JP5524887B2 - 重質油からの水素化分解油の製造方法 - Google Patents
重質油からの水素化分解油の製造方法 Download PDFInfo
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- 239000000295 fuel oil Substances 0.000 title claims description 47
- 239000003921 oil Substances 0.000 title claims description 36
- 238000000034 method Methods 0.000 title description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 147
- 239000007789 gas Substances 0.000 claims description 128
- 239000003054 catalyst Substances 0.000 claims description 69
- 229910052742 iron Inorganic materials 0.000 claims description 69
- 239000007787 solid Substances 0.000 claims description 67
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 238000006243 chemical reaction Methods 0.000 claims description 59
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 45
- 229910001882 dioxygen Inorganic materials 0.000 claims description 44
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 33
- 239000002002 slurry Substances 0.000 claims description 31
- 238000004519 manufacturing process Methods 0.000 claims description 29
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 28
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 28
- 239000007795 chemical reaction product Substances 0.000 claims description 27
- 239000001257 hydrogen Substances 0.000 claims description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 27
- 238000004517 catalytic hydrocracking Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 18
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 42
- 239000011343 solid material Substances 0.000 description 29
- 229910052717 sulfur Inorganic materials 0.000 description 29
- 239000011593 sulfur Substances 0.000 description 29
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 22
- 239000000203 mixture Substances 0.000 description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 16
- 229910052799 carbon Inorganic materials 0.000 description 16
- 239000002994 raw material Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 8
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 6
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000010779 crude oil Substances 0.000 description 5
- 230000009849 deactivation Effects 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 229910000859 α-Fe Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 239000000571 coke Substances 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000003426 co-catalyst Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910052595 hematite Inorganic materials 0.000 description 3
- 239000011019 hematite Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 229910003296 Ni-Mo Inorganic materials 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- NFMAZVUSKIJEIH-UHFFFAOYSA-N bis(sulfanylidene)iron Chemical compound S=[Fe]=S NFMAZVUSKIJEIH-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007327 hydrogenolysis reaction Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003027 oil sand Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 229910052952 pyrrhotite Inorganic materials 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 239000011275 tar sand Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910006540 α-FeOOH Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
- C10G47/02—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used
-
- 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
- C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
- C10G47/24—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions with moving solid particles
- C10G47/30—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions with moving solid particles according to the "fluidised-bed" technique
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Catalysts (AREA)
- Processing Of Solid Wastes (AREA)
Description
3FeS+10H2O → Fe3O4+3SO2+10H2 ・・・ (1)
3H2+SO2 → H2S+2H2O ・・・ (2)
2H2S+SO2 → 3S+2H2O ・・・ (3)
C+H2O → CO+H2 ・・・ (4)
C+2H2O → CO2+2H2 ・・・ (5)
CO+H2O → CO2+H2 ・・・ (6)
図1に示すシステムフローチャートに従い、石油系重質油の水素化分解を行い、水素化分解油を製造した。原料となる重質油として表1に示す留分組成の減圧蒸留残渣(以下、「VR」と称する場合がある)を用い、鉄系触媒としてリモナイトを用いた。鉄系触媒は、原料VR100質量部に対し鉄原子として1質量部加え、助触媒として硫黄を鉄系触媒の鉄添加量の1.2倍モル加えた。スラリー床反応器には、原料VR、鉄系触媒、助触媒がそれぞれ供給され、さらに後段プロセスから循環する343℃−525℃留分と+525℃留分からなる重質反応生成物が供給された。重質反応生成物の各留分の量は、343℃−525℃留分が原料VR100質量部に対し59質量部(59%VR)であり、+525℃留分が原料VR100質量部に対し50質量部(50%VR)であった。なお、原料VRに対する質量基準の割合を「%VR」で表記する。スラリー床反応器では、圧力12MPa、温度450℃の条件で90分間、水素ガスを供給しながら重質油の水素化分解を行い、水素化分解油を得た。水素化分解により、各留分が表2に示す収率で得られた。オイル(C5−525℃)収率は86.8%VRであった。
実施例1において固液分離装置で分離され1mm以下に粉砕された固形物を、反応ガスとして水蒸気のみが供給されている反応器に供給した。固形物は、反応器内で常圧下600℃、800℃、または900℃で45分間処理した。処理前および処理後の固形物の組成、および、反応器からの排出ガスの組成を表6に示す。なお表6に示す組成は、反応器に供給する固形物質量に対する各成分の質量割合を表す。
実施例1において、第1反応器に空気のみからなる第1ガスを供給し、固形物を第1反応器内で常圧下500℃で10分間第1ガスで処理した以外は、実施例1と同様にして重質油の処理を行った。第1反応器から排出された固形物の組成、および、排出ガスの組成と収支を表7に示し、第2反応器から排出された固形物の組成、および、排出ガスの組成と収支を表8に示す。なお表7および表8に示す組成は、第1反応器に供給する固形物質量に対する各成分の質量割合を表し、収支は、第1反応器に供給する固形物質量100kg当たりの各成分の物質量を表す。
Claims (8)
- (a)重質油を、鉄系触媒の存在下、スラリー床反応器中で水素化分解を行う工程と、
(b)前記工程(a)で得られた反応生成物を固液分離して、前記鉄系触媒を含有する固形物を得る工程と、
(c)前記固形物と、水蒸気と分子状酸素を含有する第1ガスとを500℃以上700℃未満の第1反応器内に供給し、前記固形物を前記第1ガスと接触させる工程と、
(d)前記工程(c)で処理された固形物と、水蒸気を含有する第2ガスとを700℃以上1000℃以下の第2反応器内に供給し、前記工程(c)で処理された固形物を前記第2ガスと接触させる工程
を有することを特徴とする重質油からの水素化分解油の製造方法。 - 前記第1ガスの水蒸気/分子状酸素モル比が5以上20以下である請求項1に記載の水素化分解油の製造方法。
- 前記第2ガスの水蒸気/分子状酸素モル比が20より大きい請求項1または2に記載の水素化分解油の製造方法。
- 前記第1反応器内の温度は前記第2反応器内の温度より低い請求項1〜3のいずれか一項に記載の水素化分解油の製造方法。
- 前記第1反応器からの排出ガスに水蒸気を加えて前記第2ガスとして用いる請求項1〜4のいずれか一項に記載の水素化分解油の製造方法。
- 前記工程(d)で生成した硫化水素および/または水素を、前記工程(a)の前記スラリー床反応器に供給する請求項1〜5のいずれか一項に記載の水素化分解油の製造方法。
- さらに、前記工程(c)および/または前記工程(d)で生成した硫化水素と二酸化硫黄をクラウス反応器に導入してクラウス反応させ、単体硫黄を得る工程(e)を有し、
前記単体硫黄を、前記工程(a)の前記スラリー床反応器に供給する請求項1〜6のいずれか一項に記載の水素化分解油の製造方法。 - 前記クラウス反応器から排出され硫化水素を含有する排出ガスを、前記工程(a)の前記スラリー床反応器に供給する請求項7に記載の水素化分解油の製造方法。
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JP2011059787A JP5524887B2 (ja) | 2011-03-17 | 2011-03-17 | 重質油からの水素化分解油の製造方法 |
BR102012005501A BR102012005501B1 (pt) | 2011-03-17 | 2012-03-12 | processo de produção de óleo hidrocraqueado a partir de óleo pesado |
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JP2011059787A JP5524887B2 (ja) | 2011-03-17 | 2011-03-17 | 重質油からの水素化分解油の製造方法 |
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JP2012193314A JP2012193314A (ja) | 2012-10-11 |
JP5524887B2 true JP5524887B2 (ja) | 2014-06-18 |
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BR (1) | BR102012005501B1 (ja) |
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JP6715709B2 (ja) * | 2016-07-11 | 2020-07-01 | 株式会社神戸製鋼所 | 水素化分解油の製造方法及び水素化分解油の製造装置 |
JP6623147B2 (ja) * | 2016-12-12 | 2019-12-18 | 株式会社神戸製鋼所 | 水素化分解油の製造方法 |
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JPS5378203A (en) * | 1976-12-21 | 1978-07-11 | Agency Of Ind Science & Technol | Gydrocracking of hydrocarbons by powdered catalysts |
US4621069A (en) * | 1983-10-03 | 1986-11-04 | Hri, Inc. | Continuous process for catalyst regeneration by staged burnoff of carbon and sulfur compounds |
JPH01131297A (ja) * | 1987-08-03 | 1989-05-24 | Res Assoc Petroleum Alternat Dev<Rapad> | 重質油の処理方法 |
JP3502221B2 (ja) * | 1995-05-25 | 2004-03-02 | 旭化成株式会社 | 硫化鉄及びその製造方法 |
JP3875001B2 (ja) * | 1999-07-21 | 2007-01-31 | 株式会社神戸製鋼所 | 石油系重質油の水素化分解方法 |
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BR102012005501A2 (pt) | 2014-05-13 |
BR102012005501B1 (pt) | 2019-01-08 |
JP2012193314A (ja) | 2012-10-11 |
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