CN101376092B - Novel bubbling bed reactor - Google Patents
Novel bubbling bed reactor Download PDFInfo
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- CN101376092B CN101376092B CN200710012680A CN200710012680A CN101376092B CN 101376092 B CN101376092 B CN 101376092B CN 200710012680 A CN200710012680 A CN 200710012680A CN 200710012680 A CN200710012680 A CN 200710012680A CN 101376092 B CN101376092 B CN 101376092B
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Abstract
The invention discloses a new fluidized bed hydrogenation reactor. The fluidized bed hydrogenation reactor of the invention comprises a cylinder-shaped reactor shell perpendicular to the ground, a three-phase separator arranged at the upper part in the reactor shell and a guiding structure arranged at the middle upper part of the reactor. The guiding structure is an annular convex structure arranged on the inner wall of the reactor and has the lengthwise section of a trapezoid or an arc along the axle of the reactor. The combination of the guiding structure and the three-phase separator increases the operating flexibility of the three-phase separator, and ensures the high-efficiency separation on the three-phase separator, thereby greatly reducing the carrying amount of catalyst. The fluidized bed hydrogenation reactor of the invention can be applied to the chemical reactions between different liquids or gases and solid grains under the condition of contacting, and is characterized bylarge catalyst inventory, high reactor utility ratio, etc.
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 improved three-phase fluidized bed hydrogenation 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 the internal structure of requirement appropriate design reactor, make it to match with the three phase separator efficiently on 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 feed opening and the reactor outlet position operation elasticity of the three phase separator that this patent is introduced are little, the catalyst that is separated by three phase separator can be attached on the catalyst feed opening and the feed opening place has the phenomenon of collaborating to take place easily, influence the separating effect of three phase separator, and the easy clog downstream device of the catalyst of taking out of is unfavorable for the long-term operation of device.
Summary of the invention
At the problem that prior art exists, the invention provides a kind of novel bubbling bed reactor that can operation steady in a long-term.This structure of reactor is simple, processing ease, and operating flexibility is big, can satisfy the needs of long period steady running.
Boiling bed hydrogenation reactor provided by the invention comprises the guide frame of middle and upper part in cylinder reactor housing perpendicular to ground, the housing and is positioned at the three phase separator of housing internal upper part, described guide frame is the annular protrusion structure that is arranged at reactor wall, and its longitudinal section along reactor axis is trapezoidal or arc.
The concrete structure of novel bubbling 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.Be provided with gas vent at the reactor shell top, the top shell wall is provided with liquid outlet, 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, comprises two concentric drums that internal diameter is different: inner core and urceolus.The whole openings in two ends up and down of described inner core and urceolus, the upper end open of urceolus is higher than the upper end open of inner core, and the lower ending opening of urceolus also should be higher than the lower ending opening of inner core.The bottom of described inner core is a taper diffuser, and the opening of this diffuser (being the lower ending opening of inner core) diameter is less than the internal diameter of reactor; The bottom of described urceolus is similarly a taper diffuser, and the opening of this diffuser (being the lower ending opening of urceolus) diameter also should be less than the internal diameter of reactor.
The inner core of described three phase separator constitutes the central tube of separator, annulus between inner core and the urceolus is formed the baffling tube of three phase separator, annulus between urceolus and the reactor wall is the supernatant liquid product collecting region of this three phase separator, the lower ending opening of described inner core is the logistics introducing port, the circular opening that the lower ending opening of inner core and reactor wall constitute is the catalyst feed opening of this three phase separator, and isolated solia particle catalyst turns back in the beds from here again.
The concrete size and the relative position of described each building block of three phase separator, all can be determined by calculating or simple test according to specific requirements such as employed catalyst size, reactor for treatment amount, reaction condition and separating effects, perhaps can be determined with reference to the patent CN02109404.7 of application before the applicant by this area designer.
Described guide frame is positioned at the reactor middle and upper part, the three phase separator of next-door neighbour top.Guide frame is the annular protrusion structure that is arranged at the reactor shell inwall, and its longitudinal section along reactor axis is trapezoidal or arc.The trapezoidal stringcourse of the guide frame of next-door neighbour's three phase separator one side or the tangent line at arc and reactor wall intersection point place and the angle that reactor wall forms are called cone of coverage, and this cone of coverage should be acute angle, preferably less than 60 degree; A side on the other side promptly is called angle of friction away from the angle that the tangent line and the reactor wall at the trapezoidal stringcourse of three phase separator or arc and reactor wall intersection point place forms, and this angle of friction also be an acute angle, preferably spends less than 60.The diameter of the targeting port that described guide frame surrounds is between the urceolus diameter and inner diameter of steel flue of three phase separator.Inner diameter of steel flue described here and urceolus diameter all are meant the diameter of inner core cylindrical section and urceolus cylindrical section.
Described gas discharge outlet generally is located at the reactor head center.
For isolated supernatant liquid is discharged reactor, the liquid outlet operated by rotary motion is on the top of reactor shell wall, and its position should be between the upper end open and lower ending opening of urceolus.
The top of described three phase separator also should be provided with certain cushion space, and the gaseous product after being separated is discharged reactor in this enrichment and from gas discharge outlet.
In general, the blade diameter length ratio scope of reactor is between 0.01～0.1.
Fluidized bed reactor of the present invention also comprises at least one parts and at least one parts toward described reactor fresh makeup catalyst from described reactor discharge catalyst usually.The parts of described fresh makeup catalyst are arranged at the position of described reactor head usually, and the parts of described discharge catalyst are usually located near the described reactor bottom.Catalyst for example is set at the reactor shell top adds pipe, and the catalyst discharge pipe is set in the bottom.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.
For make reaction raw materials in reactor with the catalyst even contact, generally also should distribution grid be set in the bottom in the described cylinder reactor housing, distribution grid can be selected for use and anyly can make gas or the equally distributed structure of liquid stream, for example can adopt the bubble cap structure.
Compared with prior art, the advantage of boiling bed hydrogenation reactor of the present invention is:
(1) reactor content outlet and three phase separator and guide frame combine, more increased the operating flexibility of three phase separator, guarantee the efficient separation of three phase separator, significantly reduced the drag-out of catalyst, avoid taking out of in a large number of catalyst catalyst.
(2) increased guide frame, can suitably reduce the position of product export mouth, reduced internal circulating load, prevented the generation of condensation coking reaction at the lower high-temperature region liquid stream of catalyst concn.
(3) increase guide frame, can suitably amplify the size of three phase separator feed opening, helped the smooth return catalizer bed of isolated catalyst, can prevent effectively that simultaneously gas from going here and there from feed opening, influenced separating effect.
Description of drawings
Fig. 1 is the structural representation of a kind of embodiment 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 guide frame.
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 reactor of the present invention are as follows:
Reaction raw materials mixes the back and enters reactor by charging aperture 1, and uniformly by beds 7, 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 logistics, 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 carry out hydrogenation reaction in reaction zone, reacted oil gas is carried the part catalyst granules secretly and is entered three phase separator 11 by the targeting port 8 that guide frame 4 surrounds, carrying out gas-liquid-solid three-phase separates: gas at first is separated, discharge reactor by gas discharge outlet 10, the catalyst that separates returns reaction zone through feed opening 13, and the supernatant liquid logistics that does not contain catalyst granules is substantially discharged reactors by liquid outlet 12.In order in time the catalyst of inactivation to be discharged reactor and fresh makeup catalyst, can add pipe 9 by the catalyst on reactor top and in reaction system, replenish fresh catalyst, and the part decaying catalyst can be discharged reaction system by the delivery pipe 14 of reactor lower part.
Guide frame 4 is trapezoidal along the longitudinal section of reactor axis, and cone of coverage and angle of friction are acute angle, preferably all less than 60 degree.Certainly guide frame 4 also can be arc or other suitable shapes along the longitudinal section of reactor axis.
Three phase separator 11 is to be made of jointly together with the inwall of reactor shell 3 the different concentric drums inner core 5 of internal diameter, urceolus 6.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 opening of above-mentioned central tube lower end diffuser is the logistics introducing port, and the circular opening that the opening of this diffuser and reactor shell 3 inwalls constitute is the catalyst feed opening.For baffling tube inner fluid speed is accelerated, improve separating effect, urceolus diffuser conical apex angle generally than inner core diffuser conical apex angle to 20 degree when young, preferably little 40～80 degree.
Further the structure and the result of use of reactor of the present invention are described below in conjunction with embodiment.
Embodiment-1
Structure according to boiling bed hydrogenation reactor 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 urceolus upper opening is higher than the inner core upper opening, and 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.The cone of coverage of annular guide frame is 20 °, and angle of friction is 28 °, and the targeting port diameter is 100mm.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.Promptly after having increased guide frame, further improve the separating effect of three phase separator, greatly reduced the drag-out of catalyst.
Embodiment-2
On the cold model experiment basis, on the 60L middle-scale device, carried out the test of isolated island reduced crude HDM.Wherein the size of reactor is identical with embodiment 1, experimental condition and the results are shown in Table 2.
Comparative example-1
This embodiment is the comparative example, and the basic structure of reactor is with embodiment 1, and difference is not to be provided with in the reactor guide frame.Reaction condition and test raw material be with embodiment 2, wherein concrete experimental condition and the results are shown in Table 2.
The relation of table 160L cold model unit oil inlet quantity, air inflow and catalyst drag-out
1000 hours result of the tests of the table medium-sized hot-die device of 260L
Claims (11)
1. novel bubbling bed reactor, described fluidized bed reactor comprises cylinder reactor housing and the three phase separator that is arranged in the housing internal upper part space, it is characterized in that, adjacent is provided with a guide frame below described three phase separator, described guide frame is the annular protrusion structure that is arranged at reactor wall, and guide frame is trapezoidal or arc along the longitudinal section of reactor axis.
2. fluidized bed reactor according to claim 1, it is characterized in that, the trapezoidal stringcourse of the guide frame of next-door neighbour's three phase separator one side or the tangent line at arc and reactor wall intersection point place and the cone of coverage that reactor wall forms are acute angle, and the angle of friction of a relative side with cone of coverage is an acute angle.
3. fluidized bed reactor according to claim 2 is characterized in that, described cone of coverage and angle of friction are all less than 60 degree.
4. fluidized bed reactor according to claim 1 is characterized in that, the diameter of the targeting port that described guide frame surrounds is between the urceolus diameter and inner diameter of steel flue of three phase separator.
5. fluidized bed reactor according to claim 1 is characterized in that, described three phase separator comprises two concentric drums inner cores and the urceolus that internal diameter is different, the whole openings in two ends up and down of described inner core and urceolus.
6. fluidized bed reactor according to claim 5 is characterized in that, the upper end open of described urceolus and lower ending opening are higher than the upper end open and the lower ending opening of inner core respectively.
7. fluidized bed reactor according to claim 5 is characterized in that, the lower end of described inner core is a taper diffuser, and the lower ending opening diameter of this diffuser is less than the internal diameter of reactor shell; The lower end of described urceolus is similarly a taper diffuser, and the lower ending opening diameter of this diffuser is less than the internal diameter of reactor shell.
8. fluidized bed reactor according to claim 1 is characterized in that, described reactor shell wall is provided with liquid outlet, and its position is between the upper end open and lower ending opening of urceolus.
9. fluidized bed reactor according to claim 1 is characterized in that, is provided with a cushion space above described three phase separator, and the gaseous product after being separated is discharged reactor in this enrichment and from gas discharge outlet.
10. fluidized bed reactor according to claim 7 is characterized in that, the conical apex angle of described urceolus diffuser than the conical apex angle of inner core diffuser to 20 degree when young.
11. fluidized bed reactor according to claim 10 is characterized in that, the conical apex angle of described urceolus diffuser is than little 40～80 degree of conical apex angle of inner core diffuser.
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| CN200710012680A CN101376092B (en) | 2007-08-27 | 2007-08-27 | Novel bubbling bed reactor |
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| CN200710012680A CN101376092B (en) | 2007-08-27 | 2007-08-27 | Novel bubbling bed reactor |
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| CN101942325B (en) * | 2009-07-09 | 2013-08-28 | 中国石油化工股份有限公司 | Heavy oil hydroprocessing method and reactor |
| CN102039106B (en) * | 2009-10-21 | 2012-09-12 | 中国石油化工股份有限公司 | Novel fluidized bed reactor |
| EP2492006A4 (en) * | 2009-10-21 | 2018-05-23 | China Petroleum & Chemical Corporation | Fluidized-bed reactor and hydrotreating method thereof |
| CN102051218B (en) * | 2009-10-27 | 2014-05-21 | 中国石油化工股份有限公司 | Hydrotreating method for inferior heavy oil material |
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| CN102453526B (en) * | 2010-10-15 | 2014-05-21 | 中国石油化工股份有限公司 | Multi-section suspension bed hydrogenation process |
| CN102451650A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Suspension bed hydrogenation reactor |
| CN102453528B (en) * | 2010-10-15 | 2014-05-21 | 中国石油化工股份有限公司 | Multi-section boiling bed residual oil hydrogenation process method |
| CN102453527B (en) * | 2010-10-15 | 2014-04-02 | 中国石油化工股份有限公司 | Catalyst grading suspension bed hydrogenation process |
| CN102451652B (en) * | 2010-10-15 | 2014-01-01 | 中国石油化工股份有限公司 | Boiling-bed reactor |
| CN102453525B (en) * | 2010-10-15 | 2014-07-23 | 中国石油化工股份有限公司 | Multi-stage boiling bed hydrogenation process |
| CN103102949B (en) * | 2011-11-10 | 2015-09-30 | 中国石油化工股份有限公司 | A kind of hydrogenation reaction system and hydroprocessing process |
| CN103657539B (en) * | 2012-09-10 | 2016-07-13 | 中国石油化工集团公司 | A kind of fluidized bed reactor |
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| CN108607476B (en) * | 2016-12-09 | 2021-02-09 | 中国石油化工股份有限公司 | Fluidized bed reactor, application thereof and method for adsorbing and desulfurizing hydrocarbon oil |
| CN107512787B (en) * | 2017-09-01 | 2021-06-18 | 上海华畅环保设备发展有限公司 | Method for sorting separation media in fluidized bed separator |
| CN111377527A (en) * | 2018-12-31 | 2020-07-07 | 中国石油化工股份有限公司 | Treatment method of high-salt-content organic wastewater |
| CN111359547A (en) * | 2019-03-15 | 2020-07-03 | 南京延长反应技术研究院有限公司 | Oil-coal co-hydrogenation micro-interface reinforced emulsion bed reaction system |
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