KR970000315A - 수소분리용 무기재료막의 제조방법 - Google Patents
수소분리용 무기재료막의 제조방법 Download PDFInfo
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- KR970000315A KR970000315A KR1019950017060A KR19950017060A KR970000315A KR 970000315 A KR970000315 A KR 970000315A KR 1019950017060 A KR1019950017060 A KR 1019950017060A KR 19950017060 A KR19950017060 A KR 19950017060A KR 970000315 A KR970000315 A KR 970000315A
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- South Korea
- Prior art keywords
- alumina support
- palladium
- support
- alumina
- membrane
- Prior art date
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- 239000001257 hydrogen Substances 0.000 title claims abstract 9
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract 9
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title claims abstract 9
- 229910010272 inorganic material Inorganic materials 0.000 title claims abstract 9
- 239000011147 inorganic material Substances 0.000 title claims abstract 9
- 238000000926 separation method Methods 0.000 title claims abstract 9
- 238000004519 manufacturing process Methods 0.000 title claims abstract 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract 26
- 239000012528 membrane Substances 0.000 claims abstract 16
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract 14
- 239000012696 Pd precursors Substances 0.000 claims abstract 10
- 238000000034 method Methods 0.000 claims abstract 10
- 229910052763 palladium Inorganic materials 0.000 claims abstract 7
- 239000011148 porous material Substances 0.000 claims abstract 7
- 238000000151 deposition Methods 0.000 claims abstract 5
- 238000010438 heat treatment Methods 0.000 claims abstract 4
- 239000000203 mixture Substances 0.000 claims abstract 4
- 238000003980 solgel method Methods 0.000 claims abstract 3
- 239000011248 coating agent Substances 0.000 claims abstract 2
- 238000000576 coating method Methods 0.000 claims abstract 2
- 238000001764 infiltration Methods 0.000 claims abstract 2
- 230000008595 infiltration Effects 0.000 claims abstract 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- 230000008021 deposition Effects 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 2
- 230000035515 penetration Effects 0.000 claims 2
- BHZSLLSDZFAPFH-UHFFFAOYSA-L palladium(2+);difluoride Chemical compound F[Pd]F BHZSLLSDZFAPFH-UHFFFAOYSA-L 0.000 claims 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims 1
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0072—Inorganic membrane manufacture by deposition from the gaseous phase, e.g. sputtering, CVD, PVD
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0048—Inorganic membrane manufacture by sol-gel transition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0069—Inorganic membrane manufacture by deposition from the liquid phase, e.g. electrochemical deposition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/04—Tubular membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/106—Membranes in the pores of a support, e.g. polymerized in the pores or voids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/108—Inorganic support material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1213—Laminated layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
- B01D71/0223—Group 8, 9 or 10 metals
- B01D71/02231—Palladium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
- C01B3/503—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion characterised by the membrane
- C01B3/505—Membranes containing palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/16—Hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/108—Hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
- B01D2323/081—Heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/42—Details of membrane preparation apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
- B01D2325/022—Asymmetric membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/10—Catalysts being present on the surface of the membrane or in the pores
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0405—Purification by membrane separation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S55/00—Gas separation
- Y10S55/05—Methods of making filter
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dispersion Chemistry (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Hydrogen, Water And Hydrids (AREA)
Abstract
본 발명은 수소분리용 무기재료막의 제조방법에 관한 것이다. 좀더 구체적으로, 본 발명은 졸겔법을 사용하여 알루미나 지지체의 중간층에 알루미나 지지막을 코팅하고 알루미나 지지막을 기공에 팔라듐을 침투증착시켜 높은 투과도와 우수한 수소 분리선택도를 지닌 수소분리용 무기재료막을 제조하는 방법에 관한 것이다. 본 발명의 무기재료막은 졸겔법을 사용하여 알루미나 졸에 팔라듐 전구체를 균일하게 분산시키고 내부를 진공상태로 유지한 알루미나 지지체에 침적코팅시켜 지지체의 중간층에 알루미나 지지막층을 형성하는 공정; 전기한 공정에서 수득한 알루미나 지지막을 팔라듐 전구체의 침투혼합액에 담가 지지체의 내부를 진공으로 유지하고 알루미나 지지막층의 기공에 팔라듐 전구체를 침투시켜 2 내지 4시간 동안 건조시키고 170내지 190℃까지 승온시켜 지지막층의 기공표면에 팔라듐을 증착시키는 공정; 및 전기 공정에서 수득한 지지막층의 기표면에 팔라듐이 증착된 알루미나 지지체의 내부를 진공으로 유지하면서 290 내지 310℃에서 열처리하는 공정을 포함한다.
Description
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
Claims (8)
- (i) 졸겔법을 사용하여 알루미나 졸에 팔라듐 전구체를 균일하게 분산시키고 내부를 진공상태로 유지한 알루미나 지지체에 침적코팅시켜 지지체의 중간층에 알루미나 지지막층을 형성하는 공정; (ⅱ) 전기한 공정에서 수득한 알루미나 지지막을 팔라듐 전구체의 침투혼합액에 담가 지지체의 내부를 진공으로 유지하고 알루미나 지지막층의 기공에 팔라듐 전구체를 침투시켜 2 내지 4시간 동안 건조시키고 170내지 190℃까지 승온시켜 지지막층의 기공표면에 팔라듐을 증착시키는 공정; 및 (ⅲ) 전기 공정에서 수득한 지지막층의 기공표면에 팔라듐이 증착된 알루미나 지지체의 내부를 진공으로 유지하면서 290 내지 310℃에서 열처리하는 공정을 포함하는 수소분리용 무기재료막의 제조방법.
- 제1항에 있어서, 알루미나 지지체로는 비대칭성 관형 알루미나 지지체를 사용하는 것을 특징으로 하는 수소분리용 무기재료막의 제조방법.
- 제1항에 있어, 알루미나 지지막층을 형성시 팔라듐 전구체로는 팔라듐 틀로라이드를 사용하는 것을 특징으로 하는 수소분리용 무기재료막의 제조방법.
- 제1항에 있어, 알루미나 졸과 팔라듐 전구체는 소니케이션에 의해 분산시키는 것을 특징으로 하는 수소분리용 무기재료막의 제조방법.
- 제1항에 있어, 팔라듐 전구체의 침투혼합액으로는 팔라듐 아세테이트를 아세톤 및 염산에 용해시킨 혼합액을 사용하는 것을 특징으로 하는 수소분리용 무기재료막의 제조방법.
- 제1항에 있어, 알루미나 지지막층의 기공에 팔라듐 전구체를 침투시켜 승온시 지지체의 외부에서 내부로 질소를 흘려주면서 승온시키는 것을 특징으로 하는 수소분리용 무기재료막의 제조방법.
- 제1항에 있어서, 팔라듐 침투증착 및 열처리는 알루미나 지지체(1)의 지지막 내부에 팔라듐을 침투증착시키기 위한 반응기(2); 알루미나 지지체(1)를 가열시키기 위한 전기로(3); 알루미나 지지체(1)의 내부로 공급되는 질소의 유량을 조절하기 위한 부피유량계(4); 및 알루미나 지지체(1)의 내부를 진공으로 유지시키기 위한 진공펌프(5)를 포함하는 침투증착장치를 사용하여 이루어지는 것을 특징으로 하는 수소분리용 무기재료막의 제조방법.
- 제1항의 제조방법에 의해 제조된, 알루미나 지지막층이 알루미나 지지체의 중간층에 형성된 구조를 지닌 수소분리용 무기재료막.※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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KR1019950017060A KR0158431B1 (ko) | 1995-06-23 | 1995-06-23 | 수소분리용 무기재료막의 제조방법 |
US08/669,005 US5782959A (en) | 1995-06-23 | 1996-06-21 | Process for preparing a composite inorganic membrane for hydrogen separation |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1019950017060A KR0158431B1 (ko) | 1995-06-23 | 1995-06-23 | 수소분리용 무기재료막의 제조방법 |
Publications (2)
Publication Number | Publication Date |
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KR970000315A true KR970000315A (ko) | 1997-01-21 |
KR0158431B1 KR0158431B1 (ko) | 1998-11-16 |
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KR1019950017060A KR0158431B1 (ko) | 1995-06-23 | 1995-06-23 | 수소분리용 무기재료막의 제조방법 |
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US (1) | US5782959A (ko) |
KR (1) | KR0158431B1 (ko) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100358078B1 (ko) * | 1999-08-23 | 2002-10-25 | 한국화학연구원 | 실리카층으로 안정화시킨 팔라듐 무기복합막 및 이의 제조방법 |
KR100595529B1 (ko) * | 2005-09-01 | 2006-07-03 | 한국화학연구원 | 용존산소 제거용 촉매 첨착형 다공성 고분자막 및 이의제조 방법 |
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US6354444B1 (en) * | 1997-07-01 | 2002-03-12 | Zenon Environmental Inc. | Hollow fiber membrane and braided tubular support therefor |
US5958098A (en) * | 1997-10-07 | 1999-09-28 | Westinghouse Savannah River Company | Method and composition in which metal hydride particles are embedded in a silica network |
JP2981884B1 (ja) * | 1998-06-29 | 1999-11-22 | 工業技術院長 | ゼオライト膜の製造方法 |
US6180559B1 (en) * | 1999-03-02 | 2001-01-30 | Eastman Chemical Company | Supported catalysts and catalyst support materials and process for the manufacture of 1,2-epoxybutane |
US6214090B1 (en) * | 1999-06-18 | 2001-04-10 | The Regents Of The University Of California | Thermally tolerant multilayer metal membrane |
JP3894529B2 (ja) * | 1999-06-28 | 2007-03-22 | ニチアス株式会社 | 除湿剤、除湿素子及びその製造方法 |
CZ20021630A3 (cs) * | 1999-11-17 | 2002-10-16 | Celanese International Corporation | Způsob výroby katalyzátoru |
JP2002033113A (ja) * | 1999-11-18 | 2002-01-31 | Toyota Motor Corp | 燃料電池用燃料ガス生成装置および水素分離用複合材 |
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KR100358078B1 (ko) * | 1999-08-23 | 2002-10-25 | 한국화학연구원 | 실리카층으로 안정화시킨 팔라듐 무기복합막 및 이의 제조방법 |
KR100595529B1 (ko) * | 2005-09-01 | 2006-07-03 | 한국화학연구원 | 용존산소 제거용 촉매 첨착형 다공성 고분자막 및 이의제조 방법 |
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US5782959A (en) | 1998-07-21 |
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