CN202527185U - Hydrothermal aging device for catalytically cracking catalyst - Google Patents
Hydrothermal aging device for catalytically cracking catalyst Download PDFInfo
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- CN202527185U CN202527185U CN2012200389266U CN201220038926U CN202527185U CN 202527185 U CN202527185 U CN 202527185U CN 2012200389266 U CN2012200389266 U CN 2012200389266U CN 201220038926 U CN201220038926 U CN 201220038926U CN 202527185 U CN202527185 U CN 202527185U
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Abstract
The utility model relates to a hydrothermal aging device for catalytically cracking a catalyst. The hydrothermal aging device comprises a fixed fluidized bed reactor (2) and a heating tile (3), wherein the heating tile (3) is positioned outside the reactor (2); a flange and a flange cover (8) are arranged on the top of the fixed fluidized bed reactor; the fixed fluidized bed reactor is divided into a pre-lifting section I, a fluidization section II and a sedimentation section III; a filter (5) is horizontally arranged on one side of the sedimentation section of the fixed fluidized bed reactor; a cooling tank (12) is arranged outside the fixed fluidized bed reactor; the filter is connected with the cooling tank through a guide pipe (10); a conveniently disassembled heating band (9) wraps the guide pipe; a hole (14) is formed in the bottom of the cooling tank; and the hole in the bottom can be adjusted to be opened and closed.
Description
Technical field
The utility model relates to a kind of experimental rig, particularly relates to a kind of hydrothermal aging device that is used for catalyst for heavy oil catalytic cracking, is used for the ultra steady deactivation process of hydrothermal treatment consists, hydrothermal aging, hydro-thermal of samples such as molecular sieve, catalytic cracking catalyst.
Background technology
In the R&D process of catalytic cracking catalyst; Often need carry out burin-in process to catalyst, and heat treatment or hydrothermal treatment consists are a kind of most important method of preparation molecular sieve and catalyst, the most conventional annealing device is a Muffle furnace; But we know; Temperature is very slowly to the aging effect of catalyst, and the catalytic cracking catalyst in the industry reaches equilibrium activity generally needs about three months, and such aging speed is insufferable in the laboratory.Therefore, adopt 800 ℃ water vapour to carry out the hydrothermal aging processing during laboratory research, only need just can reach in 4～17 hours the catalyst activity of analoging industrial device.The hydrothermal aging process of catalytic cracking catalyst is the preprocessing process that must carry out fresh catalyst in chemical industry test evaluation molecular sieve, catalyst new material, the shakedown, and the required condition of this process is the atmosphere of high temperature and steam.In order to carry out the hydrothermal aging of molecular sieve or catalyst, existingly in petroleum catalytic cracking catalyst research and development field carry out this pretreated device, needed catalyst amounts restrains tens of kilograms and does not wait from several, so the scale of treating apparatus is also different.
Fixed fluidized bed is the very important evaluation experimental device in catalysis laboratory, and its good operating flexibility is widely used in the FCC tests, at present, fixed fluidized bed use be single reactor hydrothermal aging pattern.In existing technology; The steam that carries catalyst dust is condensed into water in the reactor outlet conduit; The catalyst fines that carries also settles down simultaneously, is condensed into local a large amount of depositions of water at pipeline, very easily causes line clogging and reactor pressure is increased; Form the strong acid corrosion in the water owing to there is the appearance of condensed water can cause the sour gas that distributes in the hydrothermal aging to be diffused in addition, cause the unstable and uneasy congruent problem of device of hydrothermal aging data.
USP6,069,012 has announced a kind of follow-on fixed fluidized-bed reactor.The architecture advances of this reactor is mainly reflected in following two aspects: the feed sleeve that can change nozzle height has been adopted in (1), and the interior pipe of this sleeve pipe is used for transferring raw material oil, and sleeve pipe is used for carrying fluidizing gas; (2) set up the fluidizing gas nozzle in the reactor bottom position.This reactor catalyst fluidizing gas adopts high pure nitrogen, and the top is equipped with former oil-in and is strengthened atomizer, and this reactor only is applicable to the heavy oil catalytic cracking reaction under the normal condition and the hydrothermal aging that is not suitable for catalytic cracking catalyst is handled.
CN2512495Y has announced a kind of fixed fluidized-bed reactor that is used for FCC tests research, and this reactor is divided into the initial contact-segment of settling section, conversion zone and finish from top to bottom.Set up fluidizing agent distribution grid and sieve tray in this fixed fluidized-bed reactor; These corrective measures further improve the fluidized state of catalyst; Feedstock oil feeding manner raising from top to bottom simultaneously increases to mink cell focus catalytic cracking and harsh reaction condition adaptability to the raw material preheating temperature control ability.
CN200720169455.1 has announced a kind of fixed fluidized-bed reactor that is used for experimental study.This reactor is divided into from top to bottom: initial contact-segment three parts of settling section, conversion zone and finish.This is fixed fluidized bed to be round table-like design; In voluminous small-numerator olefin system; Product is the quickening of high temperature position linear velocity on reactor top, shortens reaction intermediate in the coexistence time of catalyst dilute phase section, is increasing aspect the polycondensation reaction that suppresses between the small-numerator olefin.
CN200720090308.5 has announced a kind of fixed fluidized-bed reactor, is provided with housing, in housing; Top is columniform settling section; The bottom is obconic conversion zone, and feedstock oil and steam get into pipe and forms the steam admission passage of looping between oil inlet pipe and the outer tube by oil inlet pipe with around the outer tube that the outer wall of oil inlet pipe is provided with; The bottom of oil inlet pipe and outer tube is provided with atomizer; The top of outer tube is provided with steam inlet pipe, and 2 layers of grid plate are set in conversion zone vertically at least, and reaction raw materials oil gets into from the top with fluidizing gas; Contact with catalyst through behind the high temperature preheating, reacted oil gas gets into oil and gas separating system through the filter at top.
A kind of Hanging Basket formula of having announced CN87212197U hydrothermal aging device that wears out; This device can significantly improve assess effectiveness, cut down the consumption of energy, but the catalyst of this device is with the arranged in series Hanging Basket; Exist the catalyst sample hydrothermal aging severity of levels different; And its catalyst is static is flow regime not, and water vapour distributes extremely inhomogeneously at the catalyst bed laminar surface with inner, is having a strong impact on the hydrothermal aging effect of catalyst.
CN101424601A has announced a kind of multi-example high-temperature rotating and roasting device, this device select for use the band centre rotational axis roaster, sample be placed on rotating shaft around; Can put one deck or two-layer; And intersect each other and put, integral body is rotated continuously, is heated evenly; Overcome the shortcoming of hanging blue hydrothermal aging fully, aging equipment can once be accomplished the hydrothermal treatment consists of 24 samples.But this device catalyst is flow regime not; And catalytic cracking catalyst voidage under the vibrations of rotating shaft diminishes; Water vapour is difficult to enter into beds inside; Cause the catalytic cracking catalyst bed behind the hydrothermal aging inner inhomogeneous with surface-active, especially the catalyst behind the hydrothermal aging can not reflect the truth of catalyst when a large amount of catalyst of processing.
CN201020150942.5 discloses the various article hydrothermal aging of a kind of catalytic cracking catalyst device, and the blind flange of this hydrothermal aging device is provided with 2～4 groups of filter and delivery lines.
The small fixed flowing bed reactor that " research of grand celebration residual oil catalytic cracking reaction rule " in 2003 11 volume 3 phases " Beijing Institute of Petrochemical Technology's journal " wherein relates to is provided with delivery line, product condensation then on blind flange.
Summary of the invention
The technical problem underlying that the utility model will solve is to be prone to stop up and the easy defective that corrosion takes place of reactor outlet pipeline to the present existing reactor outlet of fixed fluidized-bed reactor hydrothermal aging device, and a kind of fixed fluidized bed reaction unit that is used for the catalytic cracking catalyst hydrothermal aging is provided.
A kind of hydrothermal aging device that is used for catalytic cracking catalyst; Comprise fixed fluidized-bed reactor 2, heating tile 3; The heating tile is positioned at the outside of reactor; Fixed fluidized-bed reactor is by heating tile heating, and the top of fixed fluidized-bed reactor is provided with flange and blind flange 8, and the bottom of fixed fluidized-bed reactor is provided with steam entry/unload agent mouth 1; Fixed fluidized-bed reactor is divided into pre lift zone I, fluidisation section II and settling section III; Be horizontally disposed with filter 5 in settling section one side; The outside of fixed fluidized-bed reactor is provided with cooling tank 12, and filter is connected by conduit 10 with cooling tank, and the conduit external packets is wrapped with easy-to-dismount heating tape 9; But the bottom of cooling tank is provided with the hole 14 of switch, is convenient to the discharge of condensed water.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model; The blind flange 8 of fixed fluidized-bed reactor is provided with catalyst dress agent mouth 7 and thermocouple 4; The thermoinduction position of thermocouple is positioned at the central axis position of reactor, is used to measure the actual aging temperature of catalyst.The steam entry 1 that the bottom of fixed fluidized-bed reactor is provided with in hydrothermal aging as steam entry; What in the hydrothermal aging process, continue feeds water vapour by steam entry 1, and steam entry 1 stops to feed steam and can be used as and unloads the agent mouth after hydrothermal aging finishes.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model; Blind flange and reactor water plane section are circular; Blind flange 8 its diameters at fixed fluidized-bed reactor 2 tops and the maximum equal diameters of reactor 2; Be convenient to like this reactor flange lid 8 is placed in the heating tile 3, guarantee the temperature homogeneous.The top of fixed fluidized-bed reactor 2 is that blind flange top is placed with heat-preservation cotton 6, guarantees temperature and its internal temperature basically identical of reactor.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model, conduit 10 external packets that connect filter 5 and cooling tank 12 are wrapped with easy-to-dismount heating tape 9, are convenient to insulation, and heating tape 9 temperature are controlled at 100～500 ℃.Make sour gas be not easy condensation, also just can not produce the phenomenon of corrosion in pipes at duct portion.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model, the top of cooling tank 12 is provided with safety vent 11, prevents that the obstruction of cooling tank 12 outlet at bottoms from causing reactor 2 pressure to increase phenomenon.
The disclosed utility model of the present invention is equipped with circulating cooling pipe 13 in the inside of cooling tank 12, and the effect of condensation can be better like this; Circulating cooling pipe can be used circulating cooling water pipe.Below cooling tank bottom opening 14 places, can be provided with condensate liquid receiving tank 15.Make things convenient for the collection of condensate liquid.
The process that adopts the described device of the utility model to carry out the catalyst hydrothermal aging is: the dress agent mouth 1 of catalyst on fixed fluidized-bed reactor blind flange 8 packed in the fixed fluidized-bed reactor 2; The aging temperature of fixed fluidized-bed reactor is by 3 heating of heating tile; The temperature of reactor is made as 400-800 ℃, and the thermocouple 4 that inserts reactor 2 centers is used to measure the actual aging temperature of catalyst; During hydrothermal aging, first bubbling air when treating that temperature reaches design temperature, feeds water vapour from unloading agent mouth 1, cuts off air simultaneously, and water vapour gets in the reactor by unloading agent mouth 1, and ageing time is 4～17 hours.Water vapour contacts the back and gets into cooling tank 12 coolings through the filter 5 that external packets is wrapped with easy-to-dismount heating tape 9 with catalyst, cooled acid water gets into condensed water receiving tank 15 through the bottom opening 14 of cooling tank 12.After reaching ageing time, stop to feed water vapour and switch to air, stop heating.Question response device 2 temperature are reduced to room temperature, open reactor 2 bottoms and unload agent mouth 1, take out the hydrothermal aging catalyst sample; The catalyst hydrothermal aging is accomplished.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model will be dismantled the problem of whole reactor, when the filter in the existing technology takes place to stop up when the filter that has solved the fixed fluidized-bed reactor top take place to stop up; Will be earlier the heating tile be opened, the blind flange of reactor head is unloaded, also need the core component temperature thermocouple be taken out simultaneously; Waste time and energy, and adopt the described device of this utility model, the back takes place to stop up and only need heating tape 9 be taken off in filter 5; Directly unloading filter 5 gets final product with conduit 10; Only need a people to accomplish, save manpower, efficient is high.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model has solved the etching problem of fixed fluidized-bed reactor outlet conduit.Existing technological middle filtrator outlet is direct-connected to be water condenser, directly the acid water steam in the reactor is condensed into water, carries a large amount of acidic materials HCl in the condensed water, and NOx, SO2 at the local pipeline that condensed water is arranged etching problem take place very easily.Adopt the described device of this utility model, the high-temperature acidic water vapour is heated in pipeline is with 9 heating noncondensing for water, and in cooling tank 12, just is condensed into water, has reduced outlet generation corrosion failure and the device shut-down problem that causes suddenly.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model has solved the dust blockage problem of reactor outlet.In the existing technology; The steam that carries catalyst dust is condensed into water in the reactor outlet conduit; The catalyst fines that carries also settles down simultaneously; Be condensed into the local a large amount of deposition of water at pipeline, very easily cause line clogging and reactor pressure is increased, cause the hydrothermal aging data unstable with the device unsafe problems.Adopt the described device of this utility model, carry steam not sedimentation in the reactor outlet conduit of catalyst dust, if cooling tank 12 bottoms are stopped up, steam can also be discharged through safety top hole 11, and security performance increases greatly.Safety vent 11 opening diameters are 1～10mm.The bottom opening 14 of cooling tank 12, diameter are 0.5～2cm.
The described a kind of hydrothermal aging device that is used for catalytic cracking catalyst of the utility model can carry out the super stabilizing processing of molecular sieve or catalytic cracking catalyst, the hydrothermal aging of catalyst is handled; The maintenance efficiency of experimental rig is high, good reproducibility, has prolonged maintenance period greatly.This device can be used for hydrothermal aging and handles the acid strong and less catalytic cracking catalyst of granularity, and the device top takes place to stop up and the possibility of acid corrosion reduces greatly.
The described a kind of hydrothermal aging apparatus structure that is used for catalytic cracking catalyst of the utility model is compact to design, and high insulating effect is compared with existing hydrothermal aging, has greatly improved efficient.
Description of drawings:
Fig. 1 is the described hydrothermal aging device that is used for catalytic cracking catalyst of the utility model.
In Fig. 1,1-steam entry/unload the agent mouth, the 2-reactor, 3-heats tile, 4-thermocouple; The 5-filter, 6-heat-preservation cotton, 7-dress agent mouth, 8-blind flange, 9-heating tape; The 10-conduit, 11-safety vent, 12-cooling tank, 13-circulating cooling pipe, 14-bottom opening; 15-condensate liquid receiving tank, I-pre lift zone, II-fluidisation section, III-settling section.
The specific embodiment
Embodiments of the invention further specify effect of the present invention but the present invention is not limited only to embodiment.
The raw material of catalyst and specification: the catalyst of treating hydrothermal aging adopts fresh dose of the LBO-16 catalytic cracking catalyst that Catalyst Factory of Lanzhou Petrochemical Company produces.
The embodiment of 1 pair of the utility model is elaborated with reference to the accompanying drawings.
Select catalytic cracking catalyst 2～6Kg for use; Preferred 5Kg; The dress agent mouth 1 of catalyst on fixed fluidized-bed reactor blind flange 8 packed in the fixed fluidized-bed reactor 2; The aging temperature of fixed fluidized-bed reactor is by 3 heating of heating tile, and the temperature of reactor is made as 800 ℃., the thermocouple 4 that inserts reactor 2 centers is used to measure the actual aging temperature of catalyst.
During hydrothermal aging, first bubbling air when treating that temperature reaches design temperature, feeds water vapour from unloading agent mouth 1, cuts off air simultaneously, and water vapour gets in the reactor by unloading agent mouth 1.Aging catalytic cracking catalyst sample under 800 ℃ of temperature, aging 10 hours.Water vapour contacts the back and gets into cooling tank 12 coolings through the filter 5 that external packets is wrapped with easy-to-dismount heating tape 9 with catalyst, cooled acid water gets into condensed water receiving tank 15 through the bottom opening 14 of cooling tank 12.The top of cooling tank is provided with safety vent 11, and safety vent 11 opening diameters are 2mm.Bottom opening 14 diameters of cooling tank 12 are 1cm.Prevent that the obstruction of cooling tank 12 outlet at bottoms from causing reactor 2 pressure to increase phenomenon.Circulating cooling water pipe 13 is equipped with in the inside of cooling tank 12.
After reaching ageing time, stop to feed water vapour and switch to air, stop heating.
Present embodiment is explained same catalytic cracking catalyst different batches hydrothermal aging, and aging back micro-activity differs less than ± 1.0.
Adopt catalytic cracking catalyst hydrothermal aging device shown in Figure 1, catalyst adopts fresh dose of LBO-16, to fresh dose of hydrothermal aging of LBO-16 four times; Pump capacity is controlled at 12g/min; Water vapour gasification burner temperature is 700 ℃, and temperature of reactor is 800 ℃, and the hydrothermal aging time is 10 hours.
Micro anti-evaluation result behind the LBO-16 catalyst hydrothermal aging
| The catalyst title | LBO-16-1 | LBO-16-2 | LBO-16-3 | LBO-16-4 |
| Micro-activity | 68.4 | 67.9 | 68.7 | 68.2 |
This utility model and original compared with techniques are adopted in present embodiment explanation, the prolongation of its device maintenance period, reduced and safeguarded manpower.
Maintenance period with original compared with techniques the utility model
| Original technology | The utility | |
| Maintenance period | ||
| 2 months | 6 months | |
| Safeguard |
2 |
1 people |
Claims (10)
1. hydrothermal aging device that is used for catalytic cracking catalyst; Comprise fixed fluidized-bed reactor (2), heating tile (3); Heating tile (3) is positioned at the outside of reactor (2); Fixed fluidized-bed reactor is by heating tile heating, and the top of fixed fluidized-bed reactor is provided with flange and blind flange (8), and the bottom of fixed fluidized-bed reactor is provided with steam entry/unload agent mouth (1); Fixed fluidized-bed reactor is divided into pre lift zone I, fluidisation section II and settling section III; It is characterized in that being horizontally disposed with filter (5) in fixed fluidized-bed reactor settling section one side; The outside of fixed fluidized-bed reactor is provided with cooling tank (12), and filter is connected by conduit (10) with cooling tank, and the conduit external packets is wrapped with easy-to-dismount heating tape (9); The bottom opening of cooling tank (14), bottom opening can by-pass cock.
2. device according to claim 1; The blind flange (8) that it is characterized in that fixed fluidized-bed reactor is provided with catalyst dress agent mouth (7) and thermocouple (4); The thermoinduction position of thermocouple is positioned at the central axis of reactor, is used to measure the actual aging temperature of catalyst.
3. device according to claim 1 is characterized in that blind flange and reactor water plane section for circular, the maximum equal diameters of the diameter of blind flange (8) and reactor (2).
4. device according to claim 1 is characterized in that blind flange (8) top is placed with heat-preservation cotton (6).
5. device according to claim 1 is characterized in that the top of cooling tank (12) is provided with safety vent (11).
6. device according to claim 5 is characterized in that safety vent (11) opening diameter is 1～10mm.
7. device according to claim 1, the diameter that it is characterized in that bottom opening (14) is 0.5～2cm.
8. device according to claim 1 is characterized in that being provided with condensate liquid receiving tank (15) in cooling tank bottom opening (14) below.
9. device according to claim 1 is characterized in that circulating cooling pipe (13) is equipped with in the inside of cooling tank (12).
10. device according to claim 9 is characterized in that circulating cooling pipe (13) is a circulating cooling water pipe.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012200389266U CN202527185U (en) | 2012-02-07 | 2012-02-07 | Hydrothermal aging device for catalytically cracking catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012200389266U CN202527185U (en) | 2012-02-07 | 2012-02-07 | Hydrothermal aging device for catalytically cracking catalyst |
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| CN2012200389266U Expired - Fee Related CN202527185U (en) | 2012-02-07 | 2012-02-07 | Hydrothermal aging device for catalytically cracking catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056580A (en) * | 2013-03-18 | 2014-09-24 | 中国石油化工股份有限公司 | Fixed fluidized bed reactor and application thereof |
| CN104056581A (en) * | 2013-03-18 | 2014-09-24 | 中国石油化工股份有限公司 | Fixed fluidized bed reactor and application thereof |
| CN106841506A (en) * | 2015-12-07 | 2017-06-13 | 中国石油天然气股份有限公司 | A kind of catalyst hydrothermal aging device and aging method |
| CN114797690A (en) * | 2022-05-24 | 2022-07-29 | 清远市鑫辉化工有限公司 | Novel white carbon black modification equipment |
-
2012
- 2012-02-07 CN CN2012200389266U patent/CN202527185U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056580A (en) * | 2013-03-18 | 2014-09-24 | 中国石油化工股份有限公司 | Fixed fluidized bed reactor and application thereof |
| CN104056581A (en) * | 2013-03-18 | 2014-09-24 | 中国石油化工股份有限公司 | Fixed fluidized bed reactor and application thereof |
| CN104056580B (en) * | 2013-03-18 | 2016-03-02 | 中国石油化工股份有限公司 | A kind of fixed fluidized-bed reactor and application thereof |
| CN104056581B (en) * | 2013-03-18 | 2016-03-02 | 中国石油化工股份有限公司 | A kind of fixed fluidized-bed reactor and application thereof |
| CN106841506A (en) * | 2015-12-07 | 2017-06-13 | 中国石油天然气股份有限公司 | A kind of catalyst hydrothermal aging device and aging method |
| CN106841506B (en) * | 2015-12-07 | 2019-07-05 | 中国石油天然气股份有限公司 | A kind of catalyst hydrothermal aging device and aging method |
| CN114797690A (en) * | 2022-05-24 | 2022-07-29 | 清远市鑫辉化工有限公司 | Novel white carbon black modification equipment |
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Granted publication date: 20121114 Termination date: 20210207 |
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