JP6912564B2 - ゼオライト転換によるmtwフレームワーク型ゼオライトの合成 - Google Patents
ゼオライト転換によるmtwフレームワーク型ゼオライトの合成 Download PDFInfo
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- JP6912564B2 JP6912564B2 JP2019522394A JP2019522394A JP6912564B2 JP 6912564 B2 JP6912564 B2 JP 6912564B2 JP 2019522394 A JP2019522394 A JP 2019522394A JP 2019522394 A JP2019522394 A JP 2019522394A JP 6912564 B2 JP6912564 B2 JP 6912564B2
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- 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
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
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- 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
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/74—Noble metals
- B01J29/7469—MTW-type, e.g. ZSM-12, NU-13, TPZ-12 or Theta-3
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- 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
-
- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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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
-
- 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
- C01B39/026—After-treatment
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/02—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with ion-exchange material
- C10G25/03—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with ion-exchange material with crystalline alumino-silicates, e.g. molecular sieves
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/12—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
- C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
- C10G45/64—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
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- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/183—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself in framework positions
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- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/30—After treatment, characterised by the means used
- B01J2229/38—Base treatment
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- 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
- B01J37/18—Reducing with gases containing free hydrogen
Description
本出願は、2016年11月17日に出願された米国仮特許出願第62/423,271号の優先権を主張し、その開示は参照により本明細書にその全体が組み込まれる。
以下の用語は、本明細書を通して使用され、他に示されない限り、以下の意味を有する。
一般に、本MTWフレームワーク型ゼオライトは:(a)以下を含む反応混合物を調製すること:(1)FAUフレームワーク型ゼオライト;(2)ポリエチレンイミン;(3)フッ化物イオン;及び(4)水;ならびに(b)反応混合物を、MTWフレームワーク型ゼオライトの結晶を形成するのに十分な結晶化条件に供することによって合成される。
上記反応混合物からのMTWフレームワーク型ゼオライトの結晶化は、例えばポリプロピレンジャー又はTeflonラインド又はステンレス鋼オートクレーブのような適切な反応容器中で、125℃〜200℃の温度で、静的、回転又は撹拌条件下、使用される温度で結晶化が起こるのに十分な時間、例えば5〜20日間行うことができる。結晶化は通常、自己圧下、閉鎖系で行われる。
Al2O3:(n)SiO2
式中、n≧10(例えば、30〜500又は30〜100)。
以下の例示的な例は非限定的であることを意図している。
Teflonライナーに1.08gのCBV−780 Y−ゼオライト(Zeolyst International、SiO2/Al2O3モル比=80)、4.86gの脱イオン水、0.42gの線状ポリエチレンイミン(Mn=1800)及び最後に0.36gの濃HFを充填した。得られたゲルを均質になるまで撹拌した。次いで、ライナーに蓋をしてParr鋼オートクレーブ反応器内に置いた。次いでオートクレーブをオーブンに入れ、回転させながら(43rpm)11日間170℃で加熱した。固体生成物を濾過により回収し、脱イオン水で洗浄し、95℃で乾燥した。
例1からの材料を空気中595℃で5時間焼成した。焼成後、室温で3日間4.5gの0.148NのNH4OH溶液と5.5gの脱イオン水、次いで(NH3)4Pd(NO3)2溶液(pH9.5に緩衝化)とを混合し、こうして1gのゼオライトと混合した1gのこの溶液が0.5重量%のPd担持量を提供するように材料にパラジウムを担持させた。回収したPd/MTWゼオライトを脱イオン水で洗浄し、95℃で乾燥した後、空気中482℃で3時間焼成した。焼成Pd/MTW触媒を次いでペレット化し、粉砕し、20〜40メッシュに篩分けした。
Claims (9)
- 前記ポリエチレンイミンが線状ポリエチレンイミンである、請求項1に記載の方法。
- 前記線状ポリエチレンイミンが、1500〜5000の範囲の数平均分子量を有する、請求項2に記載の方法。
- 前記結晶化条件が125℃〜200℃の温度を含む、請求項1に記載の方法。
- ポリエチレンイミンをその細孔構造内に含むMTWフレームワーク型ゼオライト。
- 前記ポリエチレンイミンが線状ポリエチレンイミンである、請求項5に記載のMTWフレームワーク型ゼオライト。
- 前記線状ポリエチレンイミンが、1500〜5000の範囲の数平均分子量を有する、請求項8に記載のMTWフレームワーク型ゼオライト。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201662423271P | 2016-11-17 | 2016-11-17 | |
US62/423,271 | 2016-11-17 | ||
PCT/US2017/056925 WO2018093510A1 (en) | 2016-11-17 | 2017-10-17 | Synthesis of mtw framework type zeolites via interzeolite transformation |
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JP2020514209A JP2020514209A (ja) | 2020-05-21 |
JP2020514209A5 JP2020514209A5 (ja) | 2020-10-22 |
JP6912564B2 true JP6912564B2 (ja) | 2021-08-04 |
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JP2019522394A Active JP6912564B2 (ja) | 2016-11-17 | 2017-10-17 | ゼオライト転換によるmtwフレームワーク型ゼオライトの合成 |
Country Status (6)
Country | Link |
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US (1) | US10478811B2 (ja) |
EP (1) | EP3541749B1 (ja) |
JP (1) | JP6912564B2 (ja) |
KR (1) | KR102413863B1 (ja) |
CN (1) | CN109890757B (ja) |
WO (1) | WO2018093510A1 (ja) |
Families Citing this family (1)
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CN113772855A (zh) * | 2020-06-10 | 2021-12-10 | 中国石油化工股份有限公司 | 含镍铬废水的处理方法 |
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US3832449A (en) | 1971-03-18 | 1974-08-27 | Mobil Oil Corp | Crystalline zeolite zsm{14 12 |
US4537758A (en) | 1979-03-21 | 1985-08-27 | Mobil Oil Corporation | Process for preparing highly siliceous porous ZSM-12 type crystalline material |
US4452769A (en) | 1979-03-21 | 1984-06-05 | Mobil Oil Corporation | Method of preparing crystalline zeolite |
GB2079735A (en) | 1980-07-07 | 1982-01-27 | Chevron Res | Novel zeolite designated CZH-5 |
EP0059059B2 (en) | 1981-02-23 | 1990-04-18 | Imperial Chemical Industries Plc | Zeolites |
US4391785A (en) | 1981-12-21 | 1983-07-05 | Mobil Oil Corporation | Preparation of ZSM-12 type zeolites |
US4557919A (en) | 1983-04-12 | 1985-12-10 | Teijin Petrochemical Industries Ltd. | Production of crystalline zeolites |
US4482531A (en) | 1983-04-29 | 1984-11-13 | Mobil Oil Corporation | Synthesis of ZSM-12 zeolite |
US4552739A (en) | 1983-12-09 | 1985-11-12 | Mobil Oil Corporation | Method of preparing crystalline zeolite ZSM-12 and product |
US4539193A (en) | 1984-05-23 | 1985-09-03 | Mobil Oil Corporation | Synthesis of crystalline silicate ZSM-12 |
GB8413370D0 (en) | 1984-05-24 | 1984-06-27 | British Petroleum Co Plc | Theta-3 |
US4552738A (en) | 1984-05-25 | 1985-11-12 | Mobil Oil Corporation | Synthesis of crystalline silicate ZSM-12 |
US4585637A (en) | 1984-06-26 | 1986-04-29 | Mobil Oil Corporation | Synthesis of crystalline silicate ZSM-12 |
US4636373A (en) | 1984-06-26 | 1987-01-13 | Mobil Oil Corporation | Synthesis of crystalline silicate ZSM-12 using dibenzyldimethylammonium cations and the product produced |
US4585746A (en) | 1984-06-27 | 1986-04-29 | Mobil Oil Corporation | Synthesis of crystalline silicate ZSM-12 |
US5021141A (en) | 1990-09-14 | 1991-06-04 | Mobil Oil Corp. | Synthesis of crystalline ZSM-12 type structure |
FR2670772B1 (fr) * | 1990-12-21 | 1993-04-09 | Inst Francais Du Petrole | Zeolithe de type mtw et son procede de preparation. |
US5137705A (en) | 1991-04-08 | 1992-08-11 | Mobil Oil Corp. | Synthesis of crystalline silicate ZSM-12 |
US5192521A (en) | 1991-11-19 | 1993-03-09 | Mobil Oil Corp. | Synthesis of crystalline silicate ZSM-12 |
DE19939416A1 (de) * | 1999-08-20 | 2001-02-22 | Basf Ag | Verfahren zur Herstellung eines kristallinen, zeolithischen Feststoffs |
US6652832B2 (en) | 2001-02-05 | 2003-11-25 | Exxonmobil Oil Corporation | Synthesis of ZSM-12 |
US6660682B2 (en) * | 2001-11-30 | 2003-12-09 | Exxon Mobil Chemical Patents Inc. | Method of synthesizing molecular sieves |
US7211239B2 (en) * | 2005-04-22 | 2007-05-01 | Basf Aktiengesellschaft | Process for preparing a nanosized zeolitic material |
FR2936790B1 (fr) * | 2008-10-07 | 2010-09-24 | Inst Francais Du Petrole | Procede de preparation d'une zeolithe de type structural mtw |
US8562942B2 (en) * | 2009-04-09 | 2013-10-22 | California Institute Of Technology | Molecular sieves and related methods and structure directing agents |
US20110034749A1 (en) * | 2009-08-07 | 2011-02-10 | Exxonmobil Research And Engineering Company | Synthesis and use of ZSM-12 |
US8202506B2 (en) | 2009-11-17 | 2012-06-19 | Exxonmobil Research And Engineering Company | High activity small crystal ZSM-12 |
JP5615530B2 (ja) * | 2009-11-20 | 2014-10-29 | ユニゼオ株式会社 | Mtw型ゼオライトの製造方法 |
US8679451B2 (en) | 2009-11-20 | 2014-03-25 | Chevron U.S.A. Inc. | Method for making aluminosilicate ZSM-12 |
EP2928826B1 (en) * | 2012-12-10 | 2017-12-20 | ExxonMobil Research and Engineering Company | Synthesis of molecular sieve itq-32 |
JP2014122142A (ja) * | 2012-12-21 | 2014-07-03 | Mitsubishi Plastics Inc | 遷移金属含有ゼオライト、及びその製造方法 |
US9233856B2 (en) * | 2013-04-20 | 2016-01-12 | Uop Llc | Use of zeolitic materials for removing mercury (+2) ions from liquid streams |
US9126190B2 (en) | 2013-07-30 | 2015-09-08 | Chevron U.S.A. Inc. | Zeolite SSZ-70 having enhanced external surface area |
US9938157B2 (en) * | 2014-07-23 | 2018-04-10 | Chevron U.S.A. Inc. | Interzeolite transformation and metal encapsulation in the absence of an SDA |
US9802831B2 (en) * | 2014-07-23 | 2017-10-31 | Chevron U.S.A. Inc. | Synthesis of high silica zeolite via interzeolite transformation without OSDAs |
-
2017
- 2017-10-17 KR KR1020197017225A patent/KR102413863B1/ko active IP Right Grant
- 2017-10-17 US US15/785,546 patent/US10478811B2/en active Active
- 2017-10-17 WO PCT/US2017/056925 patent/WO2018093510A1/en unknown
- 2017-10-17 EP EP17801129.2A patent/EP3541749B1/en active Active
- 2017-10-17 JP JP2019522394A patent/JP6912564B2/ja active Active
- 2017-10-17 CN CN201780067627.0A patent/CN109890757B/zh active Active
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Publication number | Publication date |
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KR102413863B1 (ko) | 2022-06-29 |
EP3541749A1 (en) | 2019-09-25 |
CN109890757A (zh) | 2019-06-14 |
US20180133701A1 (en) | 2018-05-17 |
US10478811B2 (en) | 2019-11-19 |
CN109890757B (zh) | 2022-05-03 |
WO2018093510A1 (en) | 2018-05-24 |
EP3541749B1 (en) | 2020-05-27 |
KR20190085053A (ko) | 2019-07-17 |
JP2020514209A (ja) | 2020-05-21 |
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