JP4660093B2 - 一酸化炭素水素添加用触媒の再生 - Google Patents
一酸化炭素水素添加用触媒の再生 Download PDFInfo
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- JP4660093B2 JP4660093B2 JP2003563715A JP2003563715A JP4660093B2 JP 4660093 B2 JP4660093 B2 JP 4660093B2 JP 2003563715 A JP2003563715 A JP 2003563715A JP 2003563715 A JP2003563715 A JP 2003563715A JP 4660093 B2 JP4660093 B2 JP 4660093B2
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- catalyst
- carbon monoxide
- reactor
- gas
- hydrogen
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- 239000003054 catalyst Substances 0.000 title claims description 223
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 37
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- 230000015572 biosynthetic process Effects 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
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Classifications
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/10—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using elemental hydrogen
-
- 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
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Description
・事件整理番号37227(表題:フィッシャー−トロプシュ触媒の強化(Fischer−Tropsch Catalyst Enhancement」)
・事件整理番号37228(表題:担持された触媒の再生(Supported Catalyst Regeneration))
・事件整理番号37229(表題:担持された触媒の活性化(Supported Catalyst Activation))
・事件整理番号39158(表題:担持された触媒の処理(Supported Catalyst Treatment))
・事件整理番号39773(表題:触媒の活性化(Catalyst Enhancement))
また、出願係属中の米国特許出願第09/628,047号(2000年8月1日出願)(表題:水性低温酸化を介してコバルト触媒水素添加活性を向上させる方法(process for Increasing Cobalt Catalyst Hydrogenation Activity Via Aqueous Low Temperature Oxidation))にも関連している。
R−(COOH)n
(式中、nは1〜3であり、Rは、ニトロ基、アミノ基、水酸基またはアルコキシル基のうち1種以上により置換されていてもよい、環状または脂肪族の飽和または非飽和部分を表す。)
を有するカルボン酸から誘導される塩と定義される。カルボン酸塩の具体的な例には、限定の意図なく、ギ酸塩、酢酸塩、クエン酸塩、コハク酸塩、マロン酸塩、プロピオン酸塩、酪酸塩、吉草酸塩、カプロン酸塩、グルタル酸塩、アジピン酸塩、乳酸塩、安息香酸塩、フタル酸塩、サリチル酸塩、アスコルビン酸塩、シュウ酸塩などが含まれる。好適な金属含有酸(meta−containing acids)の好適な例には、限定の意図なく、過レニウム酸、モリブデン酸およびタングステン酸が含まれる。金属錯体には、限定の意図なく、金属アセチルアセトネート、金属エチレンジアミン、金属ジエチレントリアミンなどが含まれる。
ワックス中のチタニア担体担持コバルト系触媒の塊83g(200日間を超えて運転中のフィッシャー−トロプシュ反応器から回収)をビーカーに入れ、トルエンで覆った。混合物を85〜90℃に加熱し、手動で撹拌した。加熱/撹拌中に、塊をバラバラに砕いた。5分後、トルエン/ワックス溶液をデカントして新たなトルエンを加え、この処理を更に二回繰返した。三回目のデカントの後、残ったトルエン/触媒スラリーをブフナーロートに移し、高温でろ過した。高温のトルエンをろ過ケーク上に3回注ぎ、ろ過ケークを減圧吸引した。ろ過ケークを、ロート上で減圧を掛けて乾燥して、非発火性触媒58.4gを得た。触媒は、その高い透磁率によって示されるように、相当量の還元コバルトを含んでいた。触媒は、小さな永久磁石によって容易に動かされた。第二の試料を、ロート上で乾燥した後、終夜空気乾燥するという更なる工程を加えた、同様の方法で調製した。その特性は同じであった。
参考例からの触媒を、実験室固定床反応器で試験した。触媒(2ml、2.80g)を石英希釈材(4ml、6.54g)と混合し、内径1cmの管状反応器に入れた。ガラスウール栓を用いて、触媒床をしかるべき場所に保持した。多点熱伝対を床に挿入して、温度を監視した。初期段階で375℃、19.7気圧、水素315sccmの条件で、触媒を2時間に亘って水素で還元した。アルゴン10sccmおよび水素260sccmの流れの下で、触媒を、19.7気圧で177℃に冷却した。冷却後、供給物組成をアルゴン12sccm、水素134sccmおよび一酸化炭素/二酸化炭素混合物94sccmに変更した。これは、H 2 56.0%、CO 2 11.6%、Ar4.9%およびCO27.5%(%はモル%として示される)の名目原料組成を示した。次いで反応器を、2.8℃/時間で199℃に加熱し、その温度で24時間保持した。その後、反応器を2.8℃/時間で213℃に加熱し、その温度で試験の残りの間保持した。この温度で、CO転化率は27.3%であり、メタン選択性は7.6%であった。これらの条件下で24時間後に、CO転化率は24.3%であり、メタン選択性は7.6%であった。メタン選択性は、転化された一酸化炭素中の炭素の一部としての、製造されたメタン中の炭素と定義される。
参考例からの触媒30gをセラミック皿におき、300℃で2時間空気中で焼成した。焼成触媒を、乾燥した暗灰色の粉末として回収した。試験例1に示された手順に従って、焼成触媒の触媒活性試験を行った。CO転化率は55.0%であり、メタン選択性は10.9%であった。これらの条件下で24時間後に、CO転化率は52.4%であり、メタン選択性は10.5%であった。この試験例では、失活触媒を空気焼成することによって触媒活性が回復されうることが示される。
窒素雰囲気下、硝酸コバルト6水和物37.03gを脱イオン水25mlに加え、合計体積50mlに希釈することによって、溶液を調製した。溶液を穏やかに加熱して、全ての固体を完全に溶解し、窒素雰囲気下で保存した。合計2.60gの硝酸コバルト溶液を、300℃で2時間焼成した試験例2からの脱ロウ触媒10gに加えた。発熱は起こらず、変色も観察されなかった。空気中で更に2時間後、試料を100℃で1時間乾燥し、次いで、300℃で2時間焼成した。暗灰色の粉末11.2gを回収した。
Claims (13)
- 一酸化炭素の接触水素添加に用いられる使用済みフィッシャー−トロプシュ金属触媒の再生方法であって、該フィッシャー−トロプシュ金属触媒としてコバルトを含み、
a)上記使用済みフィッシャー−トロプシュ金属触媒の炭化水素含有量を減少させる工程;
b)酸化剤含有雰囲気下で工程a)からの脱ロウされた触媒を焼成する工程;
c)コバルト化合物の溶液により工程b)からの焼成された触媒を含浸する工程;
d)酸化剤含有雰囲気下で工程c)からの含浸された触媒を焼成する工程;および
e)200〜600℃の温度で工程d)からの焼成された触媒を水素含有ガスにより還元して、活性フィッシャー−トロプシュ金属触媒を製造する工程
を含み、工程b)およびd)の酸化剤が、酸素、空気、オゾンおよび窒素酸化物よりなる群から選択される、ことを特徴とする再生方法。 - 工程a)は、
高温で水素含有ガスと接触させる工程、
溶剤または超臨界流体により処理する工程、
溶剤または超臨界流体により処理し、次いで高温で水素含有ガスと接触させる工程、
高温で酸素含有ガスまたはスチームと接触させ、次いで高温で水素含有ガスと接触させる工程、および
溶剤または超臨界流体により処理し、高温で酸素含有ガスまたはスチームと接触させ、次いで高温で水素含有ガスと接触させる工程
よりなる群から選択される一工程により実施されることを特徴とする請求項1に記載の再生方法。 - 工程c)の前記コバルト化合物は、硝酸塩、酢酸塩、ギ酸塩、クエン酸塩および炭酸塩よりなる群から選択されるコバルト塩であることを特徴とする請求項1に記載の再生方法。
- 工程c)で用いられる前記含浸溶液の量は、前記触媒の計算細孔体積の10〜5,000%であることを特徴とする請求項1に記載の再生方法。
- 工程e)の後に、
一酸化炭素が有意に分解されない条件下で、一酸化炭素含有ガスにより処理する工程、または
一酸化炭素が有意に水素添加されない条件下で、一酸化炭素および水素を含むガスにより処理する工程
によって不動態化する工程を更に含み、上記条件は、温度が150℃未満であり、圧力が20気圧未満であり、触媒の容積あたり、1時間あたりのガスまたはガス混合物の標準状態(25℃、1気圧)での容積で表されるガス空間速度が、1〜1,000V/Hr/Vである、ことを特徴とする請求項1に記載の再生方法。 - 粉末の分級もしくは篩い分けまたは触媒スラリーのデカンテーションによって、触媒細粒を除去する工程を更に含むことを特徴とする請求項1に記載の再生方法。
- 前記触媒は、担持触媒であることを特徴とする請求項1に記載の再生方法。
- 前記触媒は、分散活性金属(DAM)触媒であることを特徴とする請求項1に記載の再生方法。
- 前記工程a)〜e)は、単一の一酸化炭素水素添加反応器において行なわれることを特徴とする請求項1に記載の再生方法。
- 前記一酸化炭素水素添加反応器は、固定床反応器であることを特徴とする請求項9に記載の再生方法。
- 再生処理された前記触媒は、一酸化炭素の接触水素添加に再利用されることを特徴とする請求項1に記載の再生方法。
- 前記触媒は、固定床HCS反応器を用いる炭化水素合成プロセスに使用され、少なくとも脱ロウ工程を原反応器内で行なうことを特徴とする請求項1に記載の再生方法。
- スラリー反応器を用いて一酸化炭素の接触水素添加を行ない、反応器を製造中としたまま、触媒を連続的に抜き出して置き換えることを特徴とする請求項1に記載の再生方法。
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US10/059,926 US6800579B2 (en) | 2002-01-29 | 2002-01-29 | Catalyst regeneration |
PCT/US2003/000150 WO2003064034A2 (en) | 2002-01-29 | 2003-01-03 | Regeneration of catalysts for carbon monoxide hydrogenation |
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US7256149B2 (en) * | 2004-02-24 | 2007-08-14 | Lyondell Chemical Technology, L.P. | Catalyst regeneration process |
US7524787B2 (en) * | 2005-01-11 | 2009-04-28 | Sasol Technology (Proprietary Limited) | Producing supported cobalt catalysts for the Fisher-Tropsch synthesis |
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JP5169047B2 (ja) | 2007-07-23 | 2013-03-27 | 住友化学株式会社 | 塩素の製造方法 |
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WO2003064034A2 (en) | 2003-08-07 |
CN1750876B (zh) | 2011-05-04 |
AR038135A1 (es) | 2004-12-29 |
US20030144366A1 (en) | 2003-07-31 |
CA2470945A1 (en) | 2003-08-07 |
CA2470945C (en) | 2011-03-15 |
ZA200404715B (en) | 2006-02-22 |
AU2003202874B2 (en) | 2010-07-15 |
JP2005516055A (ja) | 2005-06-02 |
EP1472001A2 (en) | 2004-11-03 |
CN1750876A (zh) | 2006-03-22 |
WO2003064034A3 (en) | 2003-11-27 |
EP1472001B1 (en) | 2009-12-30 |
DE60330752D1 (de) | 2010-02-11 |
TWI266649B (en) | 2006-11-21 |
TW200302132A (en) | 2003-08-01 |
US6800579B2 (en) | 2004-10-05 |
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