CN1080593C - Fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method - Google Patents
Fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method Download PDFInfo
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- CN1080593C CN1080593C CN98111445A CN98111445A CN1080593C CN 1080593 C CN1080593 C CN 1080593C CN 98111445 A CN98111445 A CN 98111445A CN 98111445 A CN98111445 A CN 98111445A CN 1080593 C CN1080593 C CN 1080593C
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- Prior art keywords
- temperature
- hydrogen
- catalyst
- feed
- fluidized bed
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- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000003213 activating effect Effects 0.000 title claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 16
- 238000009903 catalytic hydrogenation reaction Methods 0.000 title claims abstract description 9
- 230000008929 regeneration Effects 0.000 title claims description 23
- 238000011069 regeneration method Methods 0.000 title claims description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000001257 hydrogen Substances 0.000 claims abstract description 52
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 18
- 230000004913 activation Effects 0.000 claims abstract description 15
- 238000002485 combustion reaction Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 235000021050 feed intake Nutrition 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002955 isolation Methods 0.000 claims description 5
- 231100000614 poison Toxicity 0.000 claims description 5
- 230000007096 poisonous effect Effects 0.000 claims description 5
- 230000002441 reversible effect Effects 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000001172 regenerating effect Effects 0.000 abstract description 3
- 150000001879 copper Chemical class 0.000 abstract 1
- 230000000737 periodic effect Effects 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 3
- 239000002360 explosive Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a novel non-nitrogen regenerating and activating method for a gas-phase catalytic hydrogenation catalyst of a fluidized bed, particularly to a novel periodic activating and regenerating technology for modified copper CuSiO2 catalytic hydrogenation products. The method comprises the steps that after a catalyst in a fluidized bed is maintained to blow materials for 2 to 4 hours above 160DEG C, hydrogen in a system is exhausted, a hydrogen system is isolated, compressed air is led into the fluidized bed to cause the temperature of the catalyst to slowly rise, the temperature rise speed and the system pressure are controlled, and the temperature of a control center is from 380 DEG C to about 450 DEG C until the combustion is finished. When the temperature drops to 160 DEG C to 200 DEG C, the hydrogen is slowly led to strictly control the speed rate of the temperature rise. When the temperature rises to 230 DEG C to 280 DEG C, the temperature is maintained to deeply activate the catalyst until the temperature is not controlled, the hydrogen purity is increased above 89%, the temperature is controlled above 180DEG C, and the materials are blown above 2 hours to complete the activation.
Description
That fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method of the present invention relates to is a kind of modification copper C that is applicable to
u-S
iO
2The periodicity activating and regenerating new technology of catalyst hydrogenation product.
The domestic C that all adopts of nitrobenzene catalytic hydrogenation system aniline
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iO
2Catalyst, catalyst uses in certain load with in the time, because increasing with invertibity and toxicant, the lip-deep carbon deposit of catalyst activity covers, thereby activity is dropped in the time of should not remaining in operation, just must regenerate to catalyst, its usual method is that the catalyst of inactivation is burnt in air, to remove surperficial carbon deposit, activate with hydrogen again, make it to recover active, continue to use.Its major control method is: keep catalyst and reduce to normal temperature after 4 hours blowing material more than 180 ℃, use the method for " displacement " that hydrogen in the system is removed again, conventional method is to carry out physical permutations with high-purity nitrogen, and it is qualified that hydrogen content in system's tail gas＜0.5% (volume) is just calculated displacement.With more than the Steam Heating to 180 ℃, slowly, an inner catalyst temperature is slowly risen again to the logical compressed air of system, and control heating rate≤50 ℃/hr, system pressure is no more than 0.15Mpa, and control centre's temperature is about 400 ℃, up to all burnt, temperature descends, behind the regeneration ending.After this under inferior order, recover logical nitrogen in fluid bed, carry out the exchange system air, the content of oxygen＜1% (volume) is qualified in system, is warmed up to more than 180 ℃ with steam again, slowly feeds hydrogen and activates, strict control temperature rise rate, and holding temperature makes its deep activation at 260 ℃ ± 10 ℃, loses control of up to temperature, drop to 200 ℃, blow and expect that a few hours can feed intake.
In above regeneration activating process, usefulness nitrogen physical permutations process is arranged twice, need with a large amount of nitrogen, must use nitrogen production by air separation, pipeline is carried, empty substation does not need continuous running again, and the several months is just moved once, and utilization rate of equipment and installations is low and investment is big, and also need strict maintenance to maintain, assurance causes manpower financial capacity's serious waste with using with opening, and is " physical permutations " because of nitrogen replacement hydrogen again, the hydrogen that adsorbs in the catalyst endoporus can't be replaced, and the displacement of system is dropped a hint, and diffusion concentration increases progressively in environment, meets thunder and lightning, naked light, is easy to occur unexpected.
The objective of the invention is weak point at above-mentioned modification copper catalyst regeneration activating method existence, a kind of fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method is provided, air is directly adopted in regeneration, activation directly adopts hydrogen with hydrogen and oxygen in the method consumption systems of " chemical replacement ", existing regeneration, the direct weak point of bringing with nitrogen " physical permutations " of activation have been solved, it is little to have scale of investment, advantages such as operating cost is low, maintaining is easy, energy consumption is low, regeneration activating weak point consuming time, and handling safety is reliable.
Fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method takes following scheme to realize: its regeneration, activating process method are for keeping modification copper C in the fluid bed
u-S
iO
2Catalyst was blowing material 2～4 hours with hydrogen more than 160 ℃, blow the material back interior hydrogen of tail gas atmospheric valve emptying system, and isolation hydrogen gas system, feed compressed air then, fluid bed inner catalyst temperature is slowly risen, and control programming rate≤50 ℃/hr, system pressure is no more than 0.15Mpa, and control centre's temperature is about 380 ℃～450 ℃, until catalyst carbon deposit and reversible poisonous substance all burnt, temperature descends, if continue to feed a large amount of air, when temperature no longer raises, illustrate that regeneration finishes, slowly lower the temperature to system this moment, when temperature is reduced to 160 ℃～200 ℃, can remove hydrogen and isolate, close the tail gas atmospheric valve, slowly feed the strict control of hydrogen temperature rise rate, and programming rate≤50 ℃/hr, when temperature is raised to 230 ℃～280 ℃, keep, make its deep activation, lose control of up to temperature, continue to feed a large amount of hydrogen and open the tail gas atmospheric valve, improve hydrogen purity, when purity is above greater than 89%, keep system's malleation, and the control temperature is more than 180 ℃, blow material more than 2 hours, activation is finished, and production can feed intake.Whole modification copper C
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iO
2Catalyst regeneration activation process is all carried out in fluid bed.
Learn according to the relevant technologies handbook: air and hydrogen can form explosive mixture, its explosive range is 4～75%, be exactly that the aerial concentration of system's hydrogen reaches more than 4%, 75% danger close when following, can blast as naked light, if density of hydrogen is less than 4% or greater than 75%, even if running into burning things which may cause a fire disaster can not set off an explosion or burn yet, according to this principle, can know: content is less than 25% or greater than 96% in the content in hydrogen for air, and it is also just not dangerous can not form explosive mixture.In the regeneration activating process when temperature rises to more than 180 ℃, bubbling air, hydrogen, the hydrogen in airborne oxygen and the system, or the air in feeding hydrogen and the system, surfaces externally and internally immediate response at catalyst generates water, this catalyst reaction is highly beneficial to replacing, and promptly consumes two parts of hydrogen and a oxygen, also increases by four parts of nitrogen, make system safer, and very thorough, major control throughput and ventilation speed, safety has and must ensure.When another key of the present invention was bubbling air and hydrogen, the operator can look bed internal pressure, variations in temperature, can judge the scope of the explosion limit of an interior mist, increased safety guarantee again for simultaneously operation.
Facts have proved, with hydrogen, the air in " chemical replacement " method exchange system, ratio is directly used not only safe and feasible of nitrogen replacement (physical permutations), and the simple scale of investment of equipment needed thereby is little, and operating cost is low, maintaining is easy, easy to operate, required energy consumption is low, and regeneration activating takes a short time, this regeneration activating method is very economical, reasonable, and is easy to utilize.
Embodiment 1:
Keep modification copper C in the fluid bed
u-S
iO
2Catalyst blew material 2 hours with hydrogen about 160 ℃, blow the material back interior hydrogen of tail gas atmospheric valve emptying system, and isolation hydrogen gas system, feed compressed air then, fluid bed inner catalyst temperature is slowly risen, and control programming rate≤50 ℃/hr, system pressure is no more than 0.15Mpa, and control centre's temperature is about 380 ℃, until catalyst carbon deposit and reversible poisonous substance all burnt, temperature descends, if continue to feed a large amount of air, when temperature no longer raises, illustrate that regeneration finishes, slowly lower the temperature to system this moment, when temperature is reduced to 160 ℃, can remove hydrogen and isolate, close the tail gas atmospheric valve, slowly feed the strict control of hydrogen temperature rise rate, and programming rate≤50 ℃/hr, when temperature is raised to 230 ℃, keep, make its deep activation, lose control of up to temperature, continue to feed a large amount of hydrogen and open the tail gas atmospheric valve, improve hydrogen purity, when purity is above greater than 89%, keep system's malleation, and the control temperature is more than 180 ℃, blow material more than 2 hours, activation is finished, and production can feed intake.
Embodiment 2:
Keep modification copper C in the fluid bed
u-S
iO
2Catalyst blew material 3 hours with hydrogen about 180 ℃, blow the material back interior hydrogen of tail gas atmospheric valve emptying system, and isolation hydrogen gas system, feed compressed air then, fluid bed inner catalyst temperature is slowly risen, and control programming rate≤50 ℃/hr, system pressure is no more than 0.15Mpa, and control centre's temperature is about 400 ℃, until catalyst carbon deposit and reversible poisonous substance all burnt, temperature descends, if continue to feed a large amount of air, when temperature no longer raises, illustrate that regeneration finishes, slowly lower the temperature to system this moment, when temperature is reduced to 180 ℃, can remove hydrogen and isolate, close the tail gas atmospheric valve, slowly feed the strict control of hydrogen temperature rise rate, and programming rate≤50 ℃/hr, when temperature is raised to 260 ℃, keep, make its deep activation, lose control of up to temperature, continue to feed a large amount of hydrogen and open the tail gas atmospheric valve, improve hydrogen purity, when purity is above greater than 89%, keep system's malleation, and the control temperature is more than 180 ℃, blow material more than 2 hours, activation is finished, and production can feed intake.
Embodiment 3:
Keep modification copper C in the fluid bed
u-S
iO
2Catalyst blew material 4 hours with hydrogen about 200 ℃, blow the material back interior hydrogen of tail gas atmospheric valve emptying system, and isolation hydrogen gas system, feed compressed air then, fluid bed inner catalyst temperature is slowly risen, and control programming rate≤50 ℃/hr, system pressure is no more than 0.15Mpa, and control centre's temperature is about 450 ℃, until catalyst carbon deposit and reversible poisonous substance all burnt, temperature descends, if continue to feed a large amount of air, when temperature no longer raises, illustrate that regeneration finishes, slowly lower the temperature to system this moment, when temperature is reduced to 200 ℃, can remove hydrogen and isolate, close the tail gas atmospheric valve, slowly feed the strict control of hydrogen temperature rise rate, and programming rate≤50 ℃/hr, when temperature is raised to 280 ℃, keep, make its deep activation, lose control of up to temperature, continue to feed a large amount of hydrogen and open the tail gas atmospheric valve, improve hydrogen purity, when purity is above greater than 89%, keep system's malleation, and the control temperature is more than 180 ℃, blow material more than 2 hours, activation is finished, and production can feed intake.
Claims (1)
1, a kind of fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method is characterized in that regeneration, activation method are for keeping modification copper C in the fluid bed
u-S
iO
2Catalyst was blowing material 2～4 hours with hydrogen more than 160 ℃, blow the material back interior hydrogen of tail gas atmospheric valve emptying system, and isolation hydrogen gas system, feed compressed air then, fluid bed inner catalyst temperature is slowly risen, and control programming rate≤50 ℃/hr, system pressure is no more than 0.15Mpa, and control centre's temperature is about 380 ℃～450 ℃, finish until combustion catalyst carbon deposit and reversible poisonous substance, temperature descends, if continue to feed a large amount of air, when temperature no longer raises, illustrate that regeneration finishes, slowly lower the temperature to system this moment, when temperature is reduced to 160 ℃～200 ℃, can remove hydrogen and isolate, close the tail gas atmospheric valve, slowly feed the strict control of hydrogen temperature rise rate, and programming rate≤50 ℃/hr, when temperature is raised to 230 ℃～280 ℃, keep, make its deep activation, lose control of up to temperature, continue to feed a large amount of hydrogen and open the tail gas atmospheric valve, improve hydrogen purity, when purity is above greater than 89%, keep system's malleation, and the control temperature is more than 180 ℃, blow material more than 2 hours, activation is finished, and production can feed intake.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98111445A CN1080593C (en) | 1998-08-06 | 1998-08-06 | Fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98111445A CN1080593C (en) | 1998-08-06 | 1998-08-06 | Fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1213589A CN1213589A (en) | 1999-04-14 |
| CN1080593C true CN1080593C (en) | 2002-03-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN98111445A Expired - Fee Related CN1080593C (en) | 1998-08-06 | 1998-08-06 | Fluidized bed gas-phase catalytic hydrogenation catalyst non-nitrogen regeneration activating method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102077026B (en) * | 2008-05-14 | 2013-05-01 | 莱昂工程股份公司 | Combustion material process and related apparatus |
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| CN101732986B (en) * | 2008-11-20 | 2014-05-28 | 中国石油化工股份有限公司 | Method for removal of sulfur and nitrogen oxides in smoke |
| CN101829537B (en) * | 2009-03-12 | 2014-01-15 | 中国石油化工股份有限公司 | A kind of adsorbent composition containing Group IB metal component and its application |
| CN103537300B (en) * | 2012-07-12 | 2015-12-16 | 中国石油化工股份有限公司 | Produce the regeneration activating method of indoles catalyst |
| CN106647597A (en) * | 2016-10-11 | 2017-05-10 | 南京工业大学 | PLC (programmable logic controller) multi-stage temperature control method for fluidized bed catalytic combustion electric heating furnace |
| CN111056949B (en) * | 2018-10-17 | 2021-05-11 | 中国石油化工股份有限公司 | Reaction device and reaction method for preparing aniline through continuous reaction, regeneration and activation |
| CN119555732A (en) * | 2024-11-27 | 2025-03-04 | 万华化学集团股份有限公司 | A method for determining the deactivation temperature and deactivation characteristics of a hydroformylation catalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1452466A (en) * | 1975-04-04 | 1976-10-13 | Chemopetrol | Process for the production of aniline and apparatus therefor |
| EP0212602A1 (en) * | 1985-08-29 | 1987-03-04 | Bayer Ag | Process for the regeneration of catalysts for the gas phase reduction of aromatic nitro compounds |
| GB2182330A (en) * | 1985-11-01 | 1987-05-13 | First Chemical Corp | Production of an aromatic monoamine and an aromatic diamine |
| DE4039026A1 (en) * | 1990-12-07 | 1992-06-11 | Bayer Ag | METHOD FOR PRODUCING ANILINE |
| CN1129212A (en) * | 1994-08-08 | 1996-08-21 | 拜尔公司 | Process for the production of aromatic amines |
-
1998
- 1998-08-06 CN CN98111445A patent/CN1080593C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1452466A (en) * | 1975-04-04 | 1976-10-13 | Chemopetrol | Process for the production of aniline and apparatus therefor |
| EP0212602A1 (en) * | 1985-08-29 | 1987-03-04 | Bayer Ag | Process for the regeneration of catalysts for the gas phase reduction of aromatic nitro compounds |
| GB2182330A (en) * | 1985-11-01 | 1987-05-13 | First Chemical Corp | Production of an aromatic monoamine and an aromatic diamine |
| DE4039026A1 (en) * | 1990-12-07 | 1992-06-11 | Bayer Ag | METHOD FOR PRODUCING ANILINE |
| CN1129212A (en) * | 1994-08-08 | 1996-08-21 | 拜尔公司 | Process for the production of aromatic amines |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102077026B (en) * | 2008-05-14 | 2013-05-01 | 莱昂工程股份公司 | Combustion material process and related apparatus |
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| Publication number | Publication date |
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| CN1213589A (en) | 1999-04-14 |
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