RU2017100960A - Катализатор с бимодальным распределением пор, способ его получения путем перемешивания с активной фазой и его применение в гидрообработке углеводородных остатков - Google Patents
Катализатор с бимодальным распределением пор, способ его получения путем перемешивания с активной фазой и его применение в гидрообработке углеводородных остатков Download PDFInfo
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- RU2017100960A RU2017100960A RU2017100960A RU2017100960A RU2017100960A RU 2017100960 A RU2017100960 A RU 2017100960A RU 2017100960 A RU2017100960 A RU 2017100960A RU 2017100960 A RU2017100960 A RU 2017100960A RU 2017100960 A RU2017100960 A RU 2017100960A
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- Prior art keywords
- catalyst
- alumina
- aluminum
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- 239000003054 catalyst Substances 0.000 title claims 21
- 238000000034 method Methods 0.000 title claims 13
- 150000002430 hydrocarbons Chemical group 0.000 title claims 5
- 238000002156 mixing Methods 0.000 title claims 3
- 230000002902 bimodal effect Effects 0.000 title claims 2
- 238000004519 manufacturing process Methods 0.000 title 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 11
- 239000002243 precursor Substances 0.000 claims 10
- 229910052751 metal Inorganic materials 0.000 claims 8
- 239000002184 metal Substances 0.000 claims 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 6
- 239000000725 suspension Substances 0.000 claims 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 5
- 239000002253 acid Substances 0.000 claims 5
- 229910052739 hydrogen Inorganic materials 0.000 claims 5
- 239000001257 hydrogen Substances 0.000 claims 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 4
- 239000004215 Carbon black (E152) Substances 0.000 claims 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 4
- 229910052782 aluminium Inorganic materials 0.000 claims 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 4
- 229930195733 hydrocarbon Natural products 0.000 claims 4
- 230000000737 periodic effect Effects 0.000 claims 4
- 239000011574 phosphorus Substances 0.000 claims 4
- 229910052698 phosphorus Inorganic materials 0.000 claims 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 4
- 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 claims 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 3
- 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 claims 3
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims 3
- 238000006356 dehydrogenation reaction Methods 0.000 claims 3
- 239000011159 matrix material Substances 0.000 claims 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims 3
- 229910052753 mercury Inorganic materials 0.000 claims 3
- 229910052750 molybdenum Inorganic materials 0.000 claims 3
- 239000011733 molybdenum Substances 0.000 claims 3
- KVOIJEARBNBHHP-UHFFFAOYSA-N potassium;oxido(oxo)alumane Chemical compound [K+].[O-][Al]=O KVOIJEARBNBHHP-UHFFFAOYSA-N 0.000 claims 3
- 229910001388 sodium aluminate Inorganic materials 0.000 claims 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 2
- 238000000975 co-precipitation Methods 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 2
- 239000011148 porous material Substances 0.000 claims 2
- 239000000843 powder Substances 0.000 claims 2
- 239000002994 raw material Substances 0.000 claims 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 230000002378 acidificating effect Effects 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 239000012431 aqueous reaction media Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 238000004939 coking Methods 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 239000003921 oil Substances 0.000 claims 1
- 239000006259 organic additive Substances 0.000 claims 1
- 238000002459 porosimetry Methods 0.000 claims 1
- 239000012429 reaction media Substances 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
Classifications
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- B01J21/04—Alumina
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- 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
- C10G45/06—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 nickel or cobalt metal, or compounds thereof
- C10G45/08—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 nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
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- 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
- C10G45/14—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 with moving solid particles
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- 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
- C10G45/14—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 with moving solid particles
- C10G45/18—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 with moving solid particles according to the "moving-bed" technique
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- C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
- C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
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- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
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Claims (35)
1. Способ получения катализатора со смешиваемой активной фазой, содержащего по меньшей мере один металл группы VIB периодической системы элементов, необязательно по меньшей мере один металл группы VIII периодической системы элементов, необязательно фосфор и матрицу по существу из обожженного оксида алюминия, включающий следующие этапы:
a) этап растворения кислотного предшественника алюминия, выбранного из сульфата алюминия, хлорида алюминия и нитрата алюминия, в воде при температуре от 20°C до 90°C, значении pH от 0,5 до 5, в течение периода продолжительностью от 2 до 60 минут;
b) этап регулирования значения pH путем добавления в суспензию, полученную на этапе a), по меньшей мере одного щелочного предшественника, выбранного из алюмината натрия, алюмината калия, аммиака, гидроксида натрия и гидроксида калия, при температуре от 20°C до 90°C и значении pH от 7 до 10 в течение периода продолжительностью от 5 до 30 минут;
c) этап соосаждения суспензии, полученной на этапе b), путем добавления в суспензию по меньшей мере одного щелочного предшественника, выбранного из алюмината натрия, алюмината калия, аммиака, гидроксида натрия и гидроксида калия, и по меньшей мере одного кислотного предшественника, выбранного из сульфата алюминия, хлорида алюминия, нитрата алюминия, серной кислоты, соляной кислоты и азотной кислоты, причем по меньшей мере один из кислотного или щелочного предшественников содержит алюминий, относительный расход кислотного и щелочного предшественников выбирают так, чтобы получить значение pH реакционной среды в интервале от 7 до 10, и расход кислотного и щелочного предшественника или предшественников, содержащих алюминий, регулируют так, чтобы получить конечную концентрацию оксида алюминия в суспензии от 10 до 38 г/л;
d) этап фильтрации суспензии, полученной на этапе c) соосаждения, с получением алюмогеля;
e) этап сушки указанного алюмогеля, полученного на этапе d), с получением порошка,
f) этап термообработки порошка, полученного на этапе e), при температуре от 500°C до 1000°C, в течение периода продолжительностью от 2 до 10 ч, в присутствии или в отсутствие потока воздуха, содержащего до 60 об.% воды, с получением обожженного пористого оксида алюминия;
g) этап перемешивания полученного обожженного пористого оксида алюминия с раствором, содержащим по меньшей мере один предшественник металла активной фазы, с получением пасты;
h) этап формования полученной пасты,
i) этап сушки формованной пасты при температуре менее или равной 200°C, с получением сухого катализатора,
j) необязательный этап термообработки сухого катализатора при температуре от 200°C до 1000°C в присутствии или в отсутствие воды.
2. Способ по п. 1, в котором концентрация оксида алюминия в суспензии алюмогеля, полученной на этапе c), составляет от 13 до 35 г/л.
3. Способ по п. 2, в котором концентрация оксида алюминия в суспензии алюмогеля, полученной на этапе c), составляет от 15 до 33 г/л.
4. Способ по одному из пп. 1-3, в котором кислотный предшественник выбран из сульфата алюминия, хлорида алюминия и нитрата алюминия.
5. Способ по одному из пп. 1-4, в котором щелочной предшественник выбран из алюмината натрия и алюмината калия.
6. Способ по одному из пп. 1-5, в котором на этапах a), b), c) водная реакционная среда является предпочтительно водой, и указанные этапы проводят при перемешивании в отсутствие органической добавки.
7. Катализатор гидроконверсии с бимодальной пористой структурой, содержащий:
- оксидную матрицу по существу из обожженного оксида алюминия,
- активную гидрирующую-дегидрирующую фазу, содержащую по меньшей мере один металл группы VIB периодической системы элементов, необязательно по меньшей мере один металл группы VIII периодической системы элементов, необязательно фосфор,
причем указанная активная фаза по меньшей мере частично распределена посредством смешивания в указанной оксидной матрице по существу из обожженного оксида алюминия,
причем указанный катализатор имеет: удельную поверхность SBET более 100 м2/г, среднеобъемный диаметр мезопор от 12 до 25 нм включительно, среднеобъемный диаметр макропор от 250 до 1500 нм включительно, объем мезопор, измеренный интрузией на ртутном порозиметре, более или равный 0,55 мл/г, и полный объем пор, измеренный методом ртутной порозиметрии, более или равный 0,70 мл/г.
8. Катализатор гидроконверсии по п. 7, имеющий среднеобъемный диаметр мезопор, определенный интрузией на ртутном порозиметре, от 13 до 17 нм включительно.
9. Катализатор гидроконверсии по одному из пп. 7-8, объем макропор в котором составляет от 10% до 40% от полного объема пор.
10. Катализатор гидроконверсии по одному из пп. 7-9, у которого объем мезопор составляет более 0,70 мл/г.
11. Катализатор гидроконверсии по одному из пп. 7-10, не содержащий микропор.
12. Катализатор гидроконверсии по одному из пп. 7-11, в котором содержание металла группы VIB, выраженное в триоксиде металла группы VIB, составляет от 2 до 10 вес.% от полного веса катализатора, содержание металла группы VIII, выраженное в оксиде металла группы VIII, составляет от 0,0 до 3,6 вес.% от полного веса катализатора, и содержание элемента фосфор, выраженное в пентоксиде фосфора, составляет от 0 до 5 вес.% от полного веса катализатора.
13. Катализатор гидроконверсии по одному из предыдущих пунктов, в котором активная гидрирующая-дегидрирующая фаза состоит из молибдена, или никеля и молибдена, или кобальта и молибдена.
14. Катализатор гидроконверсии по п. 13, в котором активная гидрирующая-дегидрирующая фаза дополнительно содержит фосфор.
15. Способ гидрообработки тяжелого углеводородного сырья, выбранного из атмосферных остатков, вакуумных остатков с прямой перегонки, деасфальтированных масел, остатков с конверсионных процессов, таких, например, как остатки от коксования, гидроконверсии в неподвижном слое, в кипящем слое или же в движущемся слое, используемых по отдельности или в смеси, причем способ включает контактирование указанного сырья с водородом и катализатором, который может быть получен по одному из пп. 1-6, или катализатором по одному из пп. 7-14.
16. Способ гидрообработки по п. 15, осуществляемый частично в кипящем слое при температуре от 320°C до 450°C, парциальном давлении водорода от 3 МПа до 30 МПа, объемной скорости от 0,1 до 10 объемов сырья на объем катализатора в час и при отношении газообразного водорода к жидкому углеводородному сырью от 100 до 3000 нормальных кубических метров на кубический метр.
17. Способ гидрообработки по п. 15 или 16, осуществляемый по меньшей мере частично в неподвижном слое при температуре от 320°C до 450°C, парциальном давлении водорода от 3 МПа до 30 МПа, при объемной скорости от 0,05 до 5 объемов сырья на объем катализатора в час и при отношении газообразного водорода к жидкому углеводородному сырью от 200 до 5000 нормальных кубических метров на кубический метр.
18. Способ гидрообработки тяжелого углеводородного сырья типа остатков в неподвижном слое по п. 17, включающий в себя по меньшей мере:
a) стадию гидродеметаллизации,
b) стадию гидрообессеривания,
причем указанный катализатор используют по меньшей мере на одной из указанных стадий a) и b).
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PCT/EP2015/062822 WO2015189196A1 (fr) | 2014-06-13 | 2015-06-09 | Catalyseur a porosite bimodal, son procede de preparation par comalaxage de la phase active et son utilisation en hydrotraitement de residus d'hydrocarbures |
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US10604709B2 (en) | 2017-02-12 | 2020-03-31 | Magēmā Technology LLC | Multi-stage device and process for production of a low sulfur heavy marine fuel oil from distressed heavy fuel oil materials |
US11788017B2 (en) | 2017-02-12 | 2023-10-17 | Magëmã Technology LLC | Multi-stage process and device for reducing environmental contaminants in heavy marine fuel oil |
US20220410124A1 (en) * | 2019-11-29 | 2022-12-29 | Rhodia Operations | Alumina with a particular pore profile |
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US4154812A (en) * | 1977-03-25 | 1979-05-15 | W. R. Grace & Co. | Process for preparing alumina |
US4353791A (en) * | 1981-02-27 | 1982-10-12 | Standard Oil Company (Indiana) | Hydrotreating catalyst and liquefaction of coal |
US4941964A (en) * | 1988-03-14 | 1990-07-17 | Texaco Inc. | Hydrotreatment process employing catalyst with specified pore size distribution |
US4976848A (en) | 1988-10-04 | 1990-12-11 | Chevron Research Company | Hydrodemetalation and hydrodesulfurization using a catalyst of specified macroporosity |
US5089463A (en) | 1988-10-04 | 1992-02-18 | Chevron Research And Technology Company | Hydrodemetalation and hydrodesulfurization catalyst of specified macroporosity |
DE4310971A1 (de) * | 1993-04-03 | 1994-10-06 | Huels Chemische Werke Ag | Nickel/Aluminiumoxid-Katalysator, Verfahren zu seiner Herstellung, seine Verwendung sowie Verfahren zur Hydrierung von aromatischen Kohlenwasserstoffen mit Hilfe des Katalysators |
US5968348A (en) | 1994-05-16 | 1999-10-19 | Texaco Inc. | Hydroconversion process employing a phosphorus loaded NiMo catalyst with specified pore size distribution |
ATE269159T1 (de) * | 1994-07-29 | 2004-07-15 | Chevron Usa Inc | Rückstand-umwandlungskatalysator mit niedrigen makroporengehalt |
US5620592A (en) * | 1994-07-29 | 1997-04-15 | Chevron U.S.A. Inc. | Low macropore resid conversion catalyst |
WO2000033957A1 (fr) | 1998-12-08 | 2000-06-15 | Japan Energy Corporation | Catalyseur d'hydrodesulfuration et son procede de preparation |
US6589908B1 (en) * | 2000-11-28 | 2003-07-08 | Shell Oil Company | Method of making alumina having bimodal pore structure, and catalysts made therefrom |
JP4638610B2 (ja) | 2001-01-05 | 2011-02-23 | 日本ケッチェン株式会社 | 水素化処理用触媒並びに水素化処理方法 |
FR2819430B1 (fr) * | 2001-01-15 | 2003-02-28 | Inst Francais Du Petrole | Catalyseur comportant une silice-alumine et son utilisation en hydrocraquage de charges hydrocarbonees |
US6919294B2 (en) | 2002-02-06 | 2005-07-19 | Japan Energy Corporation | Method for preparing hydrogenation purification catalyst |
EP1567262B1 (en) | 2002-12-06 | 2021-02-03 | Albemarle Netherlands B.V. | Heavy feed hydroprocessing using a mixture of catalysts |
RU2376059C2 (ru) | 2003-09-17 | 2009-12-20 | Шелл Интернэшнл Рисерч Маатсхаппий Б.В. | Способ и катализатор гидроконверсии тяжелого углеводородного исходного сырья |
FR2888584B1 (fr) * | 2005-07-18 | 2010-12-10 | Inst Francais Du Petrole | Procede de production de distillats moyens par hydroisomerisation et hydrocraquage de charges issues du procede fischer-tropsch utilisant un lit de garde multifonctionnel |
US9068131B2 (en) | 2008-07-03 | 2015-06-30 | Shell Oil Company | Catalyst composition and a process that uses the catalyst composition for the hydroconversion of a heavy hydrocarbon feedstock |
FR2940143B1 (fr) * | 2008-12-18 | 2015-12-11 | Inst Francais Du Petrole | Catalyseurs d'hydrodemetallation et d'hydrodesulfuration et mise en oeuvre dans un procede d'enchainement en formulation unique |
CN103052443B (zh) | 2010-08-13 | 2016-01-20 | 国际壳牌研究有限公司 | 用废催化剂细粉制备的加氢催化剂及其用途 |
JP2014529502A (ja) * | 2011-09-01 | 2014-11-13 | アドバンスド・リフアイニング・テクノロジーズ・エルエルシー | 触媒支持体及びそれから調製される触媒 |
-
2014
- 2014-06-13 FR FR1455416A patent/FR3022157B1/fr not_active Expired - Fee Related
-
2015
- 2015-06-09 US US15/318,561 patent/US20170120229A1/en not_active Abandoned
- 2015-06-09 CN CN201580043355.1A patent/CN106922134B/zh active Active
- 2015-06-09 RU RU2017100960A patent/RU2687084C2/ru active
- 2015-06-09 EP EP15729134.5A patent/EP3154680A1/fr not_active Withdrawn
- 2015-06-09 WO PCT/EP2015/062822 patent/WO2015189196A1/fr active Application Filing
Also Published As
Publication number | Publication date |
---|---|
US20170120229A1 (en) | 2017-05-04 |
FR3022157B1 (fr) | 2017-09-01 |
FR3022157A1 (fr) | 2015-12-18 |
EP3154680A1 (fr) | 2017-04-19 |
RU2687084C2 (ru) | 2019-05-07 |
WO2015189196A1 (fr) | 2015-12-17 |
CN106922134A (zh) | 2017-07-04 |
CN106922134B (zh) | 2020-05-05 |
RU2017100960A3 (ru) | 2018-12-21 |
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