CN102310005A - Regeneration method for heavy oil hydro-treating catalyst - Google Patents
Regeneration method for heavy oil hydro-treating catalyst Download PDFInfo
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- CN102310005A CN102310005A CN2010102221528A CN201010222152A CN102310005A CN 102310005 A CN102310005 A CN 102310005A CN 2010102221528 A CN2010102221528 A CN 2010102221528A CN 201010222152 A CN201010222152 A CN 201010222152A CN 102310005 A CN102310005 A CN 102310005A
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Abstract
The invention discloses a regeneration method for a heavy oil hydro-treating catalyst. The regeneration method comprises the following steps of: performing dry distillation, washing with an acidic solution, and performing roasting coke removal treatment, wherein the dry distillation temperature is 300 to 550 DEG C, the acidic solution is a hydrochloric acid-containing solution, the weight ratio of the washing acid to the catalyst is 5 to 50L/Kg, and the acid concentration is 0.1 to 0.5mol/L. Compared with the prior art, the regeneration method has the advantage of well recovering the service performance of an inactivated catalyst.
Description
Technical field
The present invention relates to a kind of renovation process of heavy oil hydrogenating treatment catalyst, particularly draw off the processing method of regenerating behind the reactor behind the heavy oil hydrogenating treatment catalyst inactivation.
Background technology
Along with crude quality becomes the bad strictness gradually that requires with environmental regulation, hydrogen addition technology becomes the important means of oil product processing, and correspondingly, the consumption of various hydrogenation catalysts increases thereupon.Hydrogenation catalyst is inactivation gradually in use, drop to a certain degree through activity after certain service cycle after, need to stop work and handle.In the common hydrotreatment technology; The inactivation of catalyst mainly is the carbon deposit on surface, catalyst duct; The method that generally can adopt solvent extraction or roasting to take off charcoal removes; Activity of such catalysts generally can return to more than 95% of fresh catalyst activity, can reuse fully, and the regeneration times of catalyst can reach 2～6 times.
In the existing relevant decaying catalyst regeneration techniques, most of patents consider emphatically how to prevent that decaying catalyst from concentrating or the problem of excessive exotherms in regenerative process.Under oxygen containing gas, the method that adopts laser radiation is to the catalyst decoking like patent USP 5,037,785 suggestions; Patent USP 4,202, and 865 suggestions are annotated oxygen with batch (-type); Patent USP 4,780, and 195 think then that with USP 4,417,975 grades adding a certain amount of water prevents sintering of catalyst etc. in atmosphere.
Patent USP 5,916, and 835 pairs of heterogeneous decaying catalysts of titaniferous that are used for epoxidation of ethylene adopt water, alcohol, ester, nitrile, ether, aromatic hydrocarbons, ketone equal solvent to handle, and have reached the purpose of recovering catalyst activity.When adopting the solvent reclamation catalyst, different to the effect of different coking materials, relatively poor for the far-gone catalyst regeneration effect of coking charing.CN200410050722.4 uses a kind of special solvent that the hydrogenation catalyst of inactivation is carried out Regeneration Treatment; Can carry out Regeneration Treatment to catalyst for hydrotreatment of residual oil though mention; But solvent reclamation generally can only remove the coking material, and is undesirable to the regeneration effect because of the catalyst for hydrotreatment of residual oil of plated metal impurity inactivation.
In the heavy charge hydrotreatment process that comprises various residual oil and heavy oil; The inactivation of catalyst is the carbon deposit in the catalyst duct on the one hand, also be the deposition of various metals in the catalyst duct simultaneously, and the regenerability of the decaying catalyst that this mode causes is very poor; Generally only can use once; Dead catalyst can only adopt the mode of metal recovery to handle, or adopts the mode of landfill to handle, and causes the processing cost height and the problem of environmental pollution of dead catalyst.
Summary of the invention
To the deficiency of prior art, the present invention provides the regeneration treating method of a kind of heavy oil reaction back dead catalyst, can recover the serviceability of decaying catalyst preferably.
The renovation process of heavy oil hydrogenating treatment catalyst of the present invention comprises following process: the heavy oil hydrogenating treatment catalyst of inactivation at first carries out destructive distillation, adopts the acid solution washing then, then adopts the roasting decarbidize to handle.Pyrolysis temperature is 300～550 ℃; Acid solution is hydrochloric solution, and the washing acid amount is 5～50L/Kg with the ratio of catalyst, and acid concentration is 0.1～0.5mol/L; Roasting decarbidize temperature is 400～650 ℃.
In the inventive method; The apparatus and method that can adopt this area conventional are handled in the destructive distillation of decaying catalyst, as can adopting similar Maoming fluidized retoring stove, and cyclone separator are set; Prevent in the fluidized retoring catalyst granules to be taken out of; Cyclone separator can be provided with one-level, also can be provided with multistagely, also can adopt the destructive distillation device of other form.Low-temperature cracking process is adopted in destructive distillation, and the gas that destructive distillation obtains is through reclaiming corresponding liquid phase hydro carbons after the condensation.Till destructive distillation to the not obvious generation gas.
In the inventive method, the acid solution wash temperature is 10～70 ℃, is preferably 20～40 ℃, and wash time is 2～60 minutes, is preferably 10～30 minutes.Can add suitable organic additive in the acid solution.The washing that suits after the acid solution washing.
In the inventive method, this area conventional catalyst renovation process is adopted in the roasting decarbidize, as the amount of oxygen control sintering temperature that feeds during the control roasting, roasting is not to continuing consume oxygen, the catalyst regeneration bed does not have temperature rise, CO in the tail gas
2Content less than 0.05v% till.
In the inventive method, can comprise other some steps, as decaying catalyst is sieved, the catalyst after the roasting regeneration carries out activity adjustment etc.Screening can be adopted conventional method, filters out the catalyst of pulverizing or the catalyst of serious coking etc.The method of active adjustment is generally and adjusts with the solution that contains organic solvent etc. in this area.
Adopt said method of the present invention, can obtain following technique effect:
1, adopts low-temperature cracking process at first to handle decaying catalyst, in reclaiming decaying catalyst, in the part Residual oil, part coking material is obtained liquid hydrocarbon through dry distillation reactor, improved the rate of recovery of valuable product.Select suitable pyrolysis temperature, when helping the withdrawal liquid hydrocarbon, the guard catalyst structure is not damaged.
2, the catalyst after the destructive distillation adopts the acid solution washing; The metal impurities that can the effective elimination catalyst in the hydrotreatment process, deposit; Like sodium, calcium, iron, vanadium, nickel etc.; Help the abundant recovery of catalyst activity, solved and only used decarbonization method can not recover the problem of heavy-oil hydrogenation catalyst decaying catalyst.
3, the washing of low temperature distillation and acid solution organically combines; Low temperature distillation can remove part coking material; The metal impurities that deposit in the catalyst are partly come out, remove these metal impurities when helping the acid solution washing, because the metal impurities that deposit on the catalyst deposit with the coking process in course of reaction synchronously gradually; Therefore after destructive distillation removed part coking material, some metal impurities can remove in the acid solution washing process smoothly; Simultaneously; Low temperature distillation is when removing part coking material; Produce new charcoal property material; These new charcoal property materials have the certain protection effect to the reactive metal of initial load on catalyst carrier and the catalyst, avoid when acid solution washs, catalyst carrier excessively being destroyed, and have also avoided the loss of the original supported active metal of catalyst to a certain extent.
4, the method that adopts roasting to take off charcoal is at last further recovered activity of such catalysts, can the carbon deposit of catalyst be removed comparatively up hill and dale, fully recovers activity of such catalysts.
The inventive method is got up steps such as destructive distillation, pickling, roasting and suitable condition organic synthesis; Make the hydrotreating catalyst of inactivation obtain good regeneration; Experiment shows; Inactivation catalyst for hydrotreatment of residual oil activation recovering through the inventive method Regeneration Treatment has arrived fresh catalyst more than 90%, has reached the requirement that reuses, and can be used in the active lower process that requires.For example, the decaying catalyst of the 3rd reactor in the boiling bed residual oil hydrotreatment multiple reactor series connection is carried out Regeneration Treatment, join first reactor or second reactor through online displacement then.
Description of drawings
Fig. 1 is a kind of concrete process flow diagram of heavy oil hydrogenating treatment catalyst renovation process of the present invention.
Charcoal is taken off in 1-preliminary treatment 2-destructive distillation 3-Oil-gas Separation 4-pickling 5-washing 6-oven dry 7-roasting
The specific embodiment
Be example with the residual hydrocracking decaying catalyst below, specify scheme of the present invention and effect.
The inactivation catalyst for hydrotreatment of residual oil that draws off from reactor; Preliminary treatment such as can at first sieve; Adopting suitable distillation apparatus to carry out destructive distillation then handles; The gas that destructive distillation obtains reclaims liquid hydrocarbon through after the condensation, and fixed gas can get into gas train, when not having obvious gas to produce, stops destructive distillation and handles.
Distillation apparatus can be a fixed-bed type, also can be fluidized bed type or moving-bed type etc., by the mode of operation operation of existing distillation apparatus.Retort process can feed nitrogen etc. carries out gas and carries, and improves the liquid hydrocarbon productive rate, reduces the growing amount of coke.
The acid solution washing can be adopted common equipment, generally needs corrosion resistant equipment, is preferably under the stirring condition during acid solution washing and carries out.Generally need carry out water elution after the acid solution washing removes attached to the acidic materials on the catalyst.
Roasting is taken off charcoal and is adopted this area conventional method, and oxygen and temperature that the control roasting process feeds are avoided the too high destruction of causing catalyst of sintering temperature.
The inactivation catalyst for hydrotreatment of residual oil; Earlier 450 ℃ of following destructive distillation to there not being obvious gas to produce; Adopt the hydrochloric acid solution of 0.2mol/L to wash then 15 minutes, the temperature of hydrochloric acid solution washing is 50 ℃, and hydrochloric acid solution is that consumption is 8L/Kg with the ratio of catalyst; Wash dry back CO in 500 ℃ of following roasting to roasting tail gas then 2 times
2Volumetric concentration is lower than till 0.03%.Analysis shows; Indexs such as the pore volume of regenerated catalyst, specific area are near fresh catalyst; The metal impurities removal efficiency of deposition is about 82%, in residual hydrogenation small test device, carries out the regenerated catalyst evaluation, is 100% in the fresh catalyst activity; The activity of regenerated catalyst reaches 92%, can reuse.
The inactivation catalyst for hydrotreatment of residual oil; Earlier 500 ℃ of following destructive distillation to there not being obvious gas to produce; Adopt the hydrochloric acid solution of 0.4mol/L to wash then 30 minutes, the temperature of hydrochloric acid solution washing is 30 ℃, and hydrochloric acid solution is that consumption is 15L/Kg with the ratio of catalyst; Wash dry back CO in 450 ℃ of following roasting to roasting tail gas then 2 times
2Volumetric concentration is lower than till 0.03%.Analysis shows; Indexs such as the pore volume of regenerated catalyst, specific area are near fresh catalyst; The metal impurities removal efficiency of deposition is about 85%, in residual hydrogenation small test device, carries out the regenerated catalyst evaluation, is 100% in the fresh catalyst activity; The activity of regenerated catalyst reaches 93%, can reuse.
Comparative example 1
According to embodiment 1 described catalyst recovery process, only use roasting to take off the charcoal process, do not adopt destructive distillation and acid solution washing process, the result shows that the activity of regenerated catalyst is merely 65% of fresh catalyst activity, does not reach the requirement that reuses.
Comparative example 2
According to embodiment 1 described catalyst recovery process,, roasting carries out the acid solution washing after taking off charcoal, and the result shows that the activity of regenerated catalyst is 78% of a fresh catalyst activity, suitable reusing.
Claims (3)
1. the renovation process of a heavy oil hydrogenating treatment catalyst, it is characterized in that comprising following process: the heavy oil hydrogenating treatment catalyst of inactivation at first carries out destructive distillation, adopts the acid solution washing then, then adopts the roasting decarbidize to handle; Pyrolysis temperature is 300～550 ℃; Acid solution is hydrochloric solution, and the washing acid amount is 5～50L/Kg with the ratio of catalyst, and acid concentration is 0.1～0.5mol/L.
2. according to the described method of claim 1, it is characterized in that: roasting decarbidize temperature is 400～650 ℃.
3. according to the described method of claim 1, it is characterized in that: the acid solution wash temperature is 10～70 ℃, and wash time is 2～60 minutes.
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| CN2010102221528A CN102310005A (en) | 2010-07-07 | 2010-07-07 | Regeneration method for heavy oil hydro-treating catalyst |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106378209A (en) * | 2016-10-13 | 2017-02-08 | 中海油天津化工研究设计院有限公司 | Method for regenerating fats and oils hydrogenation deactivated catalyst |
| CN106459782A (en) * | 2014-03-27 | 2017-02-22 | 出光兴产株式会社 | Regeneration and Utilization Method of Heavy Oil Desulfurization Catalyst |
| CN107638889A (en) * | 2016-07-22 | 2018-01-30 | 北京华石联合能源科技发展有限公司 | A kind of useless hydrogenation catalyst regeneration method |
| CN108607619A (en) * | 2018-06-15 | 2018-10-02 | 西南化工研究设计院有限公司 | A kind of regeneration method of Dimethyl ether carbonylation methyl acetate catalysis agent |
| CN109174207A (en) * | 2018-07-11 | 2019-01-11 | 上海英保能源化工科技有限公司 | A kind of activity of hydrocatalyst restores and vulcanization process |
| US10208255B2 (en) | 2016-11-21 | 2019-02-19 | Beijin Huashi United Energy Technology and Development | Method for producing light oil through liquefying biomass |
| US10260004B2 (en) | 2016-11-21 | 2019-04-16 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Method for direct liquefaction of biomass |
| US10280370B2 (en) | 2016-11-21 | 2019-05-07 | Beijing Huashi United Energy Technology and Development Co., Ltd | One-pot liquefaction process for biomass |
| US10287506B2 (en) | 2016-11-21 | 2019-05-14 | Beijing Huashi United Energy Technology and Development Co., Ltd | Biomass liquefaction process, and fuel oils and chemical materials prepared by the same |
| US10370608B2 (en) * | 2017-04-12 | 2019-08-06 | Beijing Huashi United Energy Technology And .Development Co., Ltd. | Desulfurization process using a combination of a suspension bed and a fixed bed |
| US10369553B2 (en) | 2016-07-22 | 2019-08-06 | Beijing Huashi United Energy Technology And .Development Co., Ltd | Suspended-bed hydrogenation catalyst and regeneration method therefor |
| US10449489B2 (en) | 2017-04-12 | 2019-10-22 | Beijing Huashi United Energy Technology And Development Co. Ltd | High efficient desulfurization-regeneration system using a suspension bed |
| US10449491B2 (en) | 2017-04-12 | 2019-10-22 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Integrated system for wet desulfurization using a suspension bed and regeneration |
| US10525431B2 (en) | 2016-10-17 | 2020-01-07 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Cold-wall reactor for suspension-bed hydrogenation |
| US10703978B2 (en) | 2016-11-21 | 2020-07-07 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Composition for biomass oil, and preparation method and use thereof |
| US10744451B2 (en) | 2017-04-12 | 2020-08-18 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Wet desulfurization process using a suspension bed |
| US10876056B2 (en) | 2016-12-30 | 2020-12-29 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Process and device for hydrogenation of heavy oil using a suspension-bed |
| US10889770B2 (en) | 2016-12-30 | 2021-01-12 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Method and device for lightening heavy oil by utilizing a suspension-bed hydrogenation process |
| CN115957829A (en) * | 2022-12-26 | 2023-04-14 | 本源精化环保科技有限公司 | Regeneration method of supported catalyst for hydrogenation reduction |
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Cited By (22)
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| CN106459782A (en) * | 2014-03-27 | 2017-02-22 | 出光兴产株式会社 | Regeneration and Utilization Method of Heavy Oil Desulfurization Catalyst |
| CN106459782B (en) * | 2014-03-27 | 2018-06-22 | 出光兴产株式会社 | Regeneration and Utilization Method of Heavy Oil Desulfurization Catalyst |
| CN107638889A (en) * | 2016-07-22 | 2018-01-30 | 北京华石联合能源科技发展有限公司 | A kind of useless hydrogenation catalyst regeneration method |
| CN107638889B (en) * | 2016-07-22 | 2020-12-08 | 北京华石联合能源科技发展有限公司 | Method for regenerating waste hydrogenation catalyst |
| RU2679132C2 (en) * | 2016-07-22 | 2019-02-06 | Бэйцзин Хуаши Юнайтед Энерджи Текнолоджи Энд Девелопмент Ко., Лтд | Catalyst of hydrogenation in a suspended layer and method for its regeneration |
| US10369553B2 (en) | 2016-07-22 | 2019-08-06 | Beijing Huashi United Energy Technology And .Development Co., Ltd | Suspended-bed hydrogenation catalyst and regeneration method therefor |
| CN106378209A (en) * | 2016-10-13 | 2017-02-08 | 中海油天津化工研究设计院有限公司 | Method for regenerating fats and oils hydrogenation deactivated catalyst |
| US10525431B2 (en) | 2016-10-17 | 2020-01-07 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Cold-wall reactor for suspension-bed hydrogenation |
| US10287506B2 (en) | 2016-11-21 | 2019-05-14 | Beijing Huashi United Energy Technology and Development Co., Ltd | Biomass liquefaction process, and fuel oils and chemical materials prepared by the same |
| US10260004B2 (en) | 2016-11-21 | 2019-04-16 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Method for direct liquefaction of biomass |
| US10208255B2 (en) | 2016-11-21 | 2019-02-19 | Beijin Huashi United Energy Technology and Development | Method for producing light oil through liquefying biomass |
| US10703978B2 (en) | 2016-11-21 | 2020-07-07 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Composition for biomass oil, and preparation method and use thereof |
| US10280370B2 (en) | 2016-11-21 | 2019-05-07 | Beijing Huashi United Energy Technology and Development Co., Ltd | One-pot liquefaction process for biomass |
| US10876056B2 (en) | 2016-12-30 | 2020-12-29 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Process and device for hydrogenation of heavy oil using a suspension-bed |
| US10889770B2 (en) | 2016-12-30 | 2021-01-12 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Method and device for lightening heavy oil by utilizing a suspension-bed hydrogenation process |
| US10370608B2 (en) * | 2017-04-12 | 2019-08-06 | Beijing Huashi United Energy Technology And .Development Co., Ltd. | Desulfurization process using a combination of a suspension bed and a fixed bed |
| US10449489B2 (en) | 2017-04-12 | 2019-10-22 | Beijing Huashi United Energy Technology And Development Co. Ltd | High efficient desulfurization-regeneration system using a suspension bed |
| US10449491B2 (en) | 2017-04-12 | 2019-10-22 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Integrated system for wet desulfurization using a suspension bed and regeneration |
| US10744451B2 (en) | 2017-04-12 | 2020-08-18 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Wet desulfurization process using a suspension bed |
| CN108607619A (en) * | 2018-06-15 | 2018-10-02 | 西南化工研究设计院有限公司 | A kind of regeneration method of Dimethyl ether carbonylation methyl acetate catalysis agent |
| CN109174207A (en) * | 2018-07-11 | 2019-01-11 | 上海英保能源化工科技有限公司 | A kind of activity of hydrocatalyst restores and vulcanization process |
| CN115957829A (en) * | 2022-12-26 | 2023-04-14 | 本源精化环保科技有限公司 | Regeneration method of supported catalyst for hydrogenation reduction |
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Application publication date: 20120111 |