JP2008514420A - 貴金属触媒のエクス−シチュでの還元および乾式不動態化 - Google Patents
貴金属触媒のエクス−シチュでの還元および乾式不動態化 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 102
- 238000011066 ex-situ storage Methods 0.000 title claims abstract description 22
- 230000009467 reduction Effects 0.000 title claims description 21
- 238000002161 passivation Methods 0.000 title description 16
- 239000010970 precious metal Substances 0.000 title description 10
- 238000000034 method Methods 0.000 claims abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 239000011148 porous material Substances 0.000 claims abstract description 23
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 22
- 238000011049 filling Methods 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011593 sulfur Substances 0.000 claims abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 25
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical group [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 229910052763 palladium Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 239000010690 paraffinic oil Substances 0.000 claims 1
- 230000003213 activating effect Effects 0.000 abstract description 2
- 239000003570 air Substances 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- 238000011065 in-situ storage Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000011261 inert gas Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910003445 palladium oxide Inorganic materials 0.000 description 2
- 229910003446 platinum oxide Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- KSSJBGNOJJETTC-UHFFFAOYSA-N COC1=C(C=CC=C1)N(C1=CC=2C3(C4=CC(=CC=C4C=2C=C1)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC(=CC=C1C=1C=CC(=CC=13)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC=C(C=C1)OC Chemical compound COC1=C(C=CC=C1)N(C1=CC=2C3(C4=CC(=CC=C4C=2C=C1)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC(=CC=C1C=1C=CC(=CC=13)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC=C(C=C1)OC KSSJBGNOJJETTC-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- NOWPEMKUZKNSGG-UHFFFAOYSA-N azane;platinum(2+) Chemical compound N.N.N.N.[Pt+2] NOWPEMKUZKNSGG-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0325—Noble metals
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Abstract
【選択図】なし
Description
触媒は、アルミナ結合MCM−41に担持された0.3重量%の白金および0.9重量%のパラジウムを含む。白金およびパラジウムは、硝酸テトラアミン白金およびパラジウムの水溶液を触媒担体にまず吸収させることによって、担体表面に高度に分散される。金属をコーティング後、担体を乾燥させ、その後、空気中でか焼してテトラアミンを分解すると、細かく分散した白金およびパラジウムの酸化物が生成する。使用前に、金属の分散を損なうことなく、白金およびパラジウムの酸化物を還元することによって、触媒を活性化しなければならない。
エクス−シチュ還元では、担持された貴金属酸化物をまず乾燥させ、ロータリーか焼器中で水素と不活性ガスの混合ガスの存在下に一段で還元する。表2に示すように、ロータリーか焼器でエクス−シチュ還元の後、窒素でシールした試料上への酸素の化学吸着結果は、触媒が、貴金属の凝集もなく、完全に還元されたことを示している。
実施例2で得られた還元および不動態化された触媒試料をパイロットプラント反応器に充填し、各触媒の、水素化処理した600N脱ろうオイルの水素仕上げに対する性能評価を行った。脱ろうオイルは、予め水素化処理して、硫黄含有量を約200重量ppmにまで低減させた。
下記の例は、実施例2の2つの乾式不動態化触媒、即ち、還元貴金属を保護するための空気およびオイル細孔充填により不動態化した触媒の、より厳しい開始条件下での性能を比較するものである。還元金属の不動態化に加えて、オイル細孔充填技術もまた、触媒の貯蔵中および取り扱い中の触媒による吸湿を最小限に抑え、従って、立ち上がり時の水の生成を減少させ、更に、金属のシンタリングのリスクを低減する。
酸化物触媒の湿性ガス処理は、空気およびオイル不動態化触媒が比較される基本のケースであった。酸化物の状態の貴金属触媒を、乾燥工程(140℃)、および、約2.2psiaの水蒸気分圧の湿性ガスを用いる還元工程(220℃)に供した。これまでの研究は、これらの還元条件では金属のシンタリングが生じ、性能の低い触媒が生成されることを示している。
空気およびオイル細孔充填の還元および不動態化触媒の全てを湿性ガス処理に供した。2つの反応器に空気不動態化触媒を充填した。1つの触媒は2時間の乾燥工程(140℃)と、約1psiaの水蒸気分圧を有する湿性ガスで16時間の還元工程(140℃)に供した。第2の空気不動態化触媒は、乾燥工程を省略して、直接、湿性水素により140℃で16時間の還元を行った。
図3および図4は、湿性窒素および湿性水素で処理した場合に、空気不動態化触媒の性能がより低いことを示している。この触媒の活性が、乾燥し、そして乾性ガスで還元した触媒の活性に比べてかなり低いことは明らかである。
Claims (13)
- 細孔を有する担持金属触媒を、エクス−シチュで還元および乾式不動態化する方法であって、
(a)前記触媒を還元する工程;および
(b)前記触媒の乾燥および易流動性が保持されるように、前記触媒を不動態化する工程
を含むことを特徴とする方法。 - 前記還元工程は、水素の存在下に行われることを特徴とする請求項1に記載の方法。
- 前記触媒を不動態化する前記工程は、不活性雰囲気中で冷却する工程を含むことを特徴とする請求項1に記載の方法。
- 前記不活性雰囲気は、窒素であることを特徴とする請求項3に記載の方法。
- 前記触媒を不動態化する前記工程は、前記細孔を満たす工程を含むことを特徴とする請求項3に記載の方法。
- 前記細孔は、オイルで満たされることを特徴とする請求項5に記載の方法。
- 前記オイルは、ホワイトオイルであることを特徴とする請求項6に記載の方法。
- 前記オイルは、パラフィン系オイルであることを特徴とする請求項6に記載の方法。
- 前記細孔は、低硫黄留出物で満たされることを特徴とする請求項5に記載の方法。
- 前記細孔は、空気で満たされることを特徴とする請求項5に記載の方法。
- 前記金属触媒は、貴金属触媒であることを特徴とする請求項1に記載の方法。
- 前記触媒は、MCM−41に担持されたパラジウムおよび白金であることを特徴とする請求項1に記載の方法。
- 前記触媒を不動態化する前記工程は、
不活性雰囲気中で冷却する工程;および
空気に曝露する工程
を含むことを特徴とする請求項1に記載の方法。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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US61501604P | 2004-10-01 | 2004-10-01 | |
US60/615,016 | 2004-10-01 | ||
US11/228,366 | 2005-09-16 | ||
US11/228,366 US7407909B2 (en) | 2004-10-01 | 2005-09-16 | Ex-situ reduction and dry passivation of noble metal catalysts |
PCT/US2005/034752 WO2006039316A2 (en) | 2004-10-01 | 2005-09-27 | Ex-situ reduction and dry passivation of noble metal catalysts |
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JP2008514420A true JP2008514420A (ja) | 2008-05-08 |
JP2008514420A5 JP2008514420A5 (ja) | 2008-10-30 |
JP5134958B2 JP5134958B2 (ja) | 2013-01-30 |
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JP2007534722A Active JP5134958B2 (ja) | 2004-10-01 | 2005-09-27 | 貴金属触媒のエクス−シチュでの還元および乾式不動態化 |
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US (1) | US7407909B2 (ja) |
EP (1) | EP1814664A4 (ja) |
JP (1) | JP5134958B2 (ja) |
KR (1) | KR101192455B1 (ja) |
CA (1) | CA2581187C (ja) |
RU (1) | RU2376060C2 (ja) |
WO (1) | WO2006039316A2 (ja) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2017513707A (ja) * | 2014-04-30 | 2017-06-01 | エクソンモービル・ケミカル・パテンツ・インク | 金属含浸触媒性能を改善する方法 |
KR20210106559A (ko) * | 2019-01-25 | 2021-08-30 | 엑손모빌 케미칼 패턴츠 인코포레이티드 | 저 금속 함량 촉매의 활성화 |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2850882B1 (fr) * | 2003-02-11 | 2005-03-18 | Eurecat Sa | Passivation de catalyseur d'hydroconversion sulfure |
KR101274995B1 (ko) * | 2006-08-31 | 2013-06-14 | 재단법인 포항산업과학연구원 | 고활성 다이옥신 분해용 슬러리형 Pd/C 촉매, 그제조방법 및 이를 이용한 다이옥신 분해 방법 |
WO2015050635A1 (en) | 2013-10-03 | 2015-04-09 | Exxonmobil Chemical Patents Inc. | Hydrocarbon raffinate stream processing |
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JP5134958B2 (ja) | 2013-01-30 |
WO2006039316A3 (en) | 2006-09-08 |
US20060073965A1 (en) | 2006-04-06 |
RU2007114109A (ru) | 2008-11-10 |
KR20070063572A (ko) | 2007-06-19 |
RU2376060C2 (ru) | 2009-12-20 |
WO2006039316A2 (en) | 2006-04-13 |
CA2581187A1 (en) | 2006-04-13 |
US7407909B2 (en) | 2008-08-05 |
KR101192455B1 (ko) | 2012-10-17 |
EP1814664A4 (en) | 2011-05-11 |
CA2581187C (en) | 2012-08-07 |
EP1814664A2 (en) | 2007-08-08 |
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