Method for preparing palladium-based composite membranes

A composite membrane and hydrogen permeable technology, applied in separation methods, semi-permeable membrane separation, chemical instruments and methods, etc., can solve problems such as damage, tedious and time-consuming activation and sensitization steps, and increase stability and benefit integrity , the effect of increasing flux

Active Publication Date: 2009-05-27
NANJING TECH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation of a hydrogen-permeable palladium composite membrane in order to solve the conventional activation and sensitization steps which are cumbersome and time-consuming, and the introduction of tin causes damage to the membrane at high temperature, as well as the stability and permeation flux of the membrane. method

Method used

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  • Method for preparing palladium-based composite membranes
  • Method for preparing palladium-based composite membranes
  • Method for preparing palladium-based composite membranes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Preparation of sheet-type supported palladium membrane

[0026] ZrO with a geometric size of 29mm in diameter, 3mm in thickness and an average pore diameter of 0.2μm is used 2 Chip support.

[0027] 1) Preparation of nano-palladium and ceramic mixed slurry: 0.5g nano-palladium powder and 75g TiO with an average particle size of 200nm 2 The powder is added to 500 g of water, and then 5 g of dispersant polyethyleneimine and 10 g of thickener methyl cellulose are added to prepare a uniformly dispersed and stable mixed slurry of nano-palladium and ceramics.

[0028] 2) Preparation of small pore diameter nano-palladium and ceramic composite transition membrane layer: the flake ceramic ZrO 2 The support was slurried in the slurry prepared in step 1) for 10 seconds, dried at 30°C, and then placed in an atmosphere furnace to be calcined at 700°C for 2 hours. The surface of the macroporous support formed with a pore size of 70nm and a thickness of 5μm. Nano-palladium and ...

Embodiment 2

[0030] Example 2: Preparation of Tubular Supported Palladium Membrane

[0031] One end of the tubular support used is glaze-sealed, with a geometric outer diameter of 12mm and a total length of 33cm. The support is α-Al 2 O 3 , The thickness is 2mm, the average pore diameter is 0.2μm, the coatable film length is 5cm, and the area is 18.84cm 2 , The remaining part is coated with glaze and sealed.

[0032] 1) Preparation of nano-palladium and ceramic mixed slurry: 10g nano-palladium powder and 100g ZrO with an average particle size of 300nm 2 The powder is added to 500 g of water, and then 10 g of dispersant polymethacrylic acid and 15 g of thickener methyl cellulose are added to prepare a uniformly dispersed and stable mixed slurry of nano-palladium and ceramics.

[0033] 2) Preparation of small pore diameter nano-palladium and ceramic composite transition membrane layer: the tubular ceramic α-Al 2 O 3 The support was slurried in the slurry prepared in step 1) for 20 seconds, dried...

Embodiment 3

[0035] Example 3: Preparation of Tubular Supported Palladium Membrane

[0036] One end of the tubular support used is sealed with glaze, with a geometric outer diameter of 12mm and a total length of 50cm. The support is α-Al 2 O 3, Thickness 2mm, average pore diameter 0.5μm, coating film length is 33cm, area is 124.34cm 2 , And the remaining part is glaze sealed.

[0037] 1) Preparation of nano-palladium and ceramic mixed slurry: 40g nano-palladium powder and 50g Al with an average particle size of 400nm 2 O 3 Powder and 75g ZrO with an average particle size of 300nm 2 The powder is added to 500 g of water, and 15 g of dispersant sodium dodecylbenzene sulfonate and 20 g of thickener sodium carboxymethyl cellulose are added to prepare a uniformly dispersed and stable mixed slurry of nano-palladium and ceramics.

[0038] 2) Preparation of small pore diameter nano-palladium and ceramic composite transition membrane layer: the tubular ceramic α-Al 2 O 3 The support was slurried in the...

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Abstract

The invention relates to a preparation method for a hydrogen permeation palladium compound membrane; at first, nano palladium powder and ceramic powder are added into water; then a dispersant and a thickening agent are added to prepare the mixed slurry material of the nano palladium and the ceramic which is uniformly dispersed and stable; secondly, a macropore ceramic supporter after hanging slurry in the prepared slurry material is put into an atmosphere furnace for forging at a high temperature; the compound material transition membrane layer of the nano palladium and the ceramic with a small aperture is formed on the surface of the macropore ceramic supporter; then an electroless plating method is used to prepare an outer layer ultra thin compact palladium membrane on the compound material transition membrane layer and finally form an integral hydrogen permeation palladium compound membrane comprising the macropore ceramic supporter, the compound material transition membrane layer with the small aperture and the compact palladium layer. The method avoids the fussy steps of normal activation and sensitization, is convenient in operation, and is broad in practicability; moreover, the prepared palladium membrane is more stable under a high temperature.

Description

Technical field [0001] The invention relates to a method for preparing a hydrogen-permeable palladium membrane, in particular to the preparation of a three-layer integrated palladium composite membrane containing a macroporous support body, a small-pore diameter composite material transition layer and a dense palladium membrane. Background technique [0002] Due to its good hydrogen permeability and high temperature resistance, palladium membranes are not only used as hydrogen separation and purifiers, but also in dehydrogenation and hydrogenation reactors. At present, researchers have conducted a lot of research on palladium and its palladium alloy hydrogen permeable membranes and have achieved remarkable results, mainly focusing on the preparation of palladium membranes and permeation tests. However, the research of palladium membranes still faces some challenges, mainly in: 1. Since palladium is expensive, how to keep the membrane thickness down while ensuring the integrity of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/12B01D53/22C01B3/50
Inventor 范益群徐南平张栋强
Owner NANJING TECH UNIV
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