JP2005087900A - 熱的劣化触媒の再生方法 - Google Patents
熱的劣化触媒の再生方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 134
- 238000011069 regeneration method Methods 0.000 title abstract description 28
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 68
- 239000007864 aqueous solution Substances 0.000 claims abstract description 41
- 230000000694 effects Effects 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 230000007774 longterm Effects 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 34
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 32
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 32
- 238000010828 elution Methods 0.000 claims description 23
- 229910052785 arsenic Inorganic materials 0.000 claims description 15
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 15
- 230000001172 regenerating effect Effects 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000011260 aqueous acid Substances 0.000 claims description 5
- 239000002912 waste gas Substances 0.000 claims description 4
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- 238000010306 acid treatment Methods 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 abstract description 23
- 238000004140 cleaning Methods 0.000 description 19
- 230000006866 deterioration Effects 0.000 description 18
- 239000011575 calcium Substances 0.000 description 15
- 229910052791 calcium Inorganic materials 0.000 description 14
- 230000015556 catabolic process Effects 0.000 description 14
- 238000006731 degradation reaction Methods 0.000 description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 14
- 229910052721 tungsten Inorganic materials 0.000 description 14
- 239000010937 tungsten Substances 0.000 description 14
- 229910052700 potassium Inorganic materials 0.000 description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- 229910052720 vanadium Inorganic materials 0.000 description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 8
- 239000011591 potassium Substances 0.000 description 8
- 230000006835 compression Effects 0.000 description 7
- 238000007906 compression Methods 0.000 description 7
- 239000013543 active substance Substances 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000004220 aggregation Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 231100000572 poisoning Toxicity 0.000 description 4
- 230000000607 poisoning effect Effects 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 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 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 229910000413 arsenic oxide Inorganic materials 0.000 description 2
- 229960002594 arsenic trioxide Drugs 0.000 description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000001495 arsenic compounds Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
-
- 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
- B01D53/96—Regeneration, reactivation or recycling of reactants
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/92—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B01J38/00—Regeneration or reactivation of catalysts, in general
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- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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- B01J38/00—Regeneration or reactivation of catalysts, in general
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- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/68—Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst
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Abstract
【効果】 従来不可能とされていた熱的劣化触媒の再生が可能となった。また、これらの酸水溶液やアルカリ水溶液による洗浄は、触媒の機械的強度に影響を与えることもない。
【選択図】 なし
Description
セラミクスペーパー(厚さ:公称0.3mm)に75g/m2のアナターゼTiO2微粉を分散保持させた板状の担体前駆物(比表面積105m2/g)(以下、担体前駆物という)を580℃で時間を変化させて焼成し、比表面積の異なる担体を調製した。この担体を0.03モル/リッターのメタバナジン酸アンモニウム(NH4VO3)水溶液に30分浸漬し、乾燥・焼成し、バナジウム酸化物を吸着担持させた。次いでこれを15重量%のWO3水溶液に30分浸漬し、乾燥・焼成し、脱硝触媒を調製した。この触媒の脱硝性能を計測した。この結果を図1に示す。図1から分かるように、担体の比表面積が60m2/g以上であれば、脱硝性能はほぼ一定である。
上記(1) 熱的劣化の項に示した熱的劣化触媒を各種の洗浄液に5時間浸漬して、活性物質であるバナジウム酸化物およびタングステン酸化物の溶出性を観察した。この結果を図2に示す。また、洗浄液水素イオン濃度(pH)と溶出性の関係を図3に示す。
上記(1) 熱的劣化の項に示した熱的劣化触媒をpH1.2の硝酸水溶液に5時間浸漬してバナジウム酸化物を溶出除去した後、再び同様の条件でバナジウム酸化物を担持して再生触媒を調製し、性能を比較した。この結果を図4に示す。初期性能にほぼ等しい性能が得られた。
上記(3)熱劣化触媒の再生の項に示した触媒再生前後における圧縮強度比を表1に示す。表1から、触媒再生により圧縮強度の低下が認められないことがわかる。表1中、圧縮強度比=再生後の圧縮強度/再生前の圧縮強度。
実プラントにおける熱的劣化触媒(チタニア比表面積:40g/m2)をpH1.2の硝酸水溶液に5時間浸漬してバナジウムを溶出除去し、バナジウムを再担持した。この触媒を触媒1とする。実プラントにおける熱的劣化触媒(チタニア比表面積:40g/m2)をpH10.5のNH3水溶液に5時間浸漬してバナジウム酸化物およびタングステンを溶出除去し、チタニアを担持し、その後バナジウム酸化物およびタングステンを再担持した。この触媒を触媒2とする。触媒1と触媒2の性能を比較した。この結果を図5に示す。図5より、バナジウム酸化物の凝集に合わせて担体であるチタニアの凝集も同時に起こり、活性低下した触媒は、バナジウム酸化物およびタングステンを溶出除去しチタニアを担持した後でバナジウム酸化物およびタングステンを再担持することでほぼ初期性能まで回復できることがわかる。
セラミクスペーパー(厚さ:公称0.3mm)に75g/m2のアナターゼTiO2微粉を分散保持させた板状の担体前駆物(比表面積105m2/g)を500℃で1時間焼成し、担体を調製した。この担体を0.03モル/リッターのメタバナジン酸アンモニウム(NH4VO3)水溶液に30分浸漬し、乾燥・焼成し、バナジウム酸化物を吸着担持させた。次いでこれを15重量%のWO3水溶液に30分浸漬し、乾燥・焼成し、脱硝触媒を調製した。
板状担体に上記と同様の条件でバナジウム酸化物およびタングステン化合物を担持して標準脱硝触媒を得た。
長期間石炭焚き排ガス脱硝に使用して性能が低下した触媒について活性の測定を行い、次にこの触媒をpH1.4の硝酸水溶液に5時間浸漬し、次いでpH10.5のNH3水溶液に5時間浸漬した後、再び同様の条件でバナジウム酸化物およびタングステン酸化物を担持して劣化触媒を再生し、性能の回復性を測定した。この結果を図10に示す。
実施例2の(3)実劣化触媒の再生の項において酸、アルカリによる洗浄順序を逆にしたこと以外は、実施例2の(3)と同様の方法で再生を行った。
Claims (8)
- 還元剤としてアンモニアを用いて廃ガス中のNOxを還元除去する方法に使用される触媒であって、高温で長期使用により活性成分であるバナジウム酸化物が凝集し、活性低下した触媒を、pH6以下の酸水溶液で洗浄することにより、主として、凝集した活性成分であるバナジウム酸化物を溶出除去し、ついで活性成分であるバナジウム酸化物を再担持することを特徴とする熱的劣化触媒の再生方法。
- 酸として硝酸または塩酸を用いることを特徴とする請求項1記載の熱的劣化触媒の再生方法。
- 還元剤としてアンモニアを用いて廃ガス中のNOxを還元除去する方法に使用される触媒であって、高温で長期使用により活性成分であるバナジウム酸化物が凝集し、活性低下した触媒を、pH8以上のアルカリ水溶液で洗浄することにより、主として、活性成分であるバナジウム酸化物およびタングステン酸化物を溶出除去し、その後、担体成分であるチタン酸化物を再担持し、ついで活性成分であるバナジウム酸化物およびタングステン酸化物を再担持することを特徴とする熱的劣化触媒の再生方法。
- アルカリとしてアンモニア水を用いることを特徴とする請求項3記載の熱的劣化触媒の再生方法。
- 還元剤としてアンモニアを用いて石炭焚き排ガス中のNOxを還元除去する方法に使用される触媒であって、活性の低下した触媒をpH4以下の酸水溶液で洗浄することにより、主として、劣化成分であるアルカリ金属、アルカリ土類金属、砒素、イオウを溶出除去した後、pH8以上のアルカリ水溶液で触媒を洗浄することにより、主として、活性成分であるバナジウム酸化物およびタングステン酸化物を溶出除去し、ついで活性成分であるバナジウム酸化物およびタングステン酸化物を再担持・焼成することを特徴とする劣化触媒の再生方法。
- 酸処理、アルカリ処理、活性成分再担持処理の間に水洗処理を加えることを特徴とする請求項5記載の劣化触媒の再生方法。
- 酸として硝酸または塩酸を用いることを特徴とする請求項5記載の熱的劣化触媒の再生方法。
- アルカリとしてアンモニアを用いることを特徴とする請求項5記載の熱的劣化触媒の再生方法。
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Application Number | Priority Date | Filing Date | Title |
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JP2003325665A JP4264642B2 (ja) | 2003-09-18 | 2003-09-18 | 熱的劣化触媒の再生方法 |
KR1020067005210A KR101096938B1 (ko) | 2003-09-18 | 2004-09-21 | 열적 열화 촉매의 재생 방법 |
PCT/JP2004/014131 WO2005028102A1 (ja) | 2003-09-18 | 2004-09-21 | 熱的劣化触媒の再生方法 |
US10/572,310 US20080248943A1 (en) | 2003-09-18 | 2004-09-21 | Method of Regenerating Thermally Deteriorated Catalyst |
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ITMI20070105A1 (it) * | 2007-01-24 | 2008-07-25 | Acetilene & Derivati S I A D | Processo per la attivazione, rigenerazione e/o recupero di catalizzatori foto attivati, impiegati per il trattamento di effluenti liquidi, gas o miscele gassose, per il rivestimento di materiali e per processi di sintesi |
JP5723646B2 (ja) * | 2011-03-25 | 2015-05-27 | 日立造船株式会社 | 脱硝触媒の調製方法 |
WO2012150816A2 (ko) * | 2011-05-02 | 2012-11-08 | 한서대학교 산학협력단 | 중질유 수소화처리를 위한 재생 또는 재제조 촉매 및 그의 제조방법 |
EP2872489B1 (en) * | 2012-07-10 | 2016-12-21 | Siemens Healthcare Diagnostics Inc. | Synthesis of acridinium compounds by n-alkylation of acridans |
KR102102044B1 (ko) * | 2018-08-20 | 2020-04-23 | 주식회사 세일에프에이 | 유해가스 제거용 촉매가 함유된 펠릿 조성물의 제조 및 이의 재활용 방법 |
KR102191455B1 (ko) * | 2019-04-09 | 2020-12-15 | 주식회사 세일에프에이 | 유해가스 제거용 촉매의 제조 및 재활용 방법 |
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DE2552456C3 (de) * | 1975-11-22 | 1978-05-18 | Bayer Ag, 5090 Leverkusen | Verfahren zum Regenerieren von verbrauchten, Vanadinoxyd enthaltenden Oxydationskatalysatoren |
JPS5410294A (en) * | 1977-06-27 | 1979-01-25 | Mitsubishi Chem Ind Ltd | Regenerating method for used vanadium-titania catalyst |
JPS6041611B2 (ja) * | 1979-12-19 | 1985-09-18 | 三菱重工業株式会社 | 触媒組成物の処理方法 |
JPS57180433A (en) * | 1981-04-28 | 1982-11-06 | Mitsubishi Heavy Ind Ltd | Regeneration of used denitration catalyst |
JPS61102232A (ja) * | 1984-10-26 | 1986-05-20 | Diafoil Co Ltd | 包装用ポリエステルフィルム |
US4784980A (en) * | 1987-07-15 | 1988-11-15 | Amoco Corporation | Process for preparing zeolite A from spent cracking catalyst |
DE4200248A1 (de) * | 1992-01-08 | 1993-07-15 | Basf Ag | Verfahren zur regenerierung von metalloxid-katalysatoren |
US5928980A (en) * | 1997-02-06 | 1999-07-27 | Research Triangle Institute | Attrition resistant catalysts and sorbents based on heavy metal poisoned FCC catalysts |
US6395665B2 (en) * | 1998-07-24 | 2002-05-28 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
JP3059136B2 (ja) * | 1998-07-24 | 2000-07-04 | 三菱重工業株式会社 | 脱硝触媒の再生方法 |
CN1223404C (zh) * | 2001-02-13 | 2005-10-19 | Sk株式会社 | 选择性催化还原氮氧化物的催化剂及其制备方法 |
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JP4264642B2 (ja) | 2009-05-20 |
US20080248943A1 (en) | 2008-10-09 |
KR20060080198A (ko) | 2006-07-07 |
WO2005028102A1 (ja) | 2005-03-31 |
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