth tube wall, and controllable nanotube pore size and tube length; however, the currently prepared nanotubes have low strength and slow growth (longer anodic oxidation time is required to prepare longer nanotubes)
Moreover, Co and Al were prepared by anodic oxidation 2 o 3 Composite Nanotube Array Membrane Catalyst for the Preparation of 3-Aminomethyl-3,5,5-Trimethylcyclohexylamine Has Not Been Reported yet

Method used

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  • Preparation method and application of Co and Al2O3 compound nanotube array membrane catalyst
  • Preparation method and application of Co and Al2O3 compound nanotube array membrane catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Weigh 100g of cobalt and 400g of aluminum, put these metals into the cavity of an intermediate frequency induction furnace (purchased from Suzhou Hengfu Vacuum Technology Co., Ltd.), heat and melt at 1600°C, pour them into 8cm×10cm molds in batches, and melt to make a thickness of about 2mm Co-Al alloy sheet.

[0039] Prepared with 1wt%NH 4 F, 3200g ethylene glycol solution of 2.8v% distilled water is used as electrolyte, such as figure 2 The device shown: add urea to the electrolyte in batches, the molar ratio of the total amount of urea to the distilled water in the electrolyte is 2:3, after anodizing for 10 minutes, add the first batch of urea, accounting for 10% of the total, anodizing 2.5 After hr, about 8.2% of the total amount was added every 30 minutes; a Co-Al alloy sheet with a thickness of 2mm and a size of 8cm×10cm was used as the anode, high-purity graphite was used as the cathode, and the area ratio of the anode to the cathode was 1:1.3. The distance be...

Embodiment 2

[0042] Weigh 125g of cobalt, 370g of aluminum, 2g of nickel, and 2g of chromium, add these metals into the cavity of an intermediate frequency induction furnace (purchased from Suzhou Hengfu Vacuum Technology Co., Ltd.), heat and melt at 1600°C, and pour them into 8cm×10cm molds in batches , smelted into a Co-Al alloy sheet with a thickness of about 2 mm.

[0043] Prepared with 1.45wt%NH 4 F, 3240g of ethylene glycol solution of 2.8v% distilled water is used as electrolyte, such as figure 2 The device shown: add urea into the electrolyte in batches, the molar ratio of the total amount of urea to the distilled water in the electrolyte is 1:2, after anodizing for 5 minutes, add the first batch of urea, accounting for 12% of the total amount, and anodize for 2hr After that, 8% of the total amount was added every 30 minutes; a Co-Al alloy sheet with a thickness of 2mm and a size of 8cm×10cm was used as the anode, platinum was used as the cathode, and the area ratio of the anode ...

Embodiment 3

[0046] Weigh 100g of cobalt, 394g of aluminum, 3g of molybdenum, and 3g of iron, add these metals into the cavity of an intermediate frequency induction furnace (purchased from Suzhou Hengfu Vacuum Technology Co., Ltd.), heat and melt at 1600°C, and pour them into 8cm×10cm molds in batches , smelted into a Co-Al alloy sheet with a thickness of about 2 mm.

[0047] Preparation contains 0.5wt%NaF, 3600g of diethylene glycol solution of 1.5v% distilled water is used as electrolyte, such as figure 2 The device shown: add urea into the electrolyte in batches, the molar ratio of the total amount of urea to the distilled water in the electrolyte is 3:4, after anodizing for 8 minutes, add the first batch of urea, accounting for 20% of the total amount, and anodize for 2hr After that, add about 8.9% of the total amount every 30 minutes; take the Co-Al alloy sheet with a thickness of 2mm and a size of 8cm×10cm as the anode, ruthenium as the cathode, and the area ratio of the anode to t...

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Abstract

The invention discloses a preparation method and application of a Co and Al2O3 compound nanotube array membrane catalyst. The method comprises the following steps of: carrying out constant-pressure anodic oxidation in a urea-containing electrolyte by taking a Co-Al alloy sheet as an anode and high-purity graphite or an other conducting material as a cathode to prepare an alloy sheet with a Co and Al2O3 compound nanotube array membrane grown on a surface; then crushing the obtained alloy sheet into alloy granules, namely catalyst precursors; reducing the catalyst precursors by using H2 to obtain the Co and Al2O3 compound nanotube array membrane catalyst with uniform apertures, smooth tube walls, controllable pipe lengths and consistent pore path directions. The novel catalyst disclosed by the invention is used for preparing 3-aminomethyl-3,5,5-trimethyl cyclohexylamine (IPDA) by carrying out catalytic hydrogenation on 3-cyano-3,5,5-trimethyl cyclohexanone (IPN) and can achieve the maximal transformation rate of IPN by 100% and achieve the maximal selectivity of IPDA more than 98%.

Description

technical field [0001] The present invention relates to a kind of catalyst preparation method and its application, specifically a kind of Co and Al 2 o 3 Preparation method of composite nanotube array membrane catalyst and its use as fixed bed to prepare 3-aminomethyl-3,5,5-trimethylcyclohexanone with 3-cyano-3,5,5-trimethylcyclohexanone Use of a hydrogenation catalyst for cyclohexylamine. Background technique [0002] 3-Aminomethyl-3,5,5-trimethylcyclohexylamine (isophoronediamine, referred to as IPDA) is a raw material for the preparation of isophorone diisocyanate (IPDI), polyamide, etc.; it can also be used as Epoxy resin curing agent. It is usually composed of 3-cyano-3,5,5-trimethylcyclohexanone (isophorone nitrile, referred to as IPN), NH 3 and H 2 It can be obtained through ammoniation and hydrogenation under the action of a hydrogenation catalyst. Commonly used hydrogenation catalysts are Raney cobalt and shaped cobalt or ruthenium catalysts. [0003] Raney c...

Claims

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Application Information

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IPC IPC(8): B01J23/75C07C211/36C07C209/52C07C209/48C25D11/04B82Y40/00B82Y30/00
Inventor 王磊初乃波黎源叶飞李作金
Owner WANHUA CHEM GRP CO LTD
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