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Composite metal palladium membrane or alloy palladium membrane and its preparing method

A composite metal and palladium membrane technology, which is applied in separation methods, chemical instruments and methods, metal material coating technology, etc., can solve the problems of difficult formation of dense palladium membranes, reduced hydrogen permeation selectivity, and low hydrogen permeation volume, and achieves The effect of low manufacturing cost, high hydrogen permeability and simple process

Inactive Publication Date: 2005-07-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 2) Surface modification Due to the inhomogeneity of the surface of the porous bottom membrane, especially the inhomogeneity of the pore distribution, there will inevitably be some large pores or even defects on the surface of the bottom membrane, and it will be difficult to form a dense palladium film in the subsequent film formation process. Reduce hydrogen permeation selectivity
Surface modification is the key to preparing a composite palladium membrane with high hydrogen permeability and high hydrogen permeability selectivity. For the first modification method, a thin layer of porous material is dip-coated on the surface of the porous bottom membrane by coating technology or casting technology. , such as γ-Al 2 o 3 For porous materials, if the palladium film can be controlled to form only on the outer surface of the coated thin-layer porous material, a composite palladium film material with high hydrogen permeability can be prepared, but unfortunately, due to capillary action, the electroless plating solution is inevitably into the pores of the porous material, Pd 2+ The ions are continuously reduced and deposited in the pores of the porous material until the pores are filled and the electroless plating solution cannot enter. In this way, the surface coating that originally has a porous structure will cause secondary damage to hydrogen permeability due to the deposition of metal palladium in the pores. resistance, resulting in lower hydrogen permeation
For the second modification method, the pores of the porous bottom membrane, especially the macropores or defects, are filled with porous materials, such as γ-Al 2 o 3 , ZrO 2 , SiO 2 , CeO 2 and other porous materials to modify the surface of the base film. Similarly, due to capillary action, the electroless plating solution inevitably enters into porous materials such as γ-Al 2 o 3 , ZrO 2 , SiO 2 , CeO 2 In such channels, Pd 2+ The ions are continuously reduced and deposited in the pores of the porous material until the pores are filled and the electroless plating solution cannot enter. In this way, the material filled in the porous bottom film originally has a porous structure, but due to the pores being deposited by palladium, the same Form secondary resistance to hydrogen permeation, resulting in lower hydrogen permeation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of colloid: drop aluminum nitrate aqueous solution and sodium carbonate aqueous solution into a beaker at 55°C at the same time, control the pH value to about 8, and prepare basic aluminum carbonate colloid, wash the prepared colloid with distilled water 6 times, and set aside . The above-mentioned sodium carbonate aqueous solution is respectively replaced with potassium carbonate, ammonia water, sodium hydroxide and potassium hydroxide aqueous solution as a precipitating agent, and the corresponding colloid or precipitation is prepared by the same procedure.

[0035] Surface modification of the porous bottom membrane: use the alumina porous ceramic tube as the bottom membrane. First, use dilute hydrochloric acid and dilute sodium hydroxide to clean the porous bottom membrane material, then rinse it with distilled water, and then wash it with CCl 4 After cleaning and drying, the cleaned alumina porous ceramic tube is immersed in the colloidal solution under ...

Embodiment 2

[0048] The preparation of colloid: with embodiment 1.

[0049] Surface modification of the porous bottom membrane: a porous stainless steel tube is used as the bottom membrane, and the modification method is the same as in Example 1.

[0050] The preparation of composite palladium membrane: with embodiment 1.

[0051] Table 2 shows the Al(NO 3 ) 3 As raw materials, the colloid prepared by different precipitants was used to modify the surface of the bottom membrane of the porous stainless steel tube to form the hydrogen permeability of the composite palladium membrane.

[0052] Table 2 Hydrogen Permeability of Composite Metal Palladium Membrane

[0053] Hydrogen permeability

[0054] Precipitant Hydrogen Permeability Selectivity H 2 / N 2

[0055] m 3 / m 2 .h.bar

[0056] Sodium carbonate 38 4400

[0057] Potassium carbonate 34 5100

[0058] Ammonia 29 3500

[0059] Sodium hydroxide 33 3900

[0060]...

Embodiment 3

[0062] Preparation of colloid: Drop cerium nitrate aqueous solution and sodium carbonate aqueous solution into a beaker at 55°C at the same time, control the pH value to about 9, prepare basic cerium carbonate colloid, wash the prepared colloid with distilled water 5 times, and set aside . The above-mentioned sodium carbonate aqueous solution is respectively replaced with potassium carbonate, ammonia water, sodium hydroxide and potassium hydroxide aqueous solution as a precipitating agent, and the corresponding colloid or precipitation is prepared by the same procedure.

[0063] Surface modification of the porous bottom membrane: use the alumina porous ceramic tube as the bottom membrane. First, use dilute hydrochloric acid and dilute sodium hydroxide to clean the porous material bottom membrane, then rinse it with distilled water, and then wash it with CCl 4 After washing and drying, the cleaned alumina porous ceramic tube is immersed in the colloidal solution under vacuum co...

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Abstract

The present invention relates to a composite metal palladium membrane or alloy palladium membrane, it is characterized by that the external surface of porous base membrane is almost completely covered with metal palladium membrane or alloy palladium membrane, and said metal palladium membrane or alloy palladium membrane can be deposited in the pore channel of base membrane in small quantity, and its preparation method includes the steps of utilizing sensibilization and activation process to form palladium nucleus on the external surface of porous base membrane and adopting chemically-plating process to form palladium membrane. Said invention also provides the characteristics of said preparation method.

Description

Technical field: [0001] The invention relates to a composite metal palladium film or an alloy palladium film, and specifically provides a composite metal palladium film or an alloy palladium film with high hydrogen permeability and a special preparation technology thereof. Background technique: [0002] Palladium membrane or alloy palladium membrane has the performance of selectively permeating hydrogen, so it has broad application prospects in the field of hydrogen separation. The preparation and application of palladium membranes have been researched for decades. However, no breakthrough has been made in the preparation of palladium membranes, and the hydrogen permeability of the prepared palladium membranes has always been low. [0003] In the initial stage of research, people only prepared pure palladium membranes, that is, unsupported palladium membranes. Due to limitations such as mechanical strength, the thickness of the membranes is generally required to be greater ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/22B01D67/00B01D69/02B01D69/10B01D71/02C01B3/50
CPCB01D71/022C01B3/505B01D53/228B01D69/02B01D67/0069B01D69/10B01D69/105Y10T428/12479Y10T428/249981B01D69/106B01D71/02231B01D69/1213B01D67/0083B01D69/108B01D2323/081
Inventor 徐恒泳侯守福李文钊江魁袁立祥
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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