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Preparation method and application of palladium-ceramic-palladium bilayer composite membrane material

A technology of composite membranes and membrane materials, applied in the direction of separation methods, chemical instruments and methods, membrane technology, etc., can solve the possibility of increasing the impurity gas permeation membrane materials, palladium membrane is difficult to cover the surface carrier, single-layer palladium membrane Defects are difficult to control and other problems, to achieve the effect of reducing equipment investment capital, reducing the probability of generation, and high hydrogen permeability

Inactive Publication Date: 2018-06-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional supported metal palladium membrane adopts a single-layer loading mode. Although the usage of precious metals is reduced and the production cost is reduced, this composite palladium membrane changes the hydrogen permeation process from a bulk phase diffusion control step to an external one. Diffusion control, which increases the mass transfer resistance of hydrogen in the process of external diffusion [3]
In addition, due to the loose and porous structure of the carrier in the single-layer coating process, it is difficult for the palladium membrane to cover the surface carrier perfectly and without defects, which will cause defects, affect the integrity of the membrane material, and increase the penetration of impurity gases through the membrane material. Possibility, which in turn affects the application of membrane materials in the capture of greenhouse gases such as carbon dioxide, the separation, purification and preparation of ultra-pure hydrogen, among which the supported metal palladium membrane is used in the capture of carbon dioxide and hydrogen separation. High membrane front pressure (46bar) and membrane thickness pressure (23bar) are required, and the hydrogen recovery rate obtained is between 50% and 60%. At the same time, there are very strict requirements for the mechanical strength of the membrane material[4]
[0004] In the present invention, aiming at the deficiencies in the traditional technology and the problem that the defects of single-layer palladium film are difficult to control, the concept of double-layer palladium composite film structure is proposed, and a double-layer palladium film is prepared by combining the advantages of electroplating and electroless plating. Composite membrane material

Method used

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  • Preparation method and application of palladium-ceramic-palladium bilayer composite membrane material
  • Preparation method and application of palladium-ceramic-palladium bilayer composite membrane material
  • Preparation method and application of palladium-ceramic-palladium bilayer composite membrane material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Single-layer palladium film with an outer layer of 4 μm

[0032] 1. Vector pretreatment

[0033] The porous ceramic carrier tube is 60 mm long and has an outer diameter of 14.05 mm. First in absolute ethanol (99.9%) NaCO 3 solution (NaCO 3 concentration of 0.10mol / L) for 15 minutes to remove impurities such as oil stains on the surface. Then immerse and wash in distilled water at 50°C for 30 minutes to remove residual alcohol solution. Finally, dry it in an oven at 150°C for later use, and the program is set as:

[0034]

[0035] Sensitize the oven-dried porous ceramic tube carrier, immerse in reducing agent (dimethylaminoborane), reduce for 5 minutes, rinse the carrier tube with distilled water, then immerse in 0.05mol / L palladium sulfate and 0.02mol / L of borax mixture to activate the palladium nucleus. The cycle was repeated 5 times until the color of the surface of the carrier film changed from white to black gray. So far, the palladium core is evenly cove...

Embodiment 2

[0047] 2μm inner layer and 2μm outer palladium film

[0048] 1. Vector pretreatment

[0049] The porous ceramic carrier tube is 60 mm long and has an outer diameter of 14.05 mm. First in absolute ethanol (99.9%) NaCO 3 solution (NaCO 3 concentration of 0.10mol / L) for 15 minutes to remove impurities such as oil stains on the surface. Then immerse and wash in distilled water at 50°C for 30 minutes to remove residual alcohol solution. Finally, dry it in an oven at 150°C for later use, and the program is set as:

[0050]

[0051] Sensitize the oven-dried porous ceramic tube carrier, immerse in reducing agent (dimethylaminoborane), reduce for 5 minutes, rinse the carrier tube with distilled water, then immerse in 0.05mol / L palladium sulfate and 0.02mol / L of borax mixture to activate the palladium nucleus. The cycle was repeated 5 times until the color of the surface of the carrier film changed from white to black gray. So far, the palladium core is evenly covered, and th...

Embodiment 3

[0071] Single-layer palladium film with an outer layer of 4 μm, performance test under simulated industrial conditions

[0072] 1. Vector pretreatment

[0073] Processing method is with embodiment 1.

[0074] 2. Electroless palladium plating film

[0075] Implementation method is the same as embodiment 1.

[0076] 3. Activation treatment and performance evaluation of palladium membrane

[0077] (1) Activation treatment

[0078] Concrete operation method, with embodiment 1.

[0079] (2) Performance test of membrane material

[0080] In a simulated industrial environment, with 450ml H 2 :400ml N 2Ratio, feed reaction gas, purge side with 400ml / min N 2 , the pressure on the reaction side was kept at 2MPa, the pressure on the permeate side was tested from 0.8MPa, and then the pressure on the permeate side was reduced to 0.6MPa, 0.4MPa, 0.2MPa and 0.1MPa, respectively, and the hydrogen permeation performance under these conditions was measured. For specific experimental res...

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Abstract

The invention relates to a preparation method of a palladium-ceramic-palladium bilayer composite membrane material and application of the palladium-ceramic-palladium bilayer composite membrane material in separating hydrogen and capturing carbon dioxide. Palladium membranes are plated on the surface layer and the inner layer of a porous ceramic carrier separately, on the one hand, it is ensured that the bilayer composite palladium membrane has high hydrogen permeability, on the other hand, the amount of nitrogen penetration caused by original defects is reduced greatly, and the permeation rateof H2 per unit area is increased, so that the selectivity of the composite membrane to H2 / N2 is improved greatly. In an actual production process in which industrial waste gas containing CO, CO2, CH4and H2S is generated, H2 is separated and purified on one side of the membrane, greenhouse gas of CH4, CO and CO2 is captured and concentrated on the other side of the membrane, and meanwhile the structure of the membrane is changed, so that the mass transfer process of hydrogen in the composite membrane is changed, and bulk-phase diffusion becomes the main step for speed control, and has no obvious change along with the reaction pressure difference and temperature between both sides of the membrane.

Description

technical field [0001] The present invention relates to the preparation method of palladium-ceramic-palladium double-layer composite membrane material and its application in the separation of hydrogen and carbon dioxide capture ( figure 2 ), construct a composite system of porous ceramic support framework and dense palladium membrane main body, and apply it to CH 4 and CO 2 capture of greenhouse gases, H 2 Separation or H 2 Purifying. Specifically, the Prime Minister used the method of electroless plating to plant nuclei on the carrier, and then formed an extremely thin conductive layer through the principle of self-catalysis; then used the method of electrochemical deposition to thicken the inner and outer palladium films. , so as to achieve the purpose of practical use. In the present invention, a palladium membrane-porous ceramic carrier-palladium membrane structure is subversively designed, compared to single-layer membrane materials ( figure 1 ), the double-layer c...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D69/12B01D67/00B01D53/22C01B3/50
CPCB01D53/228B01D67/0039B01D69/12B01D71/022B01D71/025B01D2257/504B01D2257/7025C01B3/505Y02C20/20Y02C20/40Y02P20/151Y02P30/00
Inventor 安德列斯·哥德巴赫赵辰阳徐恒泳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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