CN103801287B - 一种负载型耐硫甲烷化催化剂的制备方法 - Google Patents
一种负载型耐硫甲烷化催化剂的制备方法 Download PDFInfo
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- CN103801287B CN103801287B CN201210436863.4A CN201210436863A CN103801287B CN 103801287 B CN103801287 B CN 103801287B CN 201210436863 A CN201210436863 A CN 201210436863A CN 103801287 B CN103801287 B CN 103801287B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 176
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 24
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 230000000694 effects Effects 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 238000001802 infusion Methods 0.000 claims abstract description 7
- -1 wherein M1For Co Inorganic materials 0.000 claims abstract description 7
- 238000005470 impregnation Methods 0.000 claims abstract description 4
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 29
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 16
- 229910001868 water Inorganic materials 0.000 claims description 16
- 229910002651 NO3 Inorganic materials 0.000 claims description 15
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 11
- 238000004898 kneading Methods 0.000 claims description 11
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 239000011593 sulfur Substances 0.000 claims description 10
- 238000007792 addition Methods 0.000 claims description 9
- 229910001593 boehmite Inorganic materials 0.000 claims description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 9
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 150000003863 ammonium salts Chemical class 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000001935 peptisation Methods 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000009938 salting Methods 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- 229920001971 elastomer Polymers 0.000 claims description 2
- 239000000806 elastomer Substances 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000012986 modification Methods 0.000 abstract description 5
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- 229910052750 molybdenum Inorganic materials 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 description 39
- 238000012360 testing method Methods 0.000 description 33
- 238000006243 chemical reaction Methods 0.000 description 23
- 230000003197 catalytic effect Effects 0.000 description 20
- 239000008367 deionised water Substances 0.000 description 17
- 229910021641 deionized water Inorganic materials 0.000 description 17
- 239000007789 gas Substances 0.000 description 17
- 230000015572 biosynthetic process Effects 0.000 description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 13
- 238000003786 synthesis reaction Methods 0.000 description 13
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 description 12
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 11
- 239000011259 mixed solution Substances 0.000 description 11
- 210000002966 serum Anatomy 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 235000015165 citric acid Nutrition 0.000 description 6
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 6
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 6
- 239000000725 suspension Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
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- 239000000047 product Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 150000002927 oxygen compounds Chemical class 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 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
- 238000006424 Flood reaction Methods 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 229910006213 ZrOCl2 Inorganic materials 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
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- 238000002161 passivation Methods 0.000 description 1
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- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 description 1
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CN105013472A (zh) * | 2015-06-16 | 2015-11-04 | 中国科学院山西煤炭化学研究所 | 一种适用于高浓度co甲烷化的耐硫催化剂及制法和应用 |
FR3076746B1 (fr) * | 2018-01-15 | 2022-07-01 | Ifp Energies Now | Procede de preparation d'un catalyseur particulier d'hydrogenation selective par malaxage et impregnation |
CN109433222B (zh) * | 2018-12-17 | 2022-02-08 | 新地能源工程技术有限公司 | 一种耐硫甲烷化催化剂及其制备方法 |
CN111229203A (zh) * | 2020-03-13 | 2020-06-05 | 中国华能集团清洁能源技术研究院有限公司 | 一种复合结构载体高温耐硫甲烷化催化剂及其制备方法 |
CN111266130A (zh) * | 2020-03-13 | 2020-06-12 | 中国华能集团清洁能源技术研究院有限公司 | 一种复合结构载体低温耐硫甲烷化催化剂及其制备方法 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101214442A (zh) * | 2007-12-26 | 2008-07-09 | 厦门大学 | 耐硫一氧化碳变换催化剂及其制备方法 |
CN101745401A (zh) * | 2009-12-07 | 2010-06-23 | 中国科学院山西煤炭化学研究所 | 一种负载型耐硫甲烷化催化剂及制备方法和应用 |
CN102240556A (zh) * | 2011-04-29 | 2011-11-16 | 福州大学 | 一种适用于高压工艺的co耐硫变换催化剂及其制备方法 |
CN102247861A (zh) * | 2011-05-11 | 2011-11-23 | 神华集团有限责任公司 | 一种煤制天然气高温甲烷化催化剂及其制备方法 |
CN102302929A (zh) * | 2011-07-12 | 2012-01-04 | 神华集团有限责任公司 | 一种耐硫高温甲烷化催化剂及其制备方法 |
WO2012040111A1 (en) * | 2010-09-23 | 2012-03-29 | Conocophillips Company | Sulfur-tolerant catalyst prepared through high pressure decomposition |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101214442A (zh) * | 2007-12-26 | 2008-07-09 | 厦门大学 | 耐硫一氧化碳变换催化剂及其制备方法 |
CN101745401A (zh) * | 2009-12-07 | 2010-06-23 | 中国科学院山西煤炭化学研究所 | 一种负载型耐硫甲烷化催化剂及制备方法和应用 |
WO2012040111A1 (en) * | 2010-09-23 | 2012-03-29 | Conocophillips Company | Sulfur-tolerant catalyst prepared through high pressure decomposition |
CN102240556A (zh) * | 2011-04-29 | 2011-11-16 | 福州大学 | 一种适用于高压工艺的co耐硫变换催化剂及其制备方法 |
CN102247861A (zh) * | 2011-05-11 | 2011-11-23 | 神华集团有限责任公司 | 一种煤制天然气高温甲烷化催化剂及其制备方法 |
CN102302929A (zh) * | 2011-07-12 | 2012-01-04 | 神华集团有限责任公司 | 一种耐硫高温甲烷化催化剂及其制备方法 |
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Address after: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Patentee after: CHINA ENERGY INVESTMENT Corp.,Ltd. Patentee after: Beijing low carbon clean energy research institute Address before: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Patentee before: CHINA ENERGY INVESTMENT Corp.,Ltd. Patentee before: Beijing low carbon clean energy research institute |