JP6168775B2 - 水素ガスの製造方法 - Google Patents
水素ガスの製造方法 Download PDFInfo
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- JP6168775B2 JP6168775B2 JP2012555801A JP2012555801A JP6168775B2 JP 6168775 B2 JP6168775 B2 JP 6168775B2 JP 2012555801 A JP2012555801 A JP 2012555801A JP 2012555801 A JP2012555801 A JP 2012555801A JP 6168775 B2 JP6168775 B2 JP 6168775B2
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- oxygen
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- methanol
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims description 71
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 153
- 239000007789 gas Substances 0.000 claims description 99
- 239000003054 catalyst Substances 0.000 claims description 88
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 63
- 239000001301 oxygen Substances 0.000 claims description 63
- 229910052760 oxygen Inorganic materials 0.000 claims description 63
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 46
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 44
- 239000005751 Copper oxide Substances 0.000 claims description 35
- 229910000431 copper oxide Inorganic materials 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 18
- 239000012495 reaction gas Substances 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 description 23
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 13
- 229910001882 dioxygen Inorganic materials 0.000 description 13
- 230000000694 effects Effects 0.000 description 13
- 230000007423 decrease Effects 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000008929 regeneration Effects 0.000 description 6
- 238000011069 regeneration method Methods 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 239000000567 combustion gas Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- 238000013022 venting Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000629 steam reforming Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- -1 and the like Chemical compound 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
- C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
-
- 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
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/323—Catalytic reaction of gaseous or liquid organic compounds other than hydrocarbons with gasifying agents
- C01B3/326—Catalytic reaction of gaseous or liquid organic compounds other than hydrocarbons with gasifying agents characterised by the catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/94—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the iron group metals or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- 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
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
- C01B2203/0244—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being an autothermal reforming step, e.g. secondary reforming processes
-
- 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
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1076—Copper or zinc-based catalysts
-
- 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
- C01B2203/12—Feeding the process for making hydrogen or synthesis gas
- C01B2203/1205—Composition of the feed
- C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
- C01B2203/1217—Alcohols
- C01B2203/1223—Methanol
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Hydrogen, Water And Hydrids (AREA)
Description
CH3OH + 0.5O2 → CO2 + 2H2 (1)
で表されるように、メタノールが酸化し、水素ガスと二酸化炭素ガスが生成する。このメタノールの酸化反応は、発熱反応であるため、系内の温度が上昇する。
CH3OH → CO + 2H2 (2)
で表されるように、一酸化炭素ガスと水素ガスに分解したり、式(3):
CH3OH + H2O → CO2 + 3H2 (3)
で表されるように、二酸化炭素ガスと水素ガスに分解したりする。これらの分解反応は、いずれも吸熱反応であることから、前記酸化反応で発生した熱の一部が打ち消される。その結果、系内の温度は、前記酸化反応のみが起こる場合の温度と対比して、幾分かは低い温度となる。また、これらの反応以外にも、式(4):
CO + H2O → CO2 + H2 (4)
で表されるシフト反応が起こると考えられている。
〔酸素ガス停止時間の比率〕
=〔(酸素ガスの供給を停止する時間)÷(1周期に要する時間)〕×100 (I)
で表される酸素ガス停止時間の比率は、酸化銅/酸化アルミニウム触媒の触媒活性を充分に回復させるとともに水素ガスを効率よく製造する観点から、30%以下であることが好ましい。例えば、前記1周期に要する時間を10秒間としたとき、酸素含有ガスを供給する時間が7秒間以上であり、酸素含有ガスの供給を停止する時間が3秒間以下であることが好ましい。
長さ20cm、内径2.3cmの反応器内に、酸化銅/酸化アルミニウム触媒[アルドリッチ社製、酸化銅(CuO)と酸化アルミニウム(Al2O3)との質量比〔酸化銅(CuO)/酸化アルミニウム(Al2O3)〕:12/88]を充填した後、水素ガスを含む窒素ガスを約10時間反応器内に導入することにより、酸化銅/酸化アルミニウム触媒を賦活させた。
実施例1において、空気を標準状態で2.2L/分の流量で10分間通気した後、当該空気の通気を60秒間停止する操作を1周期として周期的に繰り返したこと以外は、実施例1と同様の操作を行なった。そのとき、式(I)で表される酸素ガス停止時間の比率は、約9%であった。
その結果を表2に示す。
実施例1において、空気を標準状態で2.0L/分の一定流量で供給したこと以外は、実施例1と同様にして反応を行なった。その結果を表3に示す。
Claims (4)
- 酸素含有ガスを供給しながら触媒の存在下でメタノールと水を接触させることによって反応ガスを製造し、当該反応ガスから水素ガスを分離することによって水素ガスを製造する方法であって、前記触媒として酸化銅/酸化アルミニウム触媒を用い、前記酸化銅/酸化アルミニウム触媒をあらかじめ還元させた後に使用してメタノールの酸化反応と、当該酸化反応と並行してメタノールの分解反応とを少なくとも行ない、当該酸化反応及び分解反応に際し、酸素含有ガスの供給を一時的に停止するものであり、前記メタノールの酸化反応が式(1):
CH 3 OH + 0.5O 2 → CO 2 + 2H 2 (1)
で表わされるメタノールの酸化反応であり、前記メタノールの分解反応が式(2)および(3):
CH 3 OH → CO + 2H 2 (2)
CH 3 OH + H 2 O → CO 2 + 3H 2 (3)
で表わされるメタノールの分解反応であることを特徴とする水素ガスの製造方法。 - 酸素含有ガスの供給の開始から当該酸素含有ガスの供給の停止に至るまでの時間を10秒〜10分間に制御する請求項1に記載の水素ガスの製造方法。
- 酸素含有ガスの供給を停止させる時間が3〜60秒間である請求項1または2に記載の水素ガスの製造方法。
- 酸素含有ガスの供給を開始する時点から、当該酸素含有ガスの供給を停止させた後、次の酸素含有ガスの供給を開始するまでの1周期に要する時間に対する酸素含有ガスの供給を停止させる時間の比率が30%以下である請求項1〜3のいずれかに記載の水素ガスの製造方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011017867 | 2011-01-31 | ||
JP2011017867 | 2011-01-31 | ||
PCT/JP2012/051351 WO2012105355A1 (ja) | 2011-01-31 | 2012-01-23 | 水素ガスの製造方法 |
Related Child Applications (1)
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JP2016169920A Division JP2016196410A (ja) | 2011-01-31 | 2016-08-31 | 水素ガスの製造方法 |
Publications (2)
Publication Number | Publication Date |
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JPWO2012105355A1 JPWO2012105355A1 (ja) | 2014-07-03 |
JP6168775B2 true JP6168775B2 (ja) | 2017-07-26 |
Family
ID=46602574
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JP2012555801A Active JP6168775B2 (ja) | 2011-01-31 | 2012-01-23 | 水素ガスの製造方法 |
JP2016169920A Withdrawn JP2016196410A (ja) | 2011-01-31 | 2016-08-31 | 水素ガスの製造方法 |
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JP2016169920A Withdrawn JP2016196410A (ja) | 2011-01-31 | 2016-08-31 | 水素ガスの製造方法 |
Country Status (4)
Country | Link |
---|---|
JP (2) | JP6168775B2 (ja) |
KR (1) | KR101869580B1 (ja) |
TW (1) | TWI511920B (ja) |
WO (1) | WO2012105355A1 (ja) |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6236001A (ja) * | 1985-08-07 | 1987-02-17 | Mitsubishi Heavy Ind Ltd | メタノ−ル改質法 |
JPH04200640A (ja) * | 1990-05-25 | 1992-07-21 | Agency Of Ind Science & Technol | メタノール改質用触媒の再生法 |
JP2001226103A (ja) * | 2000-02-18 | 2001-08-21 | Nissan Motor Co Ltd | 燃料改質装置 |
ES2234618T3 (es) * | 2000-06-22 | 2005-07-01 | Consejo Superior De Investigaciones Cientificas | Procedimiento para la obtencion de hidrogeno por oxidacion parcial de metanol. |
JP4774197B2 (ja) * | 2003-05-20 | 2011-09-14 | 出光興産株式会社 | 酸素含有炭化水素の改質触媒、それを用いた水素又は合成ガスの製造方法及び燃料電池システム |
TW200836836A (en) * | 2007-03-12 | 2008-09-16 | Univ Nat Central | Hydrogen production via partial oxidation of methanol over Au/Al2O3-CuO catalysts |
CN101965311B (zh) * | 2008-02-25 | 2013-06-12 | 住友精化株式会社 | 氢的制造方法和装置 |
-
2012
- 2012-01-23 KR KR1020137022961A patent/KR101869580B1/ko active IP Right Grant
- 2012-01-23 WO PCT/JP2012/051351 patent/WO2012105355A1/ja active Application Filing
- 2012-01-23 JP JP2012555801A patent/JP6168775B2/ja active Active
- 2012-01-31 TW TW101103090A patent/TWI511920B/zh active
-
2016
- 2016-08-31 JP JP2016169920A patent/JP2016196410A/ja not_active Withdrawn
Also Published As
Publication number | Publication date |
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TW201245037A (en) | 2012-11-16 |
TWI511920B (zh) | 2015-12-11 |
KR20140023895A (ko) | 2014-02-27 |
KR101869580B1 (ko) | 2018-06-20 |
WO2012105355A1 (ja) | 2012-08-09 |
JPWO2012105355A1 (ja) | 2014-07-03 |
JP2016196410A (ja) | 2016-11-24 |
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