CN101172220A - Three-phase fluidized bed reactor - Google Patents
Three-phase fluidized bed reactor Download PDFInfo
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- CN101172220A CN101172220A CNA2006101341545A CN200610134154A CN101172220A CN 101172220 A CN101172220 A CN 101172220A CN A2006101341545 A CNA2006101341545 A CN A2006101341545A CN 200610134154 A CN200610134154 A CN 200610134154A CN 101172220 A CN101172220 A CN 101172220A
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Abstract
The invention discloses an improved three-phase fluidized layer reactor, which consists of a reactor casing body and a three-phase separator positioned at the inner upper part of the casing body, wherein, the three-phase separator is composed of the inner cylinders and outer cylinders of two concentric cylinders with different inner diameters, a float tube arranged on the outer cylinder, and the inner wall of the reactor casing body. An upper limiting apparatus and a lower limiting apparatus are arranged on the reactor casing body, and the three-phase separator is positioned between the upper limiting apparatus and the lower limiting apparatus. The reactor is mainly suitable for the chemical reaction of different kinds of liquid and gas substances under the circumstance of contacting with solid particles, and has the advantages of large catalyst inventory, high utilization rate of the reactor, and high stability of operation.
Description
Technical field
The present invention relates to a kind of gas-liquid-solid three-phase fluidized bed reactor, specifically be used for variety classes liquids and gases material and contacting a kind of three-phase fluidized bed reactor that carries out chemical reaction under the situation with solid particle.
Background technology
Fluidized bed reactor is the gas, liquid, solid three phase fluidized beds, can handle weight, the inferior feedstock oil of high metal, high asphalt content.Have pressure little, uniformity of temperature profile is fallen, can keep whole service cycle the inner catalyst activity constant, can on-stream adding fresh catalyst and take out characteristics such as dead catalyst.
Described typical ebullated bed technology among the US Re 25,770, but this process has the following disadvantages in actual applications: the catalyst in reactor reserve is less, and the space reactor utilization rate is low; Oil circulating pump maintaining expense is higher, in case and oil circulating pump work is not normal and damage, will cause catalyst to sink to assembling, the result forces device to be forced to stop work; Fluid product overstand under the on-catalytic hydroconversion condition in the reactor at high temperature is easy to carry out the coking of secondary heat scission reaction and reduces product quality.
Chinese patent CN02109404.7 has introduced a kind of novel fluidized bed reactor, compares with typical fluidized bed reactor, has characteristics such as simple in structure, processing ease and reactor utilization rate height.But owing to use particle diameter is the microspherical catalyst of 0.1～0.2mm, and catalyst is taken reactor out of with reaction oil gas easily.Guarantee the normal stable operation of this kind fluidized bed reactor, key is to require to assemble three phase separator efficiently on reactor top, the catalyst separation that reaction oil gas carries is come out, avoid catalyst from reactor, to take out of causing damage and downstream unit is impacted.The three phase separator of this patent introduction can reach separating effect preferably under normal operation, the catalyst drag-out can be controlled at below the 20wppm.But find in actual use, if oil inlet quantity or recycle hydrogen amount instability, perhaps reactor oil extraction or exhaust line are not smooth, can cause the fluctuation of liquid level in the reactor, in case surpass the top of three phase separator urceolus, three phase separator will be ineffective, causes taking out of in a large number of catalyst, not only cause the loss of catalyst, also can cause adverse effect downstream unit.In addition, the reactor that this patent is introduced is after using a period of time, the catalyst that is separated by three phase separator can be attached on the catalyst feed opening, slowly feed opening is stopped up, the catalyst that causes separating can not return reaction zone by feed opening smoothly, thereby the drag-out of catalyst is increased greatly, can not guarantee normal stable running, finally be forced to shut-down (breakdown) mainteance.
Summary of the invention
The problem to be solved in the present invention is to overcome the defective that prior art exists, and a kind of three-phase fluidized bed reactor that can operation steady in a long-term is provided.This structure of reactor is simple, processing ease, and operating flexibility is big, can satisfy the needs of long period steady running.
Fluidized bed reactor provided by the invention comprises the cylinder reactor housing and the three phase separator that is positioned at the housing internal upper part perpendicular to ground, described three phase separator is to be made of together with the inwall of reactor shell internal diameter different two concentric drums inner cores, urceolus, described reactor shell is provided with upper limit device and lower retainer, described three phase separator places between upper limit device and the lower retainer, the upper end of described urceolus is provided with floating drum, and three phase separator can be adjusted up and down between upper limit device and lower retainer along with the fluctuation of liquid level like this.
The concrete structure of three-phase fluidized bed reactor of the present invention is:
Be provided with feed(raw material)inlet and gas-liquid distributor in the bottom of described reactor shell, described gas-liquid distributor can be selected for use and anyly can make gas or the equally distributed structure of liquid stream, for example can adopt bubble cap or distributor pipe structure; Be provided with the gas products outlet at the reactor shell top, the top shell wall is provided with product offtake, and the gas and the liquid that are used for reaction is generated are derived; Described three phase separator is arranged in the housing internal upper part space, descends two ends to be respectively arranged with upper limit device and lower retainer thereon.Described stop can generally be at least 3 for the shape that is fit to arbitrarily, is generally 3-6, and is in same horizontal plane, is evenly distributed on the reactor wall.The upper limit device should be greater than the distance of three phase separator urceolus to reactor wall along reactor length radially, and lower retainer should be greater than the distance of three phase separator inner core lower openings to reactor wall along reactor length radially.
Described three phase separator is to be made of jointly together with the reactor shell inwall two different concentric drums of internal diameter, inner diameter of steel flue should be less than the urceolus diameter, whole up and down openings of inner core and urceolus, wherein the top of urceolus connects an annular floating drum, floating drum lower horizontal tangent plane will be higher than the horizontal section on the top of inner core, floating drum upper level tangent plane position should be lower than its horizontal level at vertical corresponding reactor shell top; The lower openings of described inner core is the no tip circle tapered opening that amplify the bottom, the base diameter of this cone shaped opening should be less than the internal diameter of reactor shell, and the horizontal level of set cone shaped opening bottom, inner core bottom should be lower than the horizontal level of the set open bottom in described urceolus bottom.
Above described lower retainer, decoking device can also be set, to remove particles such as catalyst that the separator feed opening sticks, coking material.Described decoking device is annular or infundibulate, and its outside diameter equals reactor inside diameter, and interior circular diameter is greater than the base diameter of inner core lower cone shape opening.In the decoking device horizontal plane at circle place apart from the vertical range distance of lower retainer less than floating drum upper level tangent plane apart from the upper limit device vertical range.Described decoking device is fixed by welding on the reactor wall, is generally 90 °～45 ° with the angle of reactor wall, is preferably 60 °.
The lower openings of the urceolus of described three phase separator also can be the no tip circle tapered opening that amplify the bottom, and the base diameter of this cone shaped opening also should be less than the internal diameter of described reactor shell.The cross section of described floating drum can be circle or polygon, and the tie point of urceolus top and floating drum can be the middle part of floating drum, or other position of bottom.The outside diameter of floating drum is less than the internal diameter of reactor shell.
Described gas discharge outlet operated by rotary motion is in the reactor head center.
Described liquid outlet generally can be arranged on reactor top near the end socket place, and the height of the floating drum upper level tangent plane of its centre-to-centre spacing three phase separator generally should be 10% of separator height at least, is preferably 20%～50%.The present invention reaches the vertical range of the cone shaped opening bottom level position that floating drum upper level tangent plane that the following stated phase separator height is meant phase separator amplifies to the inner core bottom herein, and described reactor shell height is meant the distance between the horizontal tangent of described reactor shell top end socket and bottom bulkhead.In general, the scope of the blade diameter length ratio of reactor shell can be between 0.01～0.1.
In order in course of reaction or after the reaction end, to replace catalyst easily, on reactor shell, also be provided with the online displacement auxiliary equipment of catalyst, catalyst for example is set at the reactor shell top adds pipe, the bottom is provided with the catalyst discharge pipe.Described catalyst exchange system and using method can be any suitable equipment or method, for example can carry out with reference to U.S. Pat 3398085 or the described method of US4398852.
The height of described three phase separator generally accounts for 5% of height for reactor at least, is generally 5%～35%, is preferably 7%～25%.
The floating drum upper level tangent plane of described three phase separator generally should be 10% of separator height at least apart from reactor top end socket horizontal section distance, is preferably 15%～25%.
Described three phase separator floating drum volume will guarantee separator can be floated when it immerses in the oil, and the part that this moment, floating drum immersed in the oil generally accounts for 50% of floating drum volume, is preferably 50%～80%.
The cross section of described floating drum can be circle or arbitrary polygon.
Described three phase separator is seated on the lower retainer under the effect of gravity when the reactor normal running, and the distance of its floating drum lower horizontal tangent plane and liquid level should be 5% of separator height at least, is preferably 5%～15%.When three phase separator rises under buoyancy, the extreme higher position that upper limit device control three phase separator rises, the buffer size on this position and three phase separator top has relation.When three phase separator was positioned at minimum point, the distance of floating drum upper level tangent plane and upper limit device generally was at least 10% of separator height, is preferably 10%～30%.When three phase separator rose to highest point, the catalyst that deposits to the catalyst feed opening can not extracted out from liquid outlet like this.
The height of the cone shaped opening that amplify the set bottom in described inner core and urceolus bottom should be 10% of separator height at least, is preferably 15%～75%.The height of indication cone shaped opening is meant horizontal level height poor of the horizontal level of inner core or urceolus and cone shaped opening junction and described cone shaped opening bottom herein.
Described inner core constitutes the central tube of three phase separator, annulus between inner core and the urceolus is formed the baffling tube of this three phase separator, annulus between urceolus and the reactor wall is the supernatant liquid product collecting region of this three phase separator, the cone shaped opening that amplify the bottom that described inner core bottom is provided with is the logistics introducing port, and the bottom of the cone shaped opening that amplify set bottom, described inner core bottom and the circular opening that reactor wall constitutes are the catalyst feed opening of this three phase separator.
Compared with prior art, the advantage of fluidized bed reactor of the present invention is:
(1) increased the operating flexibility of three phase separator, in reactor, can in time respond during level fluctuation, thereby guarantee that separator is in good working order all the time, guarantee the efficient separation of three phase separator to catalyst, the drag-out of catalyst can be reduced 60%～80%, avoid taking out of in a large number of catalyst.
(2) decoking device can be cleared up the catalyst feed opening under the device situation of not stopping work, and avoids catalyst and burnt grain to stop up causing behind the feed opening being forced to shut-down (breakdown) mainteance, the steady running of assurance device long period.
Description of drawings
Fig. 1 is the front view of reactor of the present invention.
Fig. 2 is the section plan view of reactor of the present invention, and wherein A-A is the vertical view of decoking device, and B-B is the vertical view of lower retainer.
Figure is the reactor front views of 3 reactors of the present invention when three phase separator rises to highest point.
The specific embodiment
For further setting forth concrete feature of the present invention, will be illustrated in conjunction with the accompanying drawings.
In conjunction with the accompanying drawings 1, the architectural feature and the operation principle of this reactor are as follows:
Reaction raw materials mixes the back and enters reactor by charging aperture 1, and uniformly by beds 16, the catalyst loading amount in the reactor shell 3 is at least 35% of reactor volume, is generally 40%～70%, is preferably 50%～60% behind gas-liquid distributor 2.Under the rolling action of gas-liquid, beds expand into certain height, and its back volume that expands is bigger by 20%～70% than its static volume usually.Gas and liquid charging stock are finished chemical reaction in reaction zone, reacted oil gas is carried the part catalyst granules secretly and is entered three phase separator 11, carrying out gas-liquid-solid three-phase separates: gas at first is separated, gas discharge outlet 10 by reactor head is discharged reactor, the catalyst that separates returns reaction zone through catalyst feed opening 14, and the liquid stream that does not contain catalyst granules substantially enters next unit by liquid outlet 12.
Three phase separator 11 is to be made of jointly together with the inwall of reactor shell 3 internal diameter different two concentric drums inner cores 5, urceolus 6, the floating drum 7 that is connected on the urceolus.Inner core 5 constitutes the central tube of this three phase separator, annulus between inner core 5 and the urceolus 6 is formed the baffling tube of this three phase separator, annulus between urceolus 6 and reactor shell 3 inwalls is a supernatant liquid product collecting region, the cone shaped opening that amplify above-mentioned central tube bottom is the logistics introducing port, and the circular opening that this conical lower section opening part and reactor shell 3 inwalls constitute is the catalyst feed opening of this three phase separator.In addition, three phase separator 11 comprises that also a decoking device 13 is used to remove the particles such as catalyst that separator feed opening 14 sticks.
The separation process of three phase separator specifies as follows: logistics at first enters the central tube that three phase separator inner core 5 constitutes through separator central tube lower cone shape opening, when this logistics rises the open top of arrival central tube, bubble is being overflowed from liquid and is being gathered in reactor shell 3 tops because of its buoyancy, discharge reactor by gas discharge outlet 10, liquid-solid phase enters the baffling district between separator inner core 5 and the urceolus 6, the downward liquid sub-fraction of baffling enters the annulus between separator urceolus 6 and reactor shell 3 inwalls, constitute product liquid speed upwards (because this liquid speed is far below the critical speed that makes the catalyst granules fluidisation, so the downward solid particle of baffling is unlikely to be brought in the supernatant layer by liquid).A large amount of circulation fluids continues will to force catalyst to return reaction zone through feed opening 14 gaps of three phase separator 11 downwards; Because of circulation fluid has produced very big downward liquid speed in the feed opening cross section, can't go up string again, guarantee that supernatant layer does not have bubble agitation so the bubble of reactor limit wall is pressed close in its underpart.Fluid product is derived reactor by liquid outlet 12, realizes fully separating.Catalyst in the metathesis reactor housing 3 can add pipe 9 by the set catalyst in reactor shell 3 tops and add fresh catalyst if desired, and the set catalyst discharge pipe 17 in bottom draws off decaying catalyst.
If device occurs unusual, increase as oil inlet quantity or recycle hydrogen amount suddenly, perhaps reactor discharge opeing or exhaust line are not smooth, can cause the rising of liquid level in the reactor, when rising to, liquid level floods 50% when above of floating drum 7, this three phase separator will be under the buoyancy that floating drum produces along with reactor in liquid level rising and raise, the liquid of avoiding carrying secretly the part catalyst directly flows through the top of floating drum 7, guarantees the separating effect of separator.After build-up of fluid in the reactor was normal, three phase separator fell back on the lower retainer 4 again.
If after the long-time running of device,, will carry out online decoking because the obstruction of catalyst feed opening 14 causes the increase of catalyst drag-out.Concrete operation method is as follows: the air inflow of reactor is brought up to 105% of normal air inflow, be preferably 105%～125%, this moment, reactor was interior because the increase of tolerance, volumetric expansion, liquid can not in time be discharged from reactor, liquid level rises in the reactor, the drive three phase separator moves upward, because the restriction of upper limit device 8, the floating drum of three phase separator just stops to rise when rising near upper limit device 8, recover normal with air inflow this moment, and three phase separator falls back to again on the lower retainer 4.In the process that three phase separator moves up and down, clear up by 13 pairs of feed openings 14 of decoking device, so particles such as catalyst that just feed opening 14 can be sticked several times repeatedly and Jiao Li are cleaned out.
Further the structure and the result of use of reactor of the present invention are described below in conjunction with embodiment.
Embodiment-1
Selection according to three phase separator size of the present invention, carried out the medium-sized reactor cold model experiment of three phase separator ebullated bed, medium-sized cold model unit is of a size of: the internal diameter=160mm of reactor shell, height=the 3000mm of reactor shell, housing dischargeable capacity 60L, separator height=380mm, separator central tube column part diameter=92mm, base diameter=the 144mm of inner core lower taper opening, height=the 41mm of inner core bottom conical section, urceolus column part diameter=128mm, base diameter=the 138mm of its tapering part opening, height=the 64mm of tapering part, the floating drum cross section is circular, diameter=100mm, its lower edge links to each other with the top of separator urceolus, difference in height=the 138mm of floating drum upper level tangent plane and inner core upper opening position, the urceolus upper opening is higher than the inner core upper opening, the bottom position of urceolus lower taper opening is higher than the bottom position of inner core lower taper opening, both difference in height=38mm, the vertical range of separator urceolus upper opening and reactor shell top tangent line is 200mm, and the vertical range of fluid product tube center distance reactor head tangent line is 338mm.Select for use aviation kerosine as liquid medium, oil inlet quantity is 40～100L/hr; Gas phase is selected nitrogen for use, and air inflow is 2～3Nm
3/ hr.It is the microspherical catalyst of 0.1～0.2mm that solid phase is selected particle diameter for use, and the catalyst buildup reserve is 50% of a reactor dischargeable capacity.Result of the test sees Table 1.
Find out from result of the test, the catalyst buildup reserve up to 50% situation under, inlet amount changes in quite wide scope, the catalyst drag-out is all extremely low, three-phase fluidization is even.Three phase separator still can keep very high separative efficiency under the situation that air inflow increases suddenly.
Embodiment-2
On the cold model experiment basis, on the 60L middle-scale device, carried out reduced crude HDM test in the sand.Wherein the size of reactor is identical with embodiment 1, experimental condition and the results are shown in Table 2.
Embodiment-3
On the cold model experiment basis, on the 60L middle-scale device, carried out reduced crude HDM test in the sand.Wherein the size of reactor is identical with embodiment 1.It is very fast to find after 1200 hours that the catalyst drag-out increases, and then the three phase separator feed opening is carried out coke cleaning treatment, and the drag-out of decoking rear catalyst returns to range of normal value.Experimental condition and the results are shown in Table 3.
The relation of table 1 60L cold model unit oil inlet quantity, air inflow and catalyst drag-out
Annotate: 6 and 7 air inflow changes in a short period of time, is used to examine or check the adaptability to changes of three phase separator.
1000 hours result of the tests of the medium-sized hot-die device of table 2 60L
2000 hours result of the tests of the medium-sized hot-die device of table 3 60L
Claims (12)
1. three-phase fluidized bed reactor, comprise reactor shell (3) and be positioned at the three phase separator (11) of described housing internal upper part perpendicular to ground, it is characterized in that, described three phase separator is to be made of together with the inwall of reactor shell (3) different two the concentric drums inner cores (5) of internal diameter, urceolus (6), be provided with floating drum (7) in the upper end of described urceolus, be respectively arranged with upper limit device (8) and lower retainer (4) at the two ends up and down of three phase separator, three phase separator can move between upper limit device and lower retainer.
2. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that the volume of described floating drum (7) satisfies it and immerses in oil and just separator can be floated at 50%～80% o'clock.
3. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that, whole up and down openings of described inner core (5) and urceolus (6), the lower openings of inner core (5) is the no tip circle tapered opening that amplify the bottom, and its horizontal level is lower than the horizontal level of the set open bottom in described urceolus bottom.
4. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that the lower openings of described urceolus (6) is the no tip circle tapered opening that amplify the bottom.
5. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that described floating drum (7) lower horizontal tangent plane will be higher than the horizontal section on the top of inner core (5).
6. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that the cross section of described floating drum (7) is circle or polygon, the tie point of urceolus top and floating drum is at the middle part of floating drum or other position of bottom.
7. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that the height of described three phase separator (11) accounts for 5% of reactor shell (3) height at least.
8. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that the height of the cone shaped opening that amplify set bottom, described inner core (5) bottom is at least 10% of phase separator (11) height.
9. according to the described three-phase fluidized bed reactor of claim 1, the horizontal level that it is characterized in that the set no tip circle conical lower portion in described inner core (5) bottom is lower than the residing horizontal level in urceolus (6) lower openings bottom, and its difference in height accounts for 5% of described phase separator (11) height at least.
10. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that the upper opening plane of living in of described urceolus (6) and the vertical range on inner core (5) upper opening plane of living in account for 20% of described phase separator (11) height at least.
11. according to the described three-phase fluidized bed reactor of claim 1, it is characterized in that being provided with decoking device (13) in the top of described lower retainer (4), described decoking device (13) is annular or infundibulate, the angle of itself and reactor wall is 90 °～45 °, by being fixedly welded on the reactor shell.
12. according to the described three-phase fluidized bed reactor of claim 11, it is characterized in that the base diameter of the interior circular diameter of described decoking device greater than inner core lower cone shape opening, in it horizontal plane at circle place apart from the vertical range distance of lower retainer less than floating drum upper level tangent plane apart from the upper limit device vertical range.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102451652A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Boiling-bed reactor |
| CN103100355A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Boiling bed reactor and applications thereof |
| CN106277690A (en) * | 2015-05-11 | 2017-01-04 | 河南昂西特热能技术有限公司 | A kind of sequential continuous thermal hydrolysis reaction unit |
| CN107297186A (en) * | 2017-07-24 | 2017-10-27 | 上海英保能源化工科技有限公司 | A kind of boiling bed hydrogenation reaction system and boiling bed hydrogenation method |
| CN109603691A (en) * | 2018-11-23 | 2019-04-12 | 聊城市鲁西化工工程设计有限责任公司 | A kind of hydration reactor and adjusting method of adjustable mixture separated space |
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| CN114981391A (en) * | 2020-01-13 | 2022-08-30 | 凯洛格·布朗及鲁特有限公司 | Slurry phase reactor with internal gas-liquid separator |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102451652A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Boiling-bed reactor |
| CN102451652B (en) * | 2010-10-15 | 2014-01-01 | 中国石油化工股份有限公司 | Boiling-bed reactor |
| CN103100355A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Boiling bed reactor and applications thereof |
| CN103100355B (en) * | 2011-11-10 | 2015-04-15 | 中国石油化工股份有限公司 | Boiling bed reactor and applications thereof |
| CN106277690A (en) * | 2015-05-11 | 2017-01-04 | 河南昂西特热能技术有限公司 | A kind of sequential continuous thermal hydrolysis reaction unit |
| CN107297186A (en) * | 2017-07-24 | 2017-10-27 | 上海英保能源化工科技有限公司 | A kind of boiling bed hydrogenation reaction system and boiling bed hydrogenation method |
| CN109603691A (en) * | 2018-11-23 | 2019-04-12 | 聊城市鲁西化工工程设计有限责任公司 | A kind of hydration reactor and adjusting method of adjustable mixture separated space |
| CN109603691B (en) * | 2018-11-23 | 2021-10-15 | 聊城市鲁西化工工程设计有限责任公司 | Hydration reactor capable of adjusting mixture separation space and adjusting method |
| CN112745958A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Desulfurized alcohol alkali liquor regeneration device, liquefied gas desulfurized alcohol system and alkali liquor regeneration method |
| CN112745958B (en) * | 2019-10-31 | 2022-12-13 | 中国石油化工股份有限公司 | Desulfurized alcohol alkali liquor regeneration device, liquefied gas desulfurized alcohol system and alkali liquor regeneration method |
| CN114981391A (en) * | 2020-01-13 | 2022-08-30 | 凯洛格·布朗及鲁特有限公司 | Slurry phase reactor with internal gas-liquid separator |
| CN114981391B (en) * | 2020-01-13 | 2024-03-26 | 凯洛格·布朗及鲁特有限公司 | Slurry phase reactor with internal gas-liquid separator |
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