JP2010517902A - パラタングステン酸アンモニウム水和物を製造する方法及びパラタングステン酸アンモニウム十水和物 - Google Patents
パラタングステン酸アンモニウム水和物を製造する方法及びパラタングステン酸アンモニウム十水和物 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 52
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 title claims abstract description 14
- -1 ammonium paratungstate decahydrate Chemical class 0.000 title claims description 14
- 239000012074 organic phase Substances 0.000 claims abstract description 64
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000605 extraction Methods 0.000 claims abstract description 31
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 44
- 239000012071 phase Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 20
- 229910021529 ammonia Inorganic materials 0.000 claims description 19
- 239000008346 aqueous phase Substances 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 229910052721 tungsten Inorganic materials 0.000 claims description 14
- 239000010937 tungsten Substances 0.000 claims description 14
- 238000005191 phase separation Methods 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000012452 mother liquor Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- 230000001747 exhibiting effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 239000000047 product Substances 0.000 description 37
- 238000002425 crystallisation Methods 0.000 description 13
- 230000008025 crystallization Effects 0.000 description 13
- 239000012535 impurity Substances 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 10
- 150000004691 decahydrates Chemical class 0.000 description 7
- 239000007858 starting material Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 230000029087 digestion Effects 0.000 description 5
- 238000000622 liquid--liquid extraction Methods 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 5
- 238000000638 solvent extraction Methods 0.000 description 5
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- PLLBRTOLHQQAQQ-UHFFFAOYSA-N 8-methylnonan-1-ol Chemical compound CC(C)CCCCCCCO PLLBRTOLHQQAQQ-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 150000004685 tetrahydrates Chemical class 0.000 description 3
- YOFPVMWVLDSWKR-UHFFFAOYSA-N 11-methyl-n-(11-methyldodecyl)dodecan-1-amine Chemical compound CC(C)CCCCCCCCCCNCCCCCCCCCCC(C)C YOFPVMWVLDSWKR-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 244000045947 parasite Species 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
W−濃縮物は苛性ソーダで消化し、かつ生じた溶液を、Mg、Al塩及び硫化水素ナトリウムの添加により、不純物、たとえばP、As、Si、V及びMoについて予備精製した。なおも含まれるアニオン及びカチオン不純物のさらなる精製工程として、有機相(7〜10%のジイソトリデシルアミン、10%のイソデカノール、残りソルベントナフサ)の使用下で、液−液抽出をおこなった。タングステンが装入されたOPは、NH3−溶液を用いて再抽出した。これに関して使用された装置は、図3に表す。
Claims (13)
- ミキサーセトラー装置中で、直接、タングステン装入有機相をアンモニア含有水性溶液で再抽出することによりパラタングステン酸アンモニウム水和物を連続的に製造する方法において、該再抽出を、NH3:W−モル比 0.83〜1.30及びタングステン装入有機相とアンモニア含有水性溶液との供給体積比 5〜25で実施することを特徴とする、ミキサーセトラー装置中で、直接タングステン装入有機相をアンモニア含有水性溶液で再抽出することによりパラタングステン酸アンモニウム水和物を連続的に製造する方法。
- 再抽出を、NH3:W−モル比 0.85〜0.95及びタングステン装入有機相とアンモニア含有水性溶液との供給体積比 10〜15で実施する、請求項1に記載の方法。
- ミキサー中での再抽出を、パラタングステン酸アンモニウム水和物の固体濃度が、ミキサー中のアンモニア含有水性相に対して100〜1200g/l、好ましくは500〜800g/lに設定されるように実施する、請求項1に記載の方法。
- ミキサー中での攪拌速度を、ミキサー中で有機相とアンモニア含有水性相との不均一な分散が達成されるように調整する、請求項1から3までのいずれか1項に記載の方法。
- タングステン装入有機相及びアンモニア含有水性溶液をミキサーの下半分に、好ましくは攪拌領域に計量供給し、かつ、生じた3相混合物をミキサーの上部領域、好ましくは自由な溢流により及び下部領域、好ましくは攪拌領域から組み合わせて取り出すことで、ミキサー中でのタングステン装入有機相とアンモニア含有水性溶液との定常状態の比を1:5から1:70の間に調整する、請求項1から4までのいずれか1項に記載の方法。
- 攪拌装置を備えた沈降タンク中で、攪拌下で相混合物を分離し、かつ攪拌装置の回転数を、パラタングステン酸アンモニウム水和物の沈降の際に一緒に連行された有機相が分離するよう調整し、その際、ミキサーからの相混合物を、好ましくは沈降タンクの有機相と水性相との間の相境界領域中に導入する、請求項1から5までのいずれか1項に記載の方法。
- 相分離後に生じた母液の量をミキサー中に供給することで、ミキサー中のパラタングステン酸アンモニウム水和物の固体濃度を100〜1200g/l、好ましくは500〜800g/lに調整する、請求項1から6までのいずれか1項に記載の方法。
- タングステン装入有機相及びアンモニア含有水性溶液の再抽出のための供給速度を、ミキサー中の有機相の滞留時間が少なくとも1分であり、かつ、ミキサー中のアンモニア含有水性相の滞在時間が3時間を上回って調整されるよう選択し、その際、有機相の滞留時間は、ミキサー中の有機相の体積(l)とタングステン装入有機相の供給速度(l/時間)との比の60倍であり、かつアンモニア含有水性相の滞留時間は、ミキサー中のアンモニア含有水性相の体積(l)とアンモニア含有水性溶液の供給速度(l/時間)との比である、請求項1から7までのいずれか1項に記載の方法。
- 少なくとも75%が少なくとも200μmの長さを有する結晶から成り、この場合、該結晶の長さと幅との比が4.5:1を下回る、パラタングステン酸アンモニウム十水和物。
- 少なくとも1.7g/cm3、好ましくは1.8〜2.2g/cm3のかさ密度を有する、請求項9に記載のパラタングステン酸アンモニウム十水和物。
- 結晶の少なくとも75%が200〜1000μmの長さ、好ましくは300〜400μmの長さを有する、請求項9に記載のパラタングステン酸アンモニウム十水和物。
- 結晶の少なくとも75%が300〜400μmの長さ及び3.0:1〜3.5:1の長さと幅との比を示す、請求項9に記載のパラタングステン酸アンモニウム十水和物。
- 生成物の全量に対して少なくとも99.99%の純度を示す、請求項9から12までのいずれか1項に記載のパラタングステン酸アンモニウム十水和物。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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DE102007005286.5 | 2007-02-02 | ||
DE102007005286A DE102007005286B4 (de) | 2007-02-02 | 2007-02-02 | Verfahren zur Herstellung von Ammoniumparawolframathydraten und Ammoniumparawolframatdekahydrat |
PCT/EP2008/050995 WO2008092837A1 (de) | 2007-02-02 | 2008-01-29 | Verfahren zur herstellung von ammoniumparawolframathydraten und ammoniumparawolframatdekahydrat |
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JP2010517902A true JP2010517902A (ja) | 2010-05-27 |
JP2010517902A5 JP2010517902A5 (ja) | 2013-09-05 |
JP5424897B2 JP5424897B2 (ja) | 2014-02-26 |
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JP2009547657A Active JP5424897B2 (ja) | 2007-02-02 | 2008-01-29 | パラタングステン酸アンモニウム水和物を製造する方法及びパラタングステン酸アンモニウム十水和物 |
Country Status (8)
Country | Link |
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US (2) | US8216533B2 (ja) |
EP (1) | EP2118017B1 (ja) |
JP (1) | JP5424897B2 (ja) |
CN (1) | CN101600654B (ja) |
DE (2) | DE102007005286B4 (ja) |
ES (1) | ES2608681T3 (ja) |
PT (1) | PT2118017T (ja) |
WO (1) | WO2008092837A1 (ja) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010517903A (ja) * | 2007-02-02 | 2010-05-27 | ハー.ツェー.スタルク ゲゼルシャフト ミット ベシュレンクテル ハフツング | パラタングステン酸アンモニウム四水和物及び高純度のパラタングステン酸アンモニウム四水和物を製造する方法 |
JP2010517901A (ja) * | 2007-02-02 | 2010-05-27 | ハー.ツェー.スタルク ゲゼルシャフト ミット ベシュレンクテル ハフツング | ヘプタモリブデン酸アンモニウムの製造法 |
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JP4797099B2 (ja) * | 2009-10-01 | 2011-10-19 | Jx日鉱日石金属株式会社 | 高純度タングステン粉末の製造方法 |
ES2694780T3 (es) | 2010-05-19 | 2018-12-27 | Saint-Gobain Glass France | Antena optimizada en la anchura de banda mediante estructura híbrida de radiador planar y lineal |
ES2612233T3 (es) | 2011-02-16 | 2017-05-12 | Saint-Gobain Glass France | Cristal transparente con capa calefactora eléctrica así como procedimiento de fabricación del mismo |
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CN113816429B (zh) * | 2021-11-12 | 2023-04-18 | 江西钨业股份有限公司 | 仲钨酸铵的颗粒粗化方法 |
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US3052516A (en) * | 1959-02-10 | 1962-09-04 | Gen Mills Inc | Process for recovering tungsten values from solution |
DE1244141B (de) * | 1962-10-26 | 1967-07-13 | Blair Burwell | Verfahren zur Herstellung von hochreinem Ammoniumparawolframat |
US4092400A (en) * | 1977-04-11 | 1978-05-30 | Engelhard Minerals & Chemicals Corp. | Process for recovering high purity tungsten compositions from wolframite ores |
US4450144A (en) * | 1981-01-19 | 1984-05-22 | Amax Inc. | Ammonium hydroxide stripping of tungsten from organic solvents |
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DE150962C (ja) | ||||
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US3158438A (en) * | 1962-09-19 | 1964-11-24 | Union Carbide Corp | Solvent extraction process for recovering tungsten values from contaminated aqueous solutions |
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- 2008-01-29 JP JP2009547657A patent/JP5424897B2/ja active Active
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- 2008-01-29 WO PCT/EP2008/050995 patent/WO2008092837A1/de active Application Filing
- 2008-01-29 CN CN2008800039606A patent/CN101600654B/zh active Active
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010517903A (ja) * | 2007-02-02 | 2010-05-27 | ハー.ツェー.スタルク ゲゼルシャフト ミット ベシュレンクテル ハフツング | パラタングステン酸アンモニウム四水和物及び高純度のパラタングステン酸アンモニウム四水和物を製造する方法 |
JP2010517901A (ja) * | 2007-02-02 | 2010-05-27 | ハー.ツェー.スタルク ゲゼルシャフト ミット ベシュレンクテル ハフツング | ヘプタモリブデン酸アンモニウムの製造法 |
JP2013212985A (ja) * | 2007-02-02 | 2013-10-17 | Hc Starck Gmbh | パラタングステン酸アンモニウム四水和物及び高純度のパラタングステン酸アンモニウム四水和物を製造する方法 |
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Publication number | Publication date |
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US20100098619A1 (en) | 2010-04-22 |
DE102007063691B4 (de) | 2011-01-13 |
US20130029153A1 (en) | 2013-01-31 |
ES2608681T3 (es) | 2017-04-12 |
WO2008092837A1 (de) | 2008-08-07 |
DE102007005286A8 (de) | 2008-12-24 |
CN101600654A (zh) | 2009-12-09 |
EP2118017A1 (de) | 2009-11-18 |
DE102007005286B4 (de) | 2009-08-27 |
US8216533B2 (en) | 2012-07-10 |
DE102007005286A1 (de) | 2008-08-07 |
PT2118017T (pt) | 2016-12-14 |
CN101600654B (zh) | 2013-05-29 |
US8440161B2 (en) | 2013-05-14 |
EP2118017B1 (de) | 2016-10-12 |
JP5424897B2 (ja) | 2014-02-26 |
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