JP6400677B2 - 蒸気を用いた水素化プロセッシング触媒の活性化 - Google Patents
蒸気を用いた水素化プロセッシング触媒の活性化 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims description 102
- 230000004913 activation Effects 0.000 title description 11
- 239000002245 particle Substances 0.000 claims description 120
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 82
- 229930195733 hydrocarbon Natural products 0.000 claims description 71
- 150000002430 hydrocarbons Chemical class 0.000 claims description 71
- 239000004215 Carbon black (E152) Substances 0.000 claims description 69
- 239000011148 porous material Substances 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 54
- 229910052759 nickel Inorganic materials 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 35
- 238000005984 hydrogenation reaction Methods 0.000 claims description 30
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 30
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 26
- 229910052717 sulfur Inorganic materials 0.000 claims description 26
- 239000011593 sulfur Substances 0.000 claims description 26
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 20
- 229910052750 molybdenum Inorganic materials 0.000 claims description 19
- 239000011733 molybdenum Substances 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 9
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 8
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 6
- 150000002816 nickel compounds Chemical class 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 12
- 238000007792 addition Methods 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- 229910017052 cobalt Inorganic materials 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- 239000007858 starting material Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000011295 pitch Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 4
- 230000023556 desulfurization Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- -1 hydrodesulfurization Chemical compound 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 125000001741 organic sulfur group Chemical class 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229930192474 thiophene Natural products 0.000 description 2
- 150000003577 thiophenes Chemical class 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 238000009904 heterogeneous catalytic hydrogenation reaction Methods 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
-
- 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
- C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
- C10G49/02—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used
- C10G49/04—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used containing nickel, cobalt, chromium, molybdenum, or tungsten metals, or compounds thereof
-
- 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
- B01J37/04—Mixing
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/883—Molybdenum and nickel
-
- 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
-
- 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
- B01J37/0027—Powdering
- B01J37/0036—Grinding
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/06—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using steam
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Catalysts (AREA)
Description
この実施例は、本発明の方法に従って蒸気を用いてさらに活性化され得る自己活性化触媒の一実施形態の代表である、触媒Aの調製を記載する。
まず、2100重量部のアルミナ(わずか2%のシリカを含有)、加熱により85.04重量部の脱イオン水中に溶解させた63.17重量部の硝酸ニッケル(Ni(NO3)2)、217.05重量部の三酸化モリブデン(MoO3)粉末および900重量部の粉砕された再生Ni/Mo/P水素化処理触媒を、マラーミキサー内で、130重量部の69.9%濃硝酸および30グラムの市販の押出助剤とともに合わせることにより、触媒Aを調製した。混合中、総量で3222.9重量部の水をこれらの成分に添加した。これらの成分をおよそ30分間混合した。混合物は、4.12のpHおよび55.21重量パーセントのLOIを有していた。次いで、混合物を1.3mm trilobeダイを使用して押し出し、1.3trilobe押出粒子を形成した。次いで、押出粒子を100℃の温度で数時間空気中で乾燥した。
この実施例は、本発明の方法に従って蒸気を用いてさらに活性化され得る自己活性化触媒の別の実施形態の代表である、触媒Bの調製を記載する。
まず、2100重量部のアルミナ、加熱により85.04重量部の脱イオン水中に溶解させた63.17重量部の硝酸ニッケル(Ni(NO3)2)、217.05重量部の三酸化モリブデン(MoO3)粉末および900重量部の粉砕されたNi/Mo/P水素化処理触媒を、マラーミキサー内で、130重量部の69.9%濃硝酸および30グラムの市販の押出助剤とともに合わせることにより、触媒Bを調製した。混合中、総量で3222.9重量部の水をこれらの成分に添加した。これらの成分をおよそ30分間混合した。混合物は、4.12のpHおよび55.21重量パーセントのLOIを有していた。次いで、混合物を1.3mm trilobeダイを使用して押し出し、1.3trilobe押出粒子を形成した。次いで、押出粒子を100℃の温度で数時間空気中で乾燥した。
この実施例では、触媒Aと同様の組成および特性を有する自己活性化触媒を用いて、それぞれ表3および4に示される蒸留特性(ASTM Method D 7169によって決定される。)および他の特性を有する脱金属化アラビア産残油に対して水素化プロセッシングを行った。
Claims (8)
- 重質炭化水素原料を処理する際に使用される自己活性化水素化プロセッシング触媒を活性化させる方法であって、前記自己活性化水素化プロセッシング触媒を蒸気と接触させることを含み、
前記自己活性化水素化プロセッシング触媒が、無機酸化物粉末、500ミクロン未満の最大寸法を有する微細に分割された状態の三酸化モリブデン粉末およびニッケル化合物を共混練し、次いで共混練混合物を粒子に成形し、焼成してそれによって焼成粒子を生じることによって作製された、前記共混練混合物を含む前記焼成粒子を含み、前記焼成粒子が、金属として、前記焼成粒子の総重量に対し1から10重量パーセントの範囲の量で存在するモリブデン、およびニッケル対前記モリブデンの重量比が0.4未満である量で存在する前記ニッケルを含み、前記焼成粒子が、前記焼成粒子の総細孔体積の70%未満が70Åから150Åの範囲の直径を有する前記焼成粒子の細孔であり、前記焼成粒子の総細孔体積の少なくとも10%が130Åから300Åの範囲の直径を有する前記焼成粒子の細孔であり、前記焼成粒子の総細孔体積の1%から10%が1000Å超の直径を有する前記焼成粒子の細孔である、細孔サイズ分布を有し、
焼成が、約450℃(842°F)から約900℃(1652°F)の範囲の制御された焼成温度で、指定された細孔構造を有する前記自己活性化触媒をもたらすのに有効な焼成時間の間行われる、方法。 - 自己活性化触媒と接触させる蒸気の量が、重質炭化水素原料の重量に対し0.01重量%から10重量%の範囲内にある、請求項1に記載の方法。
- 重質炭化水素原料を自己活性化水素化プロセッシング触媒と接触させる前に、蒸気を重質炭化水素原料に添加する、請求項2に記載の方法。
- 蒸気を、自己活性化触媒を収容する反応容器に添加する、請求項2に記載の方法。
- 重質炭化水素原料を自己活性化水素化プロセッシング触媒と接触させる前に、水を蒸気に変換するのに十分な温度である重質炭化水素原料に水を添加する、請求項1に記載の方法。
- 自己活性化触媒と接触させる蒸気の量が、重質炭化水素原料の重量に対し2重量%から6重量%の範囲内にある、請求項1に記載の方法。
- 自己活性化水素化プロセッシング触媒を用いて処理された重質炭化水素原料が、1ppmwから250ppmwの範囲のニッケル含有量、5ppmwから250ppmwの範囲のバナジウム含有量、および2重量%から8重量%の範囲の硫黄含有量を有する、請求項2に記載の方法。
- 焼成粒子を含む前記自己活性化水素化プロセッシング触媒が、約700℃(1292°F)から約790℃(1454°F)の範囲の制御された焼成温度で、指定された細孔構造を有する前記自己活性化触媒をもたらすのに有効な焼成時間の間焼成される、請求項1に記載の方法。
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US201361815455P | 2013-04-24 | 2013-04-24 | |
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PCT/US2014/034876 WO2014176197A1 (en) | 2013-04-24 | 2014-04-22 | Activation of a hydroprocessing catalyst with steam |
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EP (1) | EP2988868A1 (ja) |
JP (1) | JP6400677B2 (ja) |
KR (1) | KR102203553B1 (ja) |
CN (1) | CN105121017B (ja) |
BR (1) | BR112015027028A2 (ja) |
CA (1) | CA2909056A1 (ja) |
RU (1) | RU2667146C2 (ja) |
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GB1021966A (en) * | 1963-11-05 | 1966-03-09 | Shell Int Research | A method of activating a catalyst comprising nickel oxide, molybdenum oxide and alumina |
US3720602A (en) * | 1971-02-26 | 1973-03-13 | Exxon Research Engineering Co | Water injection in a hydrodesulfurization process |
GB1468160A (en) * | 1973-10-05 | 1977-03-23 | Shell Int Research | Hydrocarbon conversion process |
US4113589A (en) * | 1977-04-25 | 1978-09-12 | Leach Sam L | High intensity energy transfer technique |
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KR20160003711A (ko) | 2016-01-11 |
US10220374B2 (en) | 2019-03-05 |
WO2014176197A1 (en) | 2014-10-30 |
RU2015149238A (ru) | 2017-05-29 |
CA2909056A1 (en) | 2014-10-30 |
JP2016522082A (ja) | 2016-07-28 |
EP2988868A1 (en) | 2016-03-02 |
RU2667146C2 (ru) | 2018-09-17 |
US20140323293A1 (en) | 2014-10-30 |
CN105121017A (zh) | 2015-12-02 |
RU2015149238A3 (ja) | 2018-03-19 |
CN105121017B (zh) | 2018-10-16 |
TW201500539A (zh) | 2015-01-01 |
SG11201508586YA (en) | 2015-11-27 |
KR102203553B1 (ko) | 2021-01-15 |
BR112015027028A2 (pt) | 2017-07-25 |
TWI650411B (zh) | 2019-02-11 |
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