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Preparation method of palladium membrane

The technology of a palladium membrane and a palladium alloy membrane, which is applied in the field of hydrogen separation, can solve the problems of reducing the hydrogen permeability and service life of the membrane, affecting the service life of the palladium membrane, etc., and achieves the effects of superior performance, easy operation and simple equipment.

Active Publication Date: 2014-04-16
RISON HI TECH MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there have been many related reports, mainly using chemical methods for repairing. By repairing membrane defects, the selectivity has been significantly improved, and the thickness of the film layer has been increased less. However, the repaired palladium composite membrane is also very easy to The above-mentioned defects will inevitably affect the service life of the palladium membrane, and it is very important to reduce the regeneration defects during the use of the palladium membrane
Closed pores at the intersection of grain boundaries in the membrane layer will also reduce the hydrogen permeability and service life of the membrane, and there are few reports in the literature on eliminating this type of pores

Method used

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Experimental program
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Effect test

Embodiment 1

[0022] Adopting the present invention to prepare a palladium membrane on the outer surface of a tubular porous ceramic substrate comprises the following steps:

[0023] (1) The substrate used is a tubular porous ceramic with an outer diameter of 13 mm, an inner diameter of 8 mm, a length of 80 mm, and a maximum pore diameter of 2.6 μm on the surface. The substrate is cleaned and dried for later use.

[0024] (2) Using SnCl 2 / PdCl 2 The activation method is used to activate the outer surface of the above-mentioned substrate, and the sensitization solution contains SnCl 2 4g / L, hydrochloric acid 1ml / L, the activation solution contains PdCl 2 0.2g / L, hydrochloric acid 1ml / L, after sensitization and activation treatment 4 times.

[0025] (3) Immerse the activated substrate into the plating solution to start electroless plating. The composition of the plating solution: PdCl 2 5g / L, Na 2 EDTA50g / L, ammonia water 250ml / L, bath temperature 30°C. The reducing agent is 0.4mol / L ...

Embodiment 2

[0030] Adopting the present invention to prepare a palladium membrane on the outer surface of a tubular porous stainless steel substrate comprises the following steps:

[0031] (1) The substrate used is tubular porous stainless steel with an outer diameter of 12 mm, an inner diameter of 7 mm, a length of 80 mm, and a maximum pore diameter of 6.5 μm on the surface. The substrate is cleaned and dried for later use.

[0032] (2) with the step (2) (3) (4) (5) of embodiment 1, but stop electroless plating when palladium film thickness reaches 10 μ m, calculate according to the weight gain of substrate, palladium film thickness is 9.7 μ m, records Its nitrogen flux is 3.8ml / min. The flux after pressure sintering is reduced to 1.35ml / min.

[0033] (3) Carry out chemical repair on the above-mentioned palladium film, and the repair liquid is selected from 0.001mol / L Pd(OH) 2 The colloid and the membrane tube are immersed in the repair solution to make the Pd(OH) 2 The colloid penet...

Embodiment 3

[0035] Adopt the present invention to prepare palladium film on sheet type porous ceramic substrate, comprise the following steps:

[0036] (1) The substrate used is a circular sheet-type porous ceramic with a diameter of 30 mm, a thickness of 2 mm, and a maximum diameter of surface pores of 2.5 μm. The substrate is cleaned and dried for later use.

[0037] (2) Steps (2) (3) (4) (5) (6) with embodiment 1. However, based on the weight gain of the substrate, the thickness of the palladium film is 4.9 μm, and the measured nitrogen flux is reduced from 0.51ml / min to 0.22ml / min after pressure sintering. After the hydrazine repair method, the nitrogen flux was 0.10ml / min, and the nitrogen flux was 0.18ml / min after the palladium membrane was used for 900h.

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Abstract

The invention relates to a preparation method of a palladium membrane. The preparation method of the palladium membrane is characterized in that a layer of palladium or palladium alloy membrane is deposited on the surface of a porous matrix by adopting a chemical plating method; the prepared palladium membrane is sintered in an inert atmosphere with certain positive pressure; rearrangement of micro-nano scale palladium grains is facilitated; a closed hole at the grain boundary intersection and isolated micro-pores in the grains are compact, and then the residual defects are filled in a chemical repairing manner. By adopting the method, the palladium membrane which is compact and uniform in film, long in service life and high in hydrogen permeability can be prepared.

Description

technical field [0001] The invention relates to a preparation method of a palladium membrane, which is used for preparing a palladium membrane with extremely high film density, excellent hydrogen permeability and long service life, and can be widely used in hydrogen separation. Background technique [0002] Ultra-high-purity hydrogen is widely used in solar photovoltaics, fuel cells, semiconductors, LED manufacturing and other industries, and its application is inseparable from the separation and purification of hydrogen. The separation of hydrogen includes pressure swing adsorption (PSA), temperature swing adsorption (TSA), cryogenic method and membrane method, among which membrane method has become the research field because of its advantages of less investment, low energy consumption, high efficiency and convenient operation. Hot spots, this method is especially suitable for small hydrogen production systems. Membrane materials that can be used for hydrogen separation in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00C23C18/44C23F17/00
Inventor 黄彦魏浩俞健魏磊丁维华黎月华黄韬
Owner RISON HI TECH MATERIALS CO LTD
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