JP2011105566A - Mtw型ゼオライトの製造方法 - Google Patents
Mtw型ゼオライトの製造方法 Download PDFInfo
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000010457 zeolite Substances 0.000 title claims abstract description 86
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000013078 crystal Substances 0.000 claims abstract description 45
- 239000011541 reaction mixture Substances 0.000 claims abstract description 43
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 23
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 17
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 12
- 150000002894 organic compounds Chemical class 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 18
- 239000000047 product Substances 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 239000005416 organic matter Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 229910001413 alkali metal ion Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 5
- -1 methyltriethylammonium ion Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 229910001415 sodium ion Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910001388 sodium aluminate Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- VBQDSLGFSUGBBE-UHFFFAOYSA-N benzyl(triethyl)azanium Chemical compound CC[N+](CC)(CC)CC1=CC=CC=C1 VBQDSLGFSUGBBE-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- IPLONMMJNGTUAI-UHFFFAOYSA-M lithium;bromide;hydrate Chemical compound [Li+].O.[Br-] IPLONMMJNGTUAI-UHFFFAOYSA-M 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000011973 solid acid Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/42—Type ZSM-12
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7034—MTW-type, e.g. ZSM-12, NU-13, TPZ-12 or Theta-3
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Analytical Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
【解決手段】本発明のMTW型ゼオライトの製造方法は、特定のモル比で表される組成の反応混合物となるように、シリカ源、アルミナ源、アルカリ源、リチウム源、及び水を混合し、(2)SiO2/Al2O3比が10〜500である有機化合物を含まないMTW型ゼオライトを種結晶として用い、これを前記反応混合物中のシリカ成分に対して0.1〜20重量%の割合で該反応混合物に添加し、(3)前記種結晶が添加された前記反応混合物を100〜200℃で密閉加熱することを特徴とする。
【選択図】なし
Description
(1)以下に示すモル比で表される組成の反応混合物となるように、シリカ源、アルミナ源、アルカリ源、リチウム源、及び水を混合し、
SiO2/Al2O3=12〜200
Na2O/SiO2=0.1〜0.3
Li2O/(Na2O+Li2O)=0.05〜0.5
H2O/SiO2=10〜50
(2)SiO2/Al2O3比が10〜500である有機化合物を含まないMTW型ゼオライトを種結晶として用い、これを前記反応混合物中のシリカ成分に対して0.1〜20重量%の割合で該反応混合物に添加し、
(3)前記種結晶が添加された前記反応混合物を100〜200℃で密閉加熱することを特徴とするMTW型ゼオライトの製造方法を提供するものである。
・SiO2/Al2O3=12〜200
・Na2O/SiO2=0.1〜0.3
・Li2O/(Na2O+Li2O)=0.05〜0.5
・H2O/SiO2=10〜50
・SiO2/Al2O3=12〜150
・Na2O/SiO2=0.12〜0.25
・Li2O/(Na2O+Li2O)=0.1〜0.4
・H2O/SiO2=12〜30
組成分析装置:(株)バリアン製、ICP−AES LIBERTY SeriesII
テトラエチルアンモニウムヒドロキシドをSDAとして用い、水酸化アルミニウムをアルミナ源、臭化リチウムをリチウム源、微粉状シリカ(Cab−O−sil、M−5)をシリカ源とし、更に水を加えて、8TEA2O・3.5Li2O・Al2O3・40SiO2・640H2Oの組成の反応混合物を調製した。この反応混合物を密閉容器中に入れ、160℃で5日間加熱した。その生成物はMTW型ゼオライトであった。これを電気炉中で空気を流通しながら550℃で10時間焼成して、有機物を含まない種結晶1を合成した。焼成後のSiO2/Al2O3比は50.6であった。このMTW型ゼオライトのX線回折図を図1に示す。
テトラエチルアンモニウムヒドロキシドをSDAとして用い、アルミン酸ナトリウムをアルミナ源、微粉状シリカ(Cab−O−sil、M−5)をシリカ源とし、更に水を加えて、9.8TEA2O・0.79Na2O・Al2O3・80SiO2・1040H2Oの組成の反応混合物を調製した。この反応混合物を密閉容器中に入れ、160℃で8日間加熱した。その生成物はMTW型ゼオライトであった。これを電気炉中で空気を流通しながら550℃で10時間焼成して、有機物を含まない種結晶2を合成した。焼成後のSiO2/Al2O3比は101.2あった。このMTW型ゼオライトのX線回折図を図2に示す。
蒸留水5.8gに水酸化ナトリウム0.30gを溶かし、更に臭化リチウム一水和物0.31g、水酸化アルミニウム0.16g、種結晶1を0.12g、シリカ (Cab−O−Sil M5)1.20gの順に加え均一に攪拌して表1に記載した組成の反応混合物を調製した。この反応混合物を密閉容器中に入れ、140℃で7日間加熱した。生成物をろ過により分離し、水で洗浄した後60℃で乾燥した。この生成物は、図3に示すX線回折図から判るように、不純物を含まないMTW型ゼオライトであった。組成分析の結果は表1に示すとおりであった。
実施例1と同じ原料を用いて、表1に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。生成物は図4に示すX線回折図から判るように、不純物を含まないMTW型ゼオライトであった。生成物は表1に記載のとおりであった。
参考例2で合成したMTW型ゼオライト種結晶2を用いた以外は実施例1と同じ原料を用いて、表1に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。生成物は図5に示すX線回折図から判るように、不純物を含まないMTW型ゼオライトであった。生成物の組成は表1に記載のとおりであった。
種結晶1の添加量を1%とした以外は実施例1と同じ原料を用いて、表1に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。その結果、生成物及びその組成は表1に記載のとおりであった。
実施例1と原料を用いて、表1に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。その結果、生成物及びその組成は表1記載のとおりであった。
臭化リチウム一水和物を添加しないこと以外は実施例1で使用したものと同じ原料と種結晶1を用いて、表2に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。その結果、生成物は表2に記載のとおりであった。
実施例1で使用したものと同じ原料と種結晶1を用いて、表2に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。その結果、生成物は表2に記載のとおりであった。
種結晶を添加しないこと以外は実施例1で使用したものと同じ原料を用いて、表2に記載した組成の反応混合物を調製し、同表に記載の条件で加熱した。その結果、生成物は表2に記載のとおりであった。
Claims (2)
- (1)以下に示すモル比で表される組成の反応混合物となるように、シリカ源、アルミナ源、アルカリ源、リチウム源、及び水を混合し、
SiO2/Al2O3=12〜200
Na2O/SiO2=0.1〜0.3
Li2O/(Na2O+Li2O)=0.05〜0.5
H2O/SiO2=10〜50
(2)SiO2/Al2O3比が10〜500である有機化合物を含まないMTW型ゼオライトを種結晶として用い、これを前記反応混合物中のシリカ成分に対して0.1〜20重量%の割合で該反応混合物に添加し、
(3)前記種結晶が添加された前記反応混合物を100〜200℃で密閉加熱することを特徴とするMTW型ゼオライトの製造方法。 - 種結晶として、請求項1記載の製造方法で製造されたベータ型ゼオライトを用いることを特徴とする請求項1記載の製造方法。
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JP2009264550A JP5615530B2 (ja) | 2009-11-20 | 2009-11-20 | Mtw型ゼオライトの製造方法 |
DE112010004511.9T DE112010004511B4 (de) | 2009-11-20 | 2010-11-19 | Verfahren zum herstellen eines zeoliths vom mtw-typ |
KR1020127012719A KR101729356B1 (ko) | 2009-11-20 | 2010-11-19 | Mtw 형 제올라이트의 제조 방법 |
CN201080052299.5A CN102612492B (zh) | 2009-11-20 | 2010-11-19 | Mtw型沸石的制造方法 |
US13/509,677 US9333495B2 (en) | 2009-11-20 | 2010-11-19 | Method for producing MTW-type zeolite |
PCT/JP2010/070663 WO2011062256A1 (ja) | 2009-11-20 | 2010-11-19 | Mtw型ゼオライトの製造方法 |
US15/079,998 US9840423B2 (en) | 2009-11-20 | 2016-03-24 | Method for producing MTW-type zeolite |
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JP5351216B2 (ja) * | 2010-07-01 | 2013-11-27 | 日本化学工業株式会社 | ゼオライトの製造方法 |
US9802831B2 (en) * | 2014-07-23 | 2017-10-31 | Chevron U.S.A. Inc. | Synthesis of high silica zeolite via interzeolite transformation without OSDAs |
WO2018093510A1 (en) * | 2016-11-17 | 2018-05-24 | Chevron U.S.A. Inc. | Synthesis of mtw framework type zeolites via interzeolite transformation |
RU2719153C2 (ru) * | 2018-10-04 | 2020-04-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Способ получения цеолита структурой mtw |
Citations (4)
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JP5124659B2 (ja) * | 2011-01-27 | 2013-01-23 | 日本化学工業株式会社 | Mtw型ゼオライトの製造方法 |
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- 2010-11-19 WO PCT/JP2010/070663 patent/WO2011062256A1/ja active Application Filing
- 2010-11-19 CN CN201080052299.5A patent/CN102612492B/zh active Active
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JPS55116619A (en) * | 1979-01-15 | 1980-09-08 | Mobil Oil | Zeolite zsmml composition and method of producing same and method of contact inversion using same |
JPS57156322A (en) * | 1981-02-23 | 1982-09-27 | Ici Ltd | Synthetic zeolite and manufacture |
EP0162719A2 (en) * | 1984-05-24 | 1985-11-27 | The British Petroleum Company p.l.c. | Theta-3, a novel crystalline aluminosilicate and its preparation |
US5021141A (en) * | 1990-09-14 | 1991-06-04 | Mobil Oil Corp. | Synthesis of crystalline ZSM-12 type structure |
Also Published As
Publication number | Publication date |
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KR101729356B1 (ko) | 2017-04-21 |
DE112010004511T5 (de) | 2013-04-04 |
US20160200585A1 (en) | 2016-07-14 |
DE112010004511B4 (de) | 2023-05-04 |
US9840423B2 (en) | 2017-12-12 |
CN102612492B (zh) | 2014-10-08 |
US20130156689A1 (en) | 2013-06-20 |
CN102612492A (zh) | 2012-07-25 |
WO2011062256A1 (ja) | 2011-05-26 |
KR20120091222A (ko) | 2012-08-17 |
US9333495B2 (en) | 2016-05-10 |
JP5615530B2 (ja) | 2014-10-29 |
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