JP2012506483A - 合成ガスを浄化するためのプロセス - Google Patents
合成ガスを浄化するためのプロセス Download PDFInfo
- Publication number
- JP2012506483A JP2012506483A JP2011533321A JP2011533321A JP2012506483A JP 2012506483 A JP2012506483 A JP 2012506483A JP 2011533321 A JP2011533321 A JP 2011533321A JP 2011533321 A JP2011533321 A JP 2011533321A JP 2012506483 A JP2012506483 A JP 2012506483A
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- JP
- Japan
- Prior art keywords
- synthesis gas
- adsorbent
- sulfur
- metal
- calcium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 118
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 65
- 230000008569 process Effects 0.000 title claims abstract description 59
- 239000003463 adsorbent Substances 0.000 claims abstract description 114
- 229910052751 metal Inorganic materials 0.000 claims abstract description 89
- 239000002184 metal Substances 0.000 claims abstract description 89
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 63
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 53
- 239000011593 sulfur Substances 0.000 claims abstract description 53
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- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 11
- -1 particulates Chemical class 0.000 claims abstract description 8
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- 150000003624 transition metals Chemical class 0.000 claims abstract description 3
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 66
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 37
- 229910052791 calcium Inorganic materials 0.000 claims description 36
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- 150000002739 metals Chemical class 0.000 claims description 26
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 24
- 239000002028 Biomass Substances 0.000 claims description 22
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- 150000003839 salts Chemical class 0.000 claims description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 7
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 5
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- 241000195493 Cryptophyta Species 0.000 claims description 3
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims description 3
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- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 2
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- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
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- 239000000460 chlorine Substances 0.000 claims description 2
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- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims 2
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- 239000004571 lime Substances 0.000 claims 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims 2
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C27/00—Processes involving the simultaneous production of more than one class of oxygen-containing compounds
- C07C27/26—Purification; Separation; Stabilisation
- C07C27/28—Purification; Separation; Stabilisation by distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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Abstract
Description
本出願は、2008年10月22日に出願された米国特許仮出願第61/107,478号からの優先権の利益を主張し、参照によりその全体が本明細書に組み込まれる。
開示されるプロセスは、任意の互換容器または本明細書で上述される要素を含む任意の装置において使用するために適合され得る。例えば、既存の石炭またはバイオマスガス化装置を使用することができるか、または1つ以上の装置を並行または連続して配置し、生成された合成ガスの浄化、すなわち、石炭のガス化、または既存の生合成ガスの源の精製または再精製をもたらし得る。
a)合成ガスを1つ以上の吸着剤と接触させて、金属、硫黄、およびハロゲン化物を捕獲することであって、接触は、触媒キャンドルフィルタの上流で行われて浄化合成ガスを形成すること、および
b)浄化合成ガスに混合分割分解触媒を含有するキャンドルフィルタを通過させ、アンモニアおよびタールを除去し、それによって精製合成ガスを生成すること、を含む。
a)合成ガスを1つ以上の吸着剤と接触させて、金属、硫黄、およびハロゲン化物を、触媒キャンドルフィルタの上流で捕獲すること、および
b)合成ガスにタールを分解する混合触媒を含有する触媒キャンドルフィルタを通過させて、精製合成ガスを形成すること、を含み、
工程(b)における触媒は、水性ガスシフト反応を促進し、それによって、精製合成ガス中に存在する水素ガス対一酸化炭素ガスの比率を調整する。
a)生合成ガスの源を、
i)カオリン粘土またはカオリン含有金属、
ii)カルシウム系吸着剤、
から選択される1つ以上の吸着剤と接触させ、それによって金属および硫黄汚染物質を除去して、浄化合成ガスを形成すること、
b)工程(a)で形成された浄化合成ガスに触媒フィルタ要素を通過させ、それによって、固体粒子および灰を除去することであって、さらなるタールが分解され、触媒フィルタ要素は、希土類金属酸化物または塩、遷移金属酸化物または塩、もしくはそれらの組み合わせを含み、それによって精製合成ガスを形成すること、を含む。
a)流動層石炭またはバイオマスガス化装置において精製される生合成ガスの源を、
i)カオリン粘土またはカオリナイト含有物質、
ii)カルシウム系吸着剤、
を含む吸着剤混合物と接触させ、それによって金属および硫黄汚染物質を除去して、浄化合成ガスを形成すること、
b)工程(a)において形成される合成ガスに、触媒分解フィルタ要素を通過させ、それによって、固体粒子および灰を除去し、タールおよび他の炭化水素構成要素を分解することであって、分解フィルタは、希土類金属酸化物または塩、遷移金属酸化物または塩、もしくはそれらの組み合わせを含み、それによって精製合成ガスを形成すること、を含む。
さらに、吸着剤の量は、吸着剤の摂取に起因して、プロセス中に異なり得るか、または吸着剤の量は、合成ガス原料の含有量における任意の変化、例えば、異なる合成ガス原料の源が使用される場合の硫黄含有レベルの変化を補償するように調整され得る。
6NO+4NH3→5N2+6H2O 等式1
本プロセスにおいて、アンモニアガスをガス流に注入して酸化窒素、すなわち、汚染物質として存在するNOx種を除去する代わりに、酸化窒素を生ガス流に注入して、汚染アンモニアを除去する。この反応が使用される場合、流動層ガス化装置を出る処理した合成ガスは、それが隣接する容器に進入する前に冷却されなければならず、NOとNH3との触媒反応が生じる。この反応に必要な温度範囲は、300〜450℃の範囲内である。酸化窒素添加の1つの短所は、酸化窒素が、ガス化装置、例えば、石炭またはバイオマスガス化装置において生成される、合成ガス中に存在する一酸化炭素と反応し得るという事実である。この望ましくない反応は、以下の等式2において概説される。
2NO+2CO→N2+2CO2 等式2
したがって、さらなる態様において、本開示は、合成ガスを浄化するためのプロセスに関し、
a)生合成ガスを、
i)カオリン粘土またはカオリン含有物質、非晶質アルミノケイ酸塩、アルミン酸塩、およびケイ酸塩、ならびに鉛、カドミウム、ヒ素およびセレニウム、ナトリウム、およびカリウム等の微量金属を捕獲するカルシウム系吸着剤、
ii)H2S、COS、およびCS2等の硫黄含有種を捕獲するカルシウム系吸着剤、および
iii)塩素、臭素、フッ素、ヨウ素、塩化水素、臭化水素、フッ化水素、およびヨウ化水素から選択される、ハロゲン化物含有汚染物質を捕獲するカルシウム系またはマグネシウム系吸着剤、ならびに
iv)i)〜(iii)に列挙される前記汚染物質のうちの1つより多くを除去することができる吸着剤、
から選択される吸着剤の混合物と、約700℃以上の高温で接触させ、それによって、吸着剤粒子上に、金属、硫黄種、およびハロゲン化物から選択される1つ以上の汚染物質を捕獲することであって、吸着剤粒子は、浄化合成ガスを形成するように、下流フィルタにおいて捕獲されること、
b)工程(a)において形成された浄化合成ガスに、触媒分解フィルタ要素を通過させ、それによって吸着剤粒子および灰を除去し、タールおよび他の炭化水素成分を分解することであって、分解フィルタは、希土類金属酸化物または塩、遷移金属酸化物または塩、あるいはそれらの組み合わせを含み、それによって硫黄非含有、無金属の分解合成ガスを形成すること、
c)前記硫黄非含有、無金属の分解合成ガスに、冷却ゾーンを通過させることであって、前記合成ガスは、少なくとも370℃の温度に冷却され、冷却された硫黄非含有、無金属の分解合成ガスを形成すること、
d)前記冷却された硫黄非含有、無金属の分解合成ガスに、酸化窒素の源を含む容器を通過させることであって、前記酸化窒素は、前記硫黄非含有、無金属の分解合成ガス中に存在するアンモニア汚染物質と反応して、精製合成ガスを生成することと、を含む。
実施例1
内径3.5cm、加熱領域の長さ114cm、および触媒層の深さ60cmの反応管の場合は、シミュレート合成ガスにより処理される。シミュレート合成ガスは、40,000ppm(4重量%)のアンモニアを含有する窒素ガスを含んでいた。シミュレートガスを、10L/分の流速で反応管に注入したところ、触媒層におけるガス残留時間は約3.5秒であった。触媒層のすぐ先に酸化窒素をシミュレート合成ガス流に注入した。加熱領域の温度は、約260℃〜約450℃まで変化した。試験は、大気圧で行った。本システムは、約3,000ppmのNH3の生成を約16barのガス化圧でシミュレートした。これらの実験の結果を表Iに示す。
本明細書で説明されるように、酸化窒素は、合成ガスの一酸化炭素との望ましくない副反応において反応して、窒素ガスおよび二酸化炭素を形成し得る。本プロセスは、この副反応が排除されるか、または有意に減少される条件下で行われる。一酸化炭素および水素ガスを、実施例1から得たシミュレート合成ガス流に添加した。370℃以下の温度で、酸化窒素による一酸化炭素の消費は、顕著でなくなった。260℃において、シミュレート合成ガス流において減少したアンモニアの量は、約40,000ppm〜約560ppmになり、約2.5:1のNO:NH3モル比を使用して、98.6%減少した。約2:1のNO:NH3モル比において、84%のアンモニアの減少が達成された。
実施例3 試験は固定層反応器において行い、汚染金属を容易に添加するように、触媒フィルタ要素をシミュレートした。反応器は、改良された流動層触媒分解触媒を含有した。本実施例において、改良された酸化ルテニウム系物質を試験した。触媒の平均粒径は、70μmであった。温度は約425℃に維持した。合成ガスは、混入流石炭ガス化装置から220psigの圧力で反応器を通過し、様々な有機物の分解は、反応器を出入りするガスのフーリエ変換赤外(FTIR)分析によって評価した。60時間の連続合成ガス処理において、表2の結果が得られた。
以下の試験は、合成ガスから金属を捕獲する際、開示されるフィルタを損傷から保護する、すなわち、触媒の保護における、高温吸着剤の有効性を評価するために行った。輸送ガス化装置のろ過領域の上流における金属吸着剤の注入をシミュレートするために、試験は、約815℃の温度に維持された管炉内で行った。合成ガスは、混入流石炭ガス化装置から約220psigの圧力で、管炉内の管を通過し、管炉の出口において、焼結金属フィルタを通過した。反応器入口において、室を導入して、知られている量の金属を合成ガスに気化させた。微量金属の捕獲に使用される吸着剤を注入するために、管を反応器の中心線に沿って導入した。この管の末端を、反応器内の様々な位置に挿入して、フィルタに暴露する前に、合成ガスにおける吸着剤の共鳴時間を変えて、添加される金属の捕獲効率に対する共鳴時間および吸着剤の有効性を測定することができる。
Claims (22)
- 合成ガスを浄化するためのプロセスであって、
a)触媒キャンドルフィルタの上流で、合成ガスを1つ以上の吸着剤と接触させて、浄化合成ガスを形成すること、および、
b)前記浄化合成ガスに混合分解触媒を含有するキャンドルフィルタを通過させ、アンモニアおよびタールを除去し、それによって精製合成ガスを生成すること、を含む、プロセス。 - 合成ガスを浄化するためのプロセスであって、
a)合成ガスを1つ以上の触媒キャンドルフィルタの上流で1つ以上の吸着剤と接触させること、および、
b)前記合成ガスに、混合触媒を含有する前記触媒キャンドルフィルタを通過させ、それによってタールを分解して精製合成ガスを形成すること、を含み、
工程(b)における前記触媒は、水−ガス転化反応をさらに促進し、それによって前記精製合成ガス中に存在する水素ガス対一酸化炭素ガスの比率を調整する、プロセス。 - 合成ガスを浄化するためのプロセスであって、
a)生合成ガスを
i)カオリン粘土またはカオリン含有物質、非晶質アルミノケイ酸塩、アルミン酸塩、およびケイ酸塩、ならびに鉛、カドミウム、ヒ素およびセレニウム、ナトリウム、およびカリウム等の微量金属を捕獲するカルシウム系吸着剤、
ii)H2S、COS、およびCS2等の硫黄含有種を捕獲するカルシウム系吸着剤、および
iii)塩素、臭素、フッ素、ヨウ素、塩化水素、臭化水素、フッ化水素、およびヨウ化水素から選択される、ハロゲン化物含有汚染物質を捕獲するカルシウム系またはマグネシウム系吸着剤、ならびに
iv)(i)〜(iii)に列挙される前記汚染物質のうちの1つより多くを除去することができる吸着剤、
から選択される吸着剤の混合物と、約700℃以上の高温で接触させ、それによって、吸着剤粒子上に金属、硫黄種、およびハロゲン化物から選択される1つ以上の汚染物質を捕獲することであって、前記吸着剤粒子は、浄化合成ガスを形成するように、下流フィルタにおいて捕獲されること、
b)ステップ(a)において形成された前記浄化合成ガスに、触媒分解フィルタ要素を通過させ、それによって前記吸着剤粒子および灰を除去し、タールおよび他の炭化水素成分を分解することであって、前記分解フィルタは、希土類金属酸化物または塩、遷移金属酸化物または塩、あるいはそれらの組み合わせを含み、それによって硫黄非含有、無金属の分解合成ガスを形成すること、
c)前記硫黄非含有、無金属の分解合成ガスに、冷却ゾーンを通過させることであって、前記合成ガスは、少なくとも370℃の温度に冷却され、冷却された硫黄非含有、無金属の分解合成ガスを形成すること、
d)前記冷却された硫黄非含有、無金属の分解合成ガスに、酸化窒素の源を含む容器を通過させることであって、前記酸化窒素は、前記硫黄非含有、無金属の分解合成ガス中に存在するアンモニア汚染物質と反応して、精製合成ガスを生成すること、を含む、方法。 - 合成ガスを精製するための方法であって、
a)生合成ガスの源を
i)カオリン粘土またはカオリン含有金属、
ii)カルシウム系吸着剤、
から選択される1つ以上の吸着剤と接触させ、それによって、金属および硫黄汚染物質を除去して、浄化合成ガスを形成すること、
b)ステップ(a)で形成された前記浄化合成ガスに、触媒フィルタ要素を通過させて、それによって固体粒子および灰を除去することであって、さらにタールが分解され、前記触媒フィルタ要素は、希土類金属酸化物または塩、遷移金属酸化物または塩、あるいはそれらの組み合わせを含み、それによって精製合成ガスを形成すること、を含む、方法。 - 前記合成ガスの源は石炭である、請求項1〜4のいずれか一項に記載のプロセス。
- 前記合成ガスの源は、都市固形廃棄物またはスラッジ、スイッチグラス、森林ごみ、木質チップ、藻類、トウモロコシ茎葉、および稲わらから選択されるバイオマスである、請求項1〜4のいずれか一項に記載のプロセス。
- 前記金属吸着剤は、カオリン粘土、カオリン含有金属、カルシウム系吸着剤、またはそれらの混合物から選択される、請求項1〜6のいずれか一項に記載のプロセス。
- 前記硫黄吸着剤は、カルシウム系もしくはカルシウム含有物質、マグネシウム系吸着剤、またはアルカリ系吸着剤、あるいはそれらの混合物から選択される、請求項1〜7のいずれか一項に記載のプロセス。
- 前記ハロゲン吸着剤は、カルシウム系もしくはカルシウム含有物質、マグネシウム系吸着剤、またはアルカリ系吸着剤、あるいはそれらの混合物から選択される、請求項1〜8のいずれか一項に記載のプロセス。
- 前記硫黄吸着剤は、石灰、粉砕石灰、石灰石、または粉砕石灰石から選択される、請求項1〜4のいずれか一項に記載のプロセス。
- 前記硫黄吸着剤は、水酸化カルシウム、炭酸カルシウム、酸化カルシウム、ドロマイト、酸化マグネシウム、リサイクルパルプ、または紙くず材料から選択される、請求項1〜4のいずれか一項に記載のプロセス。
- 各汚染物質のための前記吸着剤は、同一の吸着剤であるか、または1つを超える汚染物質を吸着できる吸着剤の組み合わせである、請求項1〜4のいずれか一項に記載のプロセス。
- 前記硫黄吸着剤は、カルシウムを含み、添加される前記硫黄吸着剤の量は、カルシウムのモル数対硫黄のモル数が、約0.5:1〜約5:1になるようにする、請求項1〜4のいずれか一項に記載のプロセス。
- タール分解触媒は、前記合成ガスの前記触媒フィルタへの進入前に、前記合成ガス流に添加される、請求項1〜4のいずれか一項に記載のプロセス。
- ドロマイトまたは他の化合物から選択されるタール分解触媒は、前記合成ガスの前記触媒フィルタへの進入前に、前記合成ガスの中に注入される、請求項1〜4のいずれか一項に記載のプロセス。
- 前記触媒フィルタは、酸化ニッケル、酸化ニッケル、遷移金属、または希土類金属をドロマイト基質上に含む、請求項1〜4のいずれか一項に記載のプロセス。
- 前記触媒フィルタは、基質上に蒸着されるニッケル触媒を含み、Li、K、Ca、およびMgから選択される1つ以上のプロモータをさらに含む、請求項1〜4のいずれか一項に記載のプロセス。
- 前記プロセスは、石炭ガス化装置において行われる、請求項1〜17のいずれか一項に記載のプロセス。
- さらに酸化窒素の源が添加される、請求項1、2、または4のいずれか一項に記載のプロセス。
- 前記金属吸着剤は、前記合成ガスに分解触媒を通過させる前に、前記合成ガスに添加される、請求項1〜4のいずれか一項に記載のプロセス。
- 前記分解触媒は、希土類金属または遷移金属酸化物もしくは塩である、請求項1〜16のいずれか一項に記載のプロセス。
- 前記分解触媒は、プラチナ、パラジウム、イリジウム、オスミウム、ロジウム、ルテニウム、レニウム、ランタン、バナジウム、またはニッケル、あるいはそれらの混合物の酸化物または塩である、請求項1〜16のいずれか一項に記載のプロセス。
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Also Published As
Publication number | Publication date |
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EA022656B1 (ru) | 2016-02-29 |
EP2346802A4 (en) | 2012-11-21 |
WO2010048376A1 (en) | 2010-04-29 |
US20100096594A1 (en) | 2010-04-22 |
AU2009308404B2 (en) | 2015-01-22 |
EA201170600A1 (ru) | 2012-11-30 |
CN102256917A (zh) | 2011-11-23 |
BRPI0919624A2 (pt) | 2015-12-01 |
KR20110129849A (ko) | 2011-12-02 |
US8007688B2 (en) | 2011-08-30 |
EP2346802A1 (en) | 2011-07-27 |
CN102256917B (zh) | 2015-05-20 |
MX2011004326A (es) | 2011-07-28 |
AU2009308404A1 (en) | 2010-04-29 |
CA2741480A1 (en) | 2010-04-29 |
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