JP5591910B2 - キャスタブル中の硫黄化合物の除去方法 - Google Patents
キャスタブル中の硫黄化合物の除去方法 Download PDFInfo
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- JP5591910B2 JP5591910B2 JP2012502991A JP2012502991A JP5591910B2 JP 5591910 B2 JP5591910 B2 JP 5591910B2 JP 2012502991 A JP2012502991 A JP 2012502991A JP 2012502991 A JP2012502991 A JP 2012502991A JP 5591910 B2 JP5591910 B2 JP 5591910B2
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- gas
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- sulfur compound
- synthesis gas
- carbon dioxide
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- 150000003464 sulfur compounds Chemical class 0.000 title claims description 67
- 238000000034 method Methods 0.000 title claims description 46
- 230000015572 biosynthetic process Effects 0.000 claims description 61
- 238000003786 synthesis reaction Methods 0.000 claims description 61
- 238000004519 manufacturing process Methods 0.000 claims description 33
- 238000002407 reforming Methods 0.000 claims description 27
- 239000003054 catalyst Substances 0.000 claims description 25
- 238000010926 purge Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims 1
- 238000009331 sowing Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 description 125
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 88
- 229910002092 carbon dioxide Inorganic materials 0.000 description 44
- 239000001569 carbon dioxide Substances 0.000 description 44
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 30
- 238000006057 reforming reaction Methods 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000003345 natural gas Substances 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000006477 desulfuration reaction Methods 0.000 description 10
- 230000023556 desulfurization Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 238000000629 steam reforming Methods 0.000 description 8
- 229910052717 sulfur Inorganic materials 0.000 description 8
- 150000001412 amines Chemical class 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 125000004434 sulfur atom Chemical group 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 4
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002918 waste heat Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 3
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 231100000572 poisoning Toxicity 0.000 description 3
- 230000000607 poisoning effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000003779 heat-resistant material Substances 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- -1 naphtha Chemical class 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/48—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents followed by reaction of water vapour with carbon monoxide
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
- C01B2203/0233—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a steam reforming step
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- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
- C01B2203/0238—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a carbon dioxide reforming step
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- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0283—Processes for making hydrogen or synthesis gas containing a CO-shift step, i.e. a water gas shift step
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- C01B2203/0415—Purification by absorption in liquids
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- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0455—Purification by non-catalytic desulfurisation
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- C01B2203/0465—Composition of the impurity
- C01B2203/0475—Composition of the impurity the impurity being carbon dioxide
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- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0485—Composition of the impurity the impurity being a sulfur compound
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- C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
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- C01B2203/148—Details of the flowsheet involving a recycle stream to the feed of the process for making hydrogen or synthesis gas
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Catalysts (AREA)
- Aftertreatments Of Artificial And Natural Stones (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Description
式(1): CH4 + H2O → CO + 3H2
式(2): CH4 + CO2 → 2CO + 2H2
式(4): R−NH2 + H2S → R−NH3 + + HS−
配管にパージガスを流通させ乾燥焚きすることでキャスタブルの硫黄化合物が除去されることを示すため、以下の実施例1を行った。
パージガスを貫流させたキャスタブルからは合成ガス中に硫黄化合物が混入しないことを確認するため、以下の実施例2をおこなった。
パージガスを流通させる際の加熱温度による硫黄化合物除去率の変化を調べるため、実施例1と同様の試験装置を用いて、充填層の温度以外は実施例1のスチーム/窒素混合ガスの場合と同一の条件にして硫黄化合物除去試験を実施した。その結果、充填層の温度を650℃、750℃に維持してスチーム/窒素混合ガスを48時間流したときのキャスタブル中の硫黄化合物除去率は、それぞれ80%、97%であった。
スチームを含まないパージガスでの硫黄化合物除去効率を確認するため、以下の比較例を行った。
実施例1と同様の試験装置を用いて、パージガスの組成を表4中に示すように変えたほかは実施例1と同一の条件にして硫黄化合物除去試験を実施し、キャスタブル31中に残存している硫黄化合物濃度及び硫黄化合物除去率を求めた(図3)。
実施例2と同様に比較例4による硫黄化合物除去試験後のキャスタブル41(15cc)を触媒層後段に設置して改質反応試験を実施し、生成合成ガス49中への硫黄化合物の流出をSCD−GC分析により確認した(図4)。なお、キャスタブルの充填量は15ccとした。表5の結果が示すように、反応開始直後から生成ガス中への硫黄化合物の脱離が確認され、以後連続的に発生した。スチームを用いない加熱前処理では硫黄化合物の除去は不充分であることが確認された。
12 アルミナビーズ層
13 アルミナビーズ層
14 SUS反応管
15 冷却器
16 凝縮水
17 窒素ガス
21 キャスタブル
24 SUS反応管
28 リフォーミング触媒
29 合成ガス
31 キャスタブル
41 キャスタブル
49 合成ガス
Claims (5)
- 反応器及び配管の内表面に耐熱部材として施工されたキャスタブルにスチーム又はスチーム含有ガスからなるパージガスを流通させて乾燥焚きを行うことを特徴とする、キャスタブル中の硫黄化合物の除去方法。
- 前記配管が合成ガス製造装置に使用され、前記乾燥焚きを合成ガス製造装置の稼動前に行うことを特徴とする、請求項1に記載のキャスタブル中の硫黄化合物の除去方法。
- 前記乾燥焚きを合成ガス製造用装置に改質触媒を充填する前に行うことを特徴とする、請求項2に記載のキャスタブル中の硫黄化合物の除去方法。
- 前記乾燥焚きの温度は750〜900℃であることを特徴とする、請求項1〜3の何れか1項に記載のキャスタブル中の硫黄化合物の除去方法。
- 前記乾燥焚きは48時間以上行うことを特徴とする、請求項4に記載のキャスタブル中の硫黄化合物の除去方法。
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JP2012502991A JP5591910B2 (ja) | 2010-03-02 | 2011-02-21 | キャスタブル中の硫黄化合物の除去方法 |
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JP2010045698 | 2010-03-02 | ||
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JP2012502991A JP5591910B2 (ja) | 2010-03-02 | 2011-02-21 | キャスタブル中の硫黄化合物の除去方法 |
PCT/JP2011/000935 WO2011108213A1 (ja) | 2010-03-02 | 2011-02-21 | キャスタブル中の硫黄化合物の除去方法 |
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JPWO2011108213A1 JPWO2011108213A1 (ja) | 2013-06-20 |
JP5591910B2 true JP5591910B2 (ja) | 2014-09-17 |
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Country Status (11)
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US (1) | US8832967B2 (ja) |
EP (1) | EP2543431A4 (ja) |
JP (1) | JP5591910B2 (ja) |
CN (1) | CN102781565B (ja) |
AU (1) | AU2011222348B2 (ja) |
BR (1) | BR112012021914B8 (ja) |
CA (1) | CA2791861C (ja) |
EA (1) | EA019981B1 (ja) |
MY (1) | MY160346A (ja) |
WO (1) | WO2011108213A1 (ja) |
ZA (1) | ZA201206247B (ja) |
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DE102011107669B4 (de) * | 2011-07-12 | 2022-02-10 | Eberspächer Climate Control Systems GmbH & Co. KG | Kraftstoffbehandlungsvorrichtung |
US10046371B2 (en) * | 2013-03-29 | 2018-08-14 | Semes Co., Ltd. | Recycling unit, substrate treating apparatus and recycling method using the recycling unit |
US10131593B2 (en) * | 2013-08-06 | 2018-11-20 | Chiyoda Corporation | Systems and methods for producing hydrogen from a hydrocarbon and using the produced hydrogen in a hydrogenation reaction |
Citations (4)
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JP2000329323A (ja) * | 1999-03-12 | 2000-11-30 | Ube Ind Ltd | 廃棄物ガス化処理装置における高温ガス化炉構造 |
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JP2005089230A (ja) * | 2003-09-17 | 2005-04-07 | Denki Kagaku Kogyo Kk | アルミナセメント組成物及びそれを用いた不定形耐火物 |
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US2730437A (en) * | 1951-04-07 | 1956-01-10 | Raymond B Coombe | Automatic control for gas making machines |
US2721122A (en) * | 1952-09-24 | 1955-10-18 | Inst Gas Technology | Thermal method of making oil gas |
US2893853A (en) * | 1956-07-12 | 1959-07-07 | United Gas Improvement Co | Method for catalytic conversion hydrocarbons |
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CN102781565A (zh) | 2012-11-14 |
BR112012021914B1 (pt) | 2019-04-02 |
EP2543431A1 (en) | 2013-01-09 |
US20120317833A1 (en) | 2012-12-20 |
WO2011108213A1 (ja) | 2011-09-09 |
JPWO2011108213A1 (ja) | 2013-06-20 |
EA019981B1 (ru) | 2014-07-30 |
CA2791861A1 (en) | 2011-09-09 |
US8832967B2 (en) | 2014-09-16 |
CA2791861C (en) | 2016-09-06 |
EA201290736A1 (ru) | 2013-02-28 |
EP2543431A4 (en) | 2014-01-15 |
CN102781565B (zh) | 2016-04-27 |
AU2011222348B2 (en) | 2013-11-07 |
BR112012021914A2 (pt) | 2016-05-31 |
AU2011222348A1 (en) | 2012-09-20 |
BR112012021914B8 (pt) | 2019-10-01 |
MY160346A (en) | 2017-02-28 |
ZA201206247B (en) | 2013-05-29 |
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