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Defect mending method of palladium composite membrane

A defect repairing and composite membrane technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve problems such as unrealistic, inapplicable, cumbersome operation, etc., and achieve the effect of convenient operation and low cost

Active Publication Date: 2014-03-19
RISON HI TECH MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the palladium membrane needs to be sealed in the membrane module to realize its application, the palladium membrane needs to be disassembled when the above method is used for repair, which is unrealistic and cumbersome to operate, and may cause additional defects due to human factors during operation, so it is not applicable

Method used

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  • Defect mending method of palladium composite membrane
  • Defect mending method of palladium composite membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] (1) Pd / Al sealed in the component 2 o 3 For the composite membrane, the flux and hydrogen permeation selectivity tests were carried out first. The test results are: at 350°C, the nitrogen flux is 0.086m 3 h -1 m -2 bar -1 , the hydrogen flux is 9.56m 3 h -1 m -2 bar -1 , the hydrogen-nitrogen selectivity is about 111.

[0011] (2) The component is placed in a high-temperature furnace, and the temperature is raised to 350°C by nitrogen purge.

[0012] (3) Put TEOS in a bubbler with the temperature controlled at 60°C and use N 2 Purge, control the purge rate to 20ml / min through the needle valve and rotameter, pass into the membrane side, another reaction gas O 2 Pass into the substrate side, the gas flow rate is 15ml / min.

[0013] (4) After reacting for 6 hours, the flux and selectivity test was carried out again. The result was: at 350°C, the nitrogen flux was 0.012m 3 h -1 m -2 bar -1 , the hydrogen flux is 7.98m 3 h -1 m -2 bar -1 , The hydrogen-nitr...

Embodiment 2

[0015] (1) Pd / Al sealed in the component 2 o 3 For the composite membrane, the flux and hydrogen permeation selectivity tests are carried out first. The test results are: at 350°C, the nitrogen flux is 0.056m 3 h -1 m -2 bar -1 , the hydrogen flux is 10.23m 3 h -1 m -2 bar -1 , the hydrogen-nitrogen selectivity is about 183.

[0016] (2) The assembly is placed in a high-temperature furnace, and the temperature is controlled at 330°C.

[0017] (3) Inject TEOS on the membrane side of the module with a syringe, and another reaction gas O 2 Pass into the substrate side, the gas flow rate is 15ml / min.

[0018] (4) After reacting for 4 hours, the flux and selectivity test was carried out. The result was: at 350°C, the nitrogen flux was 0.0096m 3 h -1 m -2 bar -1 , the hydrogen flux is 9.71m 3 h -1 m -2 bar -1 , the hydrogen-nitrogen selectivity is about 1012, and the selectivity is increased by nearly an order of magnitude.

Embodiment 3

[0020] (1) The palladium / stainless steel composite membrane sealed in the module is first tested for flux and hydrogen permeability selectivity. The test results are: at 350°C, the nitrogen flux is 0.097m 3 h -1 m -2 bar -1 , the hydrogen flux is 19.86m 3 h -1 m -2 bar -1 , the hydrogen-nitrogen selectivity is about 204.

[0021] (2) The components are placed in a high-temperature furnace, and the temperature is controlled at 400°C.

[0022] (3) Put TEOS in a bubbler with the temperature controlled at 80°C and use N 2 For purge, the purge rate is controlled at 20ml / min through the needle valve and rotameter, and it is passed into the membrane side, and another reaction gas is passed into the substrate side, and the gas flow rate is 20ml / min.

[0023] (4) After reacting for 6 hours, the flux and selectivity test was carried out again. The result was: at 350°C, the nitrogen flux was 0.016m 3 h -1 m -2 bar -1 , the hydrogen flux is 16.25m 3 h -1 m -2 bar -1 , the ...

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Abstract

The invention relates to a defect mending method of a palladium composite membrane. According to the defect mending method, SiO2 is deposited at the defect part of the membrane by gas-phase reaction, so that in-situ mending is directly carried out on the palladium membrane in a component without need of disassembling the component, and a mending scheme is provided for the defects generated in the use process of the membrane. According to the specific technical scheme, the defect mending method comprises the steps that the membrane component is arranged in a high-temperature furnace, a silicon source is introduced into the membrane side of the palladium composite membrane in the component, steam of the silicon source occupies the defect position of the membrane, and then oxidative gas is introduced into the base side of the palladium composite membrane in the component, moves to the defect part under the driving of concentration difference, is in contact with the steam of the silicon source and reacts quickly to produce solid particles which are deposited at the defect part, so that the mending purpose is achieved. The defect mending method has the advantages that the defects generated in the use process of the membrane can be mended, the service life of the membrane can be greatly prolonged, the practicability is wide and the operation is convenient.

Description

technical field [0001] The invention relates to a method for repairing defects of a palladium composite membrane, in particular to repairing defects generated during use of the membrane, which realizes direct in-situ repair of the palladium membrane in the module without disassembling the module. Background technique [0002] Palladium composite membranes combine the unique hydrogen permeability of palladium membranes with the advantages of high permeability of porous carriers, and are increasingly used in hydrogen separation and purification. Regardless of the application, the hydrogen permeation selectivity of the palladium membrane is very important. Theoretically, the hydrogen selectivity of the defect-free palladium membrane is infinite. Defective palladium membranes, whether they are large defects such as cracks or scratches, or small defects such as pinholes, will significantly reduce the hydrogen selectivity of the membrane. When the hydrogen selectivity of the membr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D65/10C01B3/56
Inventor 黄彦黎月华胡小娟俞健魏磊魏浩
Owner RISON HI TECH MATERIALS CO LTD
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