CN103638821B - Defect repairing method for palladium composite membrane - Google Patents
Defect repairing method for palladium composite membrane Download PDFInfo
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- CN103638821B CN103638821B CN201310721809.9A CN201310721809A CN103638821B CN 103638821 B CN103638821 B CN 103638821B CN 201310721809 A CN201310721809 A CN 201310721809A CN 103638821 B CN103638821 B CN 103638821B
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- palladium
- composite membrane
- film
- membrane
- based composite
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 60
- 239000012528 membrane Substances 0.000 title claims abstract description 42
- 230000007547 defect Effects 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 22
- 239000010703 silicon Substances 0.000 claims abstract description 22
- 230000001590 oxidative effect Effects 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 9
- 238000010926 purge Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 2
- 150000002835 noble gases Chemical class 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims 3
- 229910045601 alloy Inorganic materials 0.000 claims 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- 239000012159 carrier gas Substances 0.000 claims 2
- 239000000463 material Substances 0.000 claims 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 230000001413 cellular effect Effects 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 239000010949 copper Substances 0.000 claims 1
- 230000008021 deposition Effects 0.000 claims 1
- 239000011521 glass Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical group [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 230000008439 repair process Effects 0.000 abstract description 15
- 239000007787 solid Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 description 27
- 229910052739 hydrogen Inorganic materials 0.000 description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 13
- 150000002431 hydrogen Chemical class 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 230000004907 flux Effects 0.000 description 12
- 238000010574 gas phase reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 Hydrogen Chemical class 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The inventionRelates to a defect repair technology of a palladium composite membrane, which leads SiO to be reacted in a gas phase2The palladium membrane is deposited at the membrane defect position, so that the palladium membrane in the assembly can be directly repaired in situ without disassembling the assembly, and a repair scheme is provided for the defects generated in the use process of the membrane. The specific technical scheme of the invention is as follows: the membrane component is placed in a high-temperature furnace, a silicon source is introduced into the membrane side of the palladium composite membrane in the component, silicon source steam occupies the membrane defect, oxidizing gas is introduced into the substrate side of the palladium composite membrane in the component, the oxidizing gas is driven by the concentration difference to move to the defect and contacts with the silicon source steam, the oxidizing gas reacts quickly to generate solid particles, and the solid particles are deposited at the defect, so that the purpose of repairing is achieved. The invention solves the problem of repairing the defects generated in the using process of the membrane, can greatly prolong the service life of the membrane, and has wider practicability and convenient operation.
Description
Technical field
The present invention relates to a kind of palladium-based composite membrane defect mending method, the defect that more particularly, to film produces in use
Repair, realize directly carrying out in-situ repair to the palladium film in assembly, and assembly need not be dismantled.
Background technology
Palladium-based composite membrane combines the advantage of the unique hydrogen permeability energy of palladium film and the high penetration of porous carrier, Hydrogen Separation with pure
The application of change aspect is increasingly extensive.No matter in which aspect application, the hydrogen permeation selectivity of palladium film is all most important, in theory, intact
The hydrogen selectivity of sunken palladium film is infinity.Defective palladium film, either crackle, the big defect such as cut, or pin hole class
Little defect, all can significantly reduce the hydrogen selectivity of film, when the hydrogen selectivity of film do not reach require when, the life-span of film will terminate,
This becomes the key issue of impact palladio composite membrane application, and the service life extending film is necessary.And be your gold in view of palladium
Belong to, and the cost of matrix, if directly discard to cause huge economic loss, repair palladium film defect prolonging service lifetime of film meaning
Great.
Many factors may affect the consistency of film, such as matrix, the preparation method of film, thickness etc..Even completely fine and close
Palladium film be likely to that new defect occurs after hot operation.For reduce film defect, except take preferred substrate, optimize film preparation, increasing
Outside the methods such as blooming thickness, it is also directly a kind of effective ways to film defect mending.With regard to the repairing of palladium film defect, document existing
A little report, Li Anwu etc. [split scarce repairing in Li Anwu, Xiong Guoxing, r.hughes. dense palladium film, Chinese science, 1999,29
(2): 169-173] reverse osmosiss electroless plating method is proposed, what this seminar invented before this replaces reverse osmosis with dilute reducing agent hydrazine solution
The chemical plating repairing method of agent and pd (oh) thoroughly2Colloid pretreatment and chemical plating repairing method [Hu little Juan, Wei Juan, Huang Yan .pd (oh)2Glue
Body pretreatment and electroless plating method repair composite palladium film. Nanjing University of Technology's journal, 2011,33 (2): 43-48].Yuan Lixiang etc. adopts
With " from bottom to top " method repair palladium film [Yuan Lixiang, Xu Hengyong. " from bottom to top " method repair containing defect palladium film, membrane science and skill
Art .2009,29 (3): 48-51].Palladium film is repaired using said method, hydrogen selectivity is improved, but above-mentioned method for repairing and mending pin
To be the defect that film is formed in preparation process, and the defect that film is produced during life-time service, inapplicable.Because
Palladium film need to be sealed in membrane module realizes its application, and when adopting above method to repair, need to disassemble palladium film, unrealistic,
Complex operation is thereby increases and it is possible to cause extra defect due to artificial origin during operation, inapplicable.Exploitation film produces in use
Defect repairing technique, directly in-situ repair is carried out to the palladium film in assembly, significant.
Content of the invention
The purpose of the present invention: provide a kind of palladium-based composite membrane defect mending method, for palladium film defect, especially with process
The defect of middle generation, directly carries out in-situ repair to the palladium film being sealed in assembly, improves the hydrogen separation purity of film, and extending film makes
Use the life-span.For realizing preferable repair efficiency, the solid that reaction generates need to be made only to be deposited on scarce on the basis of not damaging palladium film
Fall into place, select to deposit sio in fault location2, it is because micropore sio2Generate beneficial to hydrogen separation.The resolving ideas of the present invention are:
Silicon source is passed through the film side of palladium-based composite membrane in assembly, silicon source steam occupies film fault location, subsequently oxidizing gas is passed through assembly
The matrix side of interior palladium-based composite membrane, the concentration official post oxic gas molecule of film both sides spreads to film fault location, connects with silicon source vapour molecule
Touch, react at once and generate solids particles precipitate in fault location, until defect mending finishes.Concrete technical scheme is as follows: will
Palladium membrane component is placed in the high temperature furnace of uniform temperature, and temperature control is in the suitable operating temperature range of palladium film (in hydrogeneous atmosphere
300-500℃；Without nitrogen atmosphere 25-500 DEG C).First silicon source is passed through the film side of palladium-based composite membrane in assembly, then by oxidizing gas
Lead to the matrix side of assembly inner membrance, gas flow is unsuitable excessive, in 10-30ml/min about, both sides all keep normal pressure, film both sides
Concentration official post two gas contact in fault location and react, when film is fine and close, reaction is automatically stopped.After reaction terminates, need
To carry out reduction treatment in hydrogen atmosphere.Silicon source is passed through mode two kinds, and one, silicon source is placed in bubbler, it is heated to one
Constant temperature degree (60-100 DEG C), logical noble gases enter the membrane module (pipe between bubbler and reative cell to carry silicon source steam
Road is heated to mutually synthermal in case steam condenses), two, it is injected directly in assembly with syringe such as syringe.Preferably the latter, reason
One, direct injection silicon source, the silicon source vapor concentration of film side is high, can reduce reaction temperature, control in palladium film suitable long-term work temperature
In the range of degree.Two, first injecting silicon source can preferably control reaction in film fault location, realize controlled gas phase reaction, reach height
Effect is repaired.Because first injection silicon source can make film defect can be washed in the silicon source steam of high concentration, so lead to oxidizing gas again
When, because concentration difference oxic gas spread to film fault location, contact with the silicon source vapour molecule of high concentration in film fault location and occur immediately
Reaction, gas phase reaction controls well and occurs in fault location.This method be suitable for palladium film repairing, operator do not need by palladium film from
Disassemble it is not necessary to find the position of palladium film defect in assembly, when the repair is completed, reaction can terminate automatically.
Beneficial effect:
The present invention deposits sio by controlled gas phase reaction in film fault location2Repair palladium film, it is directly right that its ingenious part is
In assembly, palladium film carries out in-situ repair, need not dismantle assembly, easy to operate, low cost.Respectively from the both sides of film lead to reaction raw materials,
This 3 points of concentration difference being preferentially passed through silicon source steam with film both sides makes reaction control well in film fault location, realizes efficient repairing
Mend.The sio of deposition2Not only the effect of filling up is played to film, micropore sio can also be utilized2Hydrogen separating property, be the hydrogen permeability of film
Can contribute.
Brief description
Fig. 1 schematic diagram repairing palladium-based composite membrane defect method disclosed by the invention.
After Fig. 2 adopts this patent methods described to repair palladium film, pd/al2o3The surface topography of composite membrane.
Specific embodiment
Embodiment 1
(1) pd/al in assembly will be sealed in2o3Composite membrane, first carries out flux and hydrogen permeation selectivity test, test result
For: when 350 DEG C, nitrogen flux is 0.086m3h-1m-2bar-1, hydrogen is 9.56m3h-1m-2bar-1, hydrogen nitrogen selectivity is about
111.
(2) assembly is placed in high temperature furnace, and nitrogen purging is warming up to 350 DEG C.
(3) teos is placed in bubbler, temperature control, at 60 DEG C, uses n2Purging, by needle valve and spinner flowmeter
Control purge rates are 20ml/min, are passed through film side, another reaction gas o2It is passed through matrix side, gas flow rate is 15ml/min.
(4) after reaction 6h, then flux and selectivity test are carried out, result is: when 350 DEG C, nitrogen flux is 0.012m3h- 1m-2bar-1, hydrogen is 7.98m3h-1m-2bar-1, hydrogen nitrogen selectivity is about 665, and selectivity improves.
Embodiment 2
(1) pd/al in assembly will be sealed in2o3Composite membrane, first carries out flux and hydrogen permeation selectivity test, test result
For: when 350 DEG C, nitrogen flux is 0.056m3h-1m-2bar-1, hydrogen is 10.23m3h-1m-2bar-1, hydrogen nitrogen selectivity is about
For 183.
(2) assembly is placed in high temperature furnace, and temperature control is at 330 DEG C.
(3) film side in assembly for the needle cylinder injection teos, another reaction gas o are used2It is passed through matrix side, gas flow rate is
15ml/min.
(4) after reaction 4h, then flux and selectivity test are carried out, result is: when 350 DEG C, nitrogen flux is 0.0096m3h-1m-2bar-1, hydrogen is 9.71m3h-1m-2bar-1, hydrogen nitrogen selectivity is about 1012, and selectivity improves nearly an order of magnitude.
Embodiment 3
(1) by the palladium/rustless steel composite membrane being sealed in assembly, flux and hydrogen permeation selectivity test, test knot are first carried out
Fruit is: when 350 DEG C, nitrogen flux is 0.097m3h-1m-2bar-1, hydrogen is 19.86m3h-1m-2bar-1, hydrogen nitrogen selectivity
It is about 204.
(2) assembly is placed in high temperature furnace, and temperature control is at 400 DEG C.
(3) teos is placed in bubbler, temperature control, at 80 DEG C, uses n2Purging, by needle valve and spinner flowmeter
Control purge rates are 20ml/min, are passed through film side, another reaction gas is passed through matrix side, and gas flow rate is 20ml/min.
(4) after reaction 6h, then flux and selectivity test are carried out, result is: when 350 DEG C, nitrogen flux is 0.016m3h- 1m-2bar-1, hydrogen is 16.25m3h-1m-2bar-1, hydrogen nitrogen selectivity is about 1015, and film selectivity improves.
Claims (7)
1. a kind of palladium-based composite membrane defect mending method, it is characterised in that being placed in palladium membrane component in high temperature furnace, silicon source steam is led to
Enter the film side of palladium-based composite membrane in assembly, silicon source steam occupies film fault location, then is passed through oxygen to the matrix side of palladium-based composite membrane in assembly
The property changed gas, oxidizing gas to fault location movement, and are contacted with the silicon source steam of fault location, quickly under the ordering about of concentration difference
Reaction generates sio2It is deposited on fault location, reaches the purpose of repairing, realize the defect direct in-situ of palladium film in assembly is repaired.
2. palladium-based composite membrane defect mending method according to claim 1 is it is characterised in that silicon source steam is to meet gas phase
The siliceous thing of deposition, described siliceous thing is teos or sih4.
3. palladium-based composite membrane defect mending method according to claim 1 is it is characterised in that silicon source steam is passed through the side of assembly
Formula has carrier gas purge or direct injection.
4. palladium-based composite membrane defect mending method according to claim 3 is it is characterised in that carrier gas is noble gases n2, ar or
he.
5. palladium-based composite membrane defect mending method according to claim 1 is it is characterised in that oxidizing gas are o2, h2O or
o3.
6. palladium-based composite membrane defect mending method according to claim 1 it is characterised in that reaction temperature be 300-500 DEG C,
Response time is 2-10h.
7. palladium-based composite membrane defect mending method according to claim 1 is it is characterised in that the film material of palladium-based composite membrane is
Simple metal palladium or palldium alloy, described palldium alloy is palladium-silver, the alloy composite film of porpezite, palladium copper or palladium nickel；The matrix of palladium-based composite membrane
Material is porous ceramicss, cellular glass or porous stainless steel.
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| CN201310721809.9A CN103638821B (en) | 2013-12-23 | 2013-12-23 | Defect repairing method for palladium composite membrane |
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| CN201310721809.9A CN103638821B (en) | 2013-12-23 | 2013-12-23 | Defect repairing method for palladium composite membrane |
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| CN103638821B true CN103638821B (en) | 2017-01-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017180141A1 (en) * | 2016-04-14 | 2017-10-19 | Lockheed Martin Corporation | Selective interfacial mitigation of graphene defects |
| CN109722632A (en) * | 2017-10-31 | 2019-05-07 | 陕西南水汽车配件制造有限公司 | A kind of aluminum alloy control arm forging coarse grains on surface ring control method |
| KR102015002B1 (en) * | 2017-12-26 | 2019-08-27 | 예일 유니버시티 | Method for restoration of compromised water treatment membrane using surface functionalized silica microparticles |
| CN112546870B (en) * | 2020-11-25 | 2022-09-20 | 南京工业大学 | In-situ repair technology |
Citations (3)
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| US5672388A (en) * | 1994-07-08 | 1997-09-30 | Exxon Research & Engineering Company | Membrane reparation and poer size reduction using interfacial ozone assisted chemical vapor deposition |
| CN101560654A (en) * | 2008-04-18 | 2009-10-21 | 中国科学院大连化学物理研究所 | Method for repairing defects of palladium and palladium alloy composite membranes |
| CN102491271A (en) * | 2011-12-09 | 2012-06-13 | 丹阳奥恩能源科技发展有限公司 | Method for repairing defects of palladium membrane component |
-
2013
- 2013-12-23 CN CN201310721809.9A patent/CN103638821B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5672388A (en) * | 1994-07-08 | 1997-09-30 | Exxon Research & Engineering Company | Membrane reparation and poer size reduction using interfacial ozone assisted chemical vapor deposition |
| CN101560654A (en) * | 2008-04-18 | 2009-10-21 | 中国科学院大连化学物理研究所 | Method for repairing defects of palladium and palladium alloy composite membranes |
| CN102491271A (en) * | 2011-12-09 | 2012-06-13 | 丹阳奥恩能源科技发展有限公司 | Method for repairing defects of palladium membrane component |
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