CN100548459C - A kind of slurry attitude bed consersion unit and application process thereof - Google Patents
A kind of slurry attitude bed consersion unit and application process thereof Download PDFInfo
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- CN100548459C CN100548459C CNB200610089023XA CN200610089023A CN100548459C CN 100548459 C CN100548459 C CN 100548459C CN B200610089023X A CNB200610089023X A CN B200610089023XA CN 200610089023 A CN200610089023 A CN 200610089023A CN 100548459 C CN100548459 C CN 100548459C
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Abstract
A kind of slurry attitude bed consersion unit and application process thereof, this equipment comprises tedge reactor 1 and sedimentation pipe 4, the bottom of tedge reactor 1 is a reaction zone 14, top is the decanting zone 2 that caliber enlarges, the top of decanting zone 2 is provided with exhaust outlet 6, the bottom of tedge 1 is provided with charging aperture 3 and gas distributor 5, pipeline 7 is used to connect decanting zone 2 and sedimentation pipe 4, and aperture position is in the inside of sedimentation pipe 4, sedimentation pipe 4 bottoms are magnetic Disengagement zone 15, its lower end is by conical nozzle 10, return duct 11 is connected with the lower end of tedge reactor 1, and sedimentation pipe 4 tops are provided with liquid outlet opening 13.Adopt equipment of the present invention and separation method, improved the space availability ratio of reactor; Adopt sedimentation, magnetic to separate and the isolation technics of filtering combination simultaneously, make that the equipment volume of separating part is little, efficient is high and save the space.
Description
Technical field
The present invention relates to equipment and method that solia particle is separated from liquid, more particularly, relate to a kind of equipment and application process thereof that attitude bed reaction system liquid and solid particle separate continuously that be used for starching.
Background technology
Fischer-Tropsch (Fischer-Tropsch) is synthetic to be the important method that synthesis gas is converted into liquid hydrocarbon through catalyst action.In recent years, along with the worsening shortages of petroleum resources, natural gas resource and coal resources become the important selection that substitutes oil, thereby the Fischer-Tropsch synthetic technology demonstrates good prospects for application.Fischer-Tropsch synthesis device type mainly comprises: three classes such as fixed bed reactors, fluidized-bed reactor and paste state bed reactor.Wherein, paste state bed reactor is simple in structure, is easy to move heat, can synthesize high-quality paraffin under lower temperature, and synthetic paraffin wax product is of many uses, the added value height.Therefore utilize paste state bed reactor to carry out the low temperature Fischer-Tropsch and become an important artificial oil production route.
The problem that adopts slurry attitude bed reaction technology to exist is mainly: material Transfer is slower in the slurries, in order to eliminate interior diffusion influence, increase the contact area of catalyst and reactant, catalyst is general to adopt tens microns even thinner particle, thereby makes product and catalyst granules be difficult to separate.
How to realize liquid-solid separation effectively, become the key technology of using slurry attitude bed course of reaction.At present, what the realization Separation of Solid and Liquid was comparatively general in slurry attitude bed reaction system is sedimentation techniques, and the principle of its separation is in sedimentation device, and the gravity of the solid particle that utilization suspends own makes its sinking and separates with product liquid.
US 6068760, WO 02/097007A2 all disclose and have adopted sedimentation techniques to realize that slurry attitude bed reacts the method for liquid-solid separation, reacted slurries are drawn reactor, behind a sedimentation pipe, slurries enter sedimentation pipe and carry out sedimentation, supernatant liquor is discharged as product, and the thick slurry Returning reactor circulation of a large amount of catalyst granules is contained in lower floor.
The disclosed separation method of EP 1405664A1 is that the slurries of drawing reactor body are directly introduced settling tank.Be provided with baffle plate in the settling tank, and height of baffle plate is higher than liquid level in the settling tank, therefore after slurry stream was crossed the slit of baffle plate and tank base, clear liquid slowly rose and flows out above settling tank, and contains the outlet Returning reactor main body of the underflow of particle in the settling tank bottom.
Utilize single sedimentation techniques to realize Separation of Solid and Liquid comparatively completely, obtaining the minimum product liquid of solids content then requires sedimentation device must volume very big to guarantee enough sedimentation times, this has just caused the most of area and the space of equipment to be taken by sedimentation device, and production efficiency is lower.The more little catalyst of particle diameter in addition, help more that Fischer-Tropsch is synthetic to carry out, and simultaneously in course of reaction catalyst abrasion can produce the minimum pressed powder of particle diameter, but be that the separating effect of the littler catalyst granules sedimentation techniques of several microns or particle diameter is not good for particle diameter.
CN 1433838A discloses the separation method and the equipment of liquid artificial oil and solid catalyst in a kind of paste state bed reactor, this method will contain the slurry oil of catalyst granules and introduce a component from the unit, after carrying out sedimentation separation, apply high-intensity magnetic field in the bottom of sedimentation unit to quicken Separation of Solid and Liquid speed, but the separation equipment of its application is in the reactor body, because Fischer-Tropsch synthesis device diameter often more than 5 meters, is difficult to produce uniform magnetic field in the reactor, and the equipment heaviness involves great expense; Simultaneously can't carry out demagnetization, cause the reunion of magnetization catalyst, and then make that reactor can not normal running producing magnetized catalyst; For the separation of the minimum nonmagnetic powder of the particle diameter of catalyst abrasion generation, this patent does not propose effective separation method in addition.
WO 94/16807 discloses and has a kind ofly realized the method for Separation of Solid and Liquid at reactor inner filtration slurries, in case but catalyst granules stops up filter assemblies, the regeneration difficulty of filter assemblies then, thereby be unfavorable for large-scale continuous production.Therefore must adopt more efficiently solid-liquid separation technique to be applied to synthetic this plasmoid attitude bed course of reaction of Fischer-Tropsch, the realization catalyst granules separates fully with the artificial oil product.
Summary of the invention
The purpose of this invention is to provide a kind of slurry attitude bed consersion unit of realizing that simple and effectively gas-liquid-solid three-phase is separated continuously.
Another object of the present invention provides a kind of attitude bed consersion unit of starching and is applied to starch the method that the reaction of attitude bed realizes the continuous separation of gas-liquid-solid three-phase.
Slurry attitude bed consersion unit provided by the invention comprises tedge reactor 1 and sedimentation pipe 4, the bottom of tedge reactor 1 is a reaction zone 14, top is the decanting zone 2 that caliber enlarges, the top of decanting zone 2 is provided with exhaust outlet 6, the bottom of tedge reactor 1 is provided with charging aperture 3 and gas distributor 5, pipeline 7 is used to connect decanting zone 2 and sedimentation pipe 4, and aperture position is in the inside of sedimentation pipe 4, sedimentation pipe 4 bottoms are magnetic Disengagement zone 15, its lower end is by conical nozzle 10, return duct 11 is connected with the lower end of tedge reactor 1, and sedimentation pipe 4 tops are provided with liquid outlet opening 13.
In the equipment provided by the invention, the decanting zone 2 on described tedge reactor 1 top links to each other with lower reaction zone 14 by bullet.Wherein the height of decanting zone 2 is 0.1～0.5 of tedge reactor 1 height overall, and the caliber ratio of decanting zone 2 and reaction zone 14 is 1.1～10: 1, preferred 1.5～4: 1.
In the equipment provided by the invention, can also between the decanting zone 2 on described tedge reactor 1 top and sedimentation pipe 4, heat exchanger be set, can be one or more, purpose is that the part heat that will generate in the course of reaction shifts out tedge reactor 1, and with the heat transmission equipment heat-shift, help keeping temperature stabilization in the tedge reactor 1.
In the equipment provided by the invention, the aperture position of described pipeline 7 in sedimentation pipe 4 inside can be in any position in the sedimentation pipe 4, and preferred opening is in the bottom of sedimentation pipe 4.
In the equipment provided by the invention, the described magnetic Disengagement zone 15 outer magnetic separation systems 8 that are provided with.Magnetic separation system 8 can be that the mode of twining the energising solenoid and/or permanent magnet being set on 15 outer walls of magnetic Disengagement zone realizes.15 bottoms, described magnetic Disengagement zone design conical nozzle 10 connects return duct 11, and at this, catalyst accelerated motion is returned tedge reactor 1 and recycled.Behind the magnetic Disengagement zone 15 the demagnetization district can also be set, make the catalyst granules demagnetization that 15 magnetization are assembled in the magnetic Disengagement zone, with the dispersed catalyst particle; The demagnetization district can be by twining wire coil at return duct 11 outer walls, and regularly logical high-frequency ac current produces high-frequency alternating magnetic field and realizes the demagnetization function.
In the equipment provided by the invention, the bottom of described sedimentation pipe 4 is provided with catalyst feeds and catalyst discharge port.Catalyst feeds and catalyst discharge port are used for online displacement catalyst, as: drop into fresh catalyst, shed the catalyst of wearing and tearing, magnetization or inactivation.
In the equipment provided by the invention, described liquid outlet opening 13 can also connect filtration system.Filtration system is the filter plant that comprises filter medium and blowback system that works alone more than the cover.
The present invention also provides the application process of above-mentioned slurry attitude bed consersion unit, and reacted slurries separate, realize that gas-solid liquid three-phase separates continuously after the filter operation through twice sedimentation, magnetic.Concrete steps comprise: reaction mass is by charging aperture 3 access arrangements, in tedge reactor 1, mix with loop slurry, mixed slurries react in tedge reactor 1, travel up to decanting zone 2 then and carry out gas-liquid separation, gas is discharged from the exhaust outlet 6 at top, thicker catalyst granules relies on gravitational settling to turn back to reaction zone 14, and the slurries that contain thin catalyst granules enter sedimentation once more the sedimentation pipe 4 from decanting zone 2 through pipeline 7, catalyst granules in the sedimentation pipe 4 in the dense slurries of lower floor is by the effect of magnetic Disengagement zone 8 externally-applied magnetic fields, and accelerated motion is by conical nozzle 10, return duct 11 turns back in the tedge reactor 1 and recycles; Sedimentation pipe 4 clear liquid is at the middle and upper levels discharged as fluid product through liquid outlet opening 13.
In the method provided by the invention, clear liquid can also system's 9 filtrations be back as fluid product after filtration again behind liquid outlet opening 13 at the middle and upper levels for described sedimentation pipe 4.Supernatant liquor is introduced filtration system 9, after filtering, removes the remaining minimum pressed powder of micro-particle diameter owing to the catalyst abrasion generation, obtains qualified fluid product.Can select for use two filter plants alternately to filter, in the time of a filter filtering catalyst powder, another filter carries out pulse cleaning.
To the material of the filter medium in the filtration system 9 without limits, can use the filtering material of sintered metal mesh micropore filter material, sintering metal powder micropore filter material, metal micro-holes membrane material, sintered metal fiber poromerics, micropore ceramics material, ceramic membrane material or other type among the present invention.
In the method provided by the invention, described catalyst is the iron-based that can be magnetized under the magnetic field, Ni-based, cobalt-base catalyst.Catalyst can be a support type, also can be all metal catalyst of amorphous alloy class.The particle diameter of solid catalyst particle is preferably in 10 μ m～200 mu m ranges.
Slurry attitude bed consersion unit provided by the invention adopts the gas-solid liquid three-phase of outer circulation mode realization response rear slurry to separate continuously, makes that the tedge reactor in the slurry attitude bed reaction system is used for course of reaction fully, has improved the space availability ratio of reactor; Adopt twice sedimentation, magnetic to separate and the isolation technics of filtering combination simultaneously, make that the equipment volume of separating part is little, efficient is high and save the space.
The application process of slurry attitude bed consersion unit provided by the invention makes reacted slurries realize that after twice sedimentation, magnetic separation, filter operation gas-solid liquid three-phase separates continuously, the continuous high-efficient that can realize solid catalyst particle, liquid form product and reacting gas separates, discharging continuously.
Description of drawings
Accompanying drawing is the schematic diagram of equipment provided by the invention.
Wherein: 1-tedge reactor; The 2-decanting zone; The 3-charging aperture; The 4-sedimentation pipe; The 5-gas distributor; The 6-exhaust outlet; 7-tedge reactor upper end tapping line; The 8-magnetic separation system; The 9-filtration system; The 10-conical nozzle; The 11-return duct; The 12-anti-magnetized coil; The 13-pipeline; The 14-reaction zone; 15-magnetic Disengagement zone.
The specific embodiment
Specify the continuous separation method that slurry bed circulatory flow reactor provided by the invention is used for Fischer-Tropsch building-up process liquid and solid particle below in conjunction with accompanying drawing, but therefore the present invention is not restricted.
As shown in drawings: the synthesis gas reaction thing enters reactor from the bottom feed mouth 3 of tedge reactor 1 through gas distributor 5, be mixed into reaction zone 14 with slurries wherein, in uphill process with slurries in the catalyst granules haptoreaction generate liquid hydrocarbon, liquid hydrocarbon and unreacted gas rise to the decanting zone 2 on reactor top with catalyst granules, because the sectional area of decanting zone 2 is greater than the sectional area of reactor lower part reaction zone 14, here the flow velocity of slurries reduces, bigger catalyst granules returns reaction zone 14 by gravitational settling, bubble in the slurries breaks, unreacted gas separates with slurries, discharges from the exhaust outlet 6 at top; More fine grain catalyst then enters in the sedimentation pipe 4 through pipeline 7 with liquid, and pipeline 7 is opened on the bottom of sedimentation pipe 4, and at this, slurries are sedimentation once more, and catalyst granules separates with liquid hydrocarbon, obtains the dense slurries of supernatant liquor and lower floor; Catalyst granules in the dense slurries of sedimentation pipe 4 bottoms under the effect of the externally-applied magnetic field that magnetic separating device 8 provides, the directed acceleration enters return duct 11 by conical nozzle 10, return duct 11 outer walls twine anti-magnetized coil, and regularly logical high-frequency ac current produces high-frequency alternating magnetic field and realizes the demagnetization function.Catalyst after demagnetization flows into the bottom cycle of tedge reactor 1 and uses; The supernatant liquor on sedimentation pipe 4 tops enters filtration system 9 through pipeline 13, removes the wherein minimum catalyst fines of particle diameter after filtration, obtains liquid hydrocarbon product.
The following examples illustrate further to method provided by the invention, but not thereby limiting the invention.
Embodiment
The reactor height is 10m, and the caliber of reaction zone is 300mm, and the caliber of decanting zone is 600mm, and the decanting zone height is 25% of a reactor height overall; Reaction raw materials is a synthesis gas, and wherein volumn concentration is: hydrogen is 66%, and carbon monoxide is 34%, and volume space velocity is: 1200h
-1The cobalt-base catalyst that catalyst is produced for DEGUSSA company, the trade mark is B2112Z, 80 microns of catalyst average grain diameters; The reactor reaction temperature is 260 ℃, and pressure is 1.8MPa; Magnetic Disengagement zone, sedimentation pipe bottom magnetic field intensity is 20 kiloampere/rice, and the demagnetization district adopts the alternating current of 150 KHzs; It is filter medium that filtration system adopts the ceramic membrane of 0.5 micron of average pore size, adopt method provided by the invention to react, solid grain size is after testing below 1 micron in the product, solid content in this particle size range is 0.1% of a catalyst total amount, and therefore the solid-liquid separation efficiency of separation method provided by the invention is 99.9%.
Claims (13)
1, a kind of slurry attitude bed consersion unit, it is characterized in that this equipment comprises tedge reactor (1) and sedimentation pipe (4), the bottom of tedge reactor (1) is reaction zone (14), top is the decanting zone (2) that caliber enlarges, the top of decanting zone (2) is provided with exhaust outlet (6), the bottom of tedge reactor (1) is provided with charging aperture (3) and gas distributor (5), pipeline (7) is used to connect decanting zone (2) and sedimentation pipe (4), and aperture position is in the inside of sedimentation pipe (4), sedimentation pipe (4) bottom is magnetic Disengagement zone (15), its lower end is by conical nozzle (10), return duct (11) is connected with the lower end of tedge reactor (1), and sedimentation pipe (4) top is provided with liquid outlet opening (13).
2,, it is characterized in that the decanting zone (2) on described tedge reactor (1) top links to each other by bullet with lower reaction zone (14) according to the equipment of claim 1.
3,, it is characterized in that the decanting zone (2) on described tedge reactor (1) top and the caliber ratio of lower reaction zone (14) are 1.1～10 according to the equipment of claim 1.
4,, it is characterized in that described caliber ratio is 1.5～4 according to the equipment of claim 3.
5,, it is characterized in that between described tedge reactor (1) upper end and the sedimentation pipe (4) heat exchanger being set according to the equipment of claim 1.
6,, it is characterized in that described pipeline (7) is in the bottom of sedimentation pipe at the inner opening of sedimentation pipe (4) according to the equipment of claim 1.
7,, it is characterized in that described magnetic Disengagement zone (15) equipment sidewall peripheral hardware puts magnetic separation system (8) according to the equipment of claim 1.
8,, it is characterized in that the downstream area of described magnetic Disengagement zone (15) is provided with the demagnetization district according to the equipment of claim 1.
9,, it is characterized in that described liquid outlet opening (13) connects filtration system (9) according to the equipment of claim 1.
10,, it is characterized in that the bottom of described sedimentation pipe (4) is provided with catalyst feeds and catalyst discharge port according to the equipment of claim 1.
11, the application process of the equipment of claim 1, it is characterized in that reaction mass is by charging aperture (3) access arrangement, in tedge reactor (1), mix with loop slurry, mixed slurries react in tedge (1), travel up to decanting zone (2) then and carry out gas-liquid separation, gas is discharged from the exhaust outlet (6) at top, thicker catalyst granules relies on gravitational settling to turn back to reaction zone (14), and the slurries that contain thin catalyst granules enter sedimentation once more the sedimentation pipe (4) from decanting zone (2) through pipeline (7), catalyst granules in the sedimentation pipe (4) in the dense slurries of lower floor is by the effect of magnetic Disengagement zone (8) externally-applied magnetic field, and accelerated motion is by conical nozzle (10), return duct (11) turns back in the tedge reactor (1) and recycles; Sedimentation pipe (4) clear liquid is at the middle and upper levels discharged as fluid product through liquid outlet opening (13).
12, according to the method for claim 11, it is characterized in that with sedimentation pipe (4) at the middle and upper levels clear liquid behind liquid outlet opening (13) more after filtration system (9) filter the back as fluid product.
13,, it is characterized in that described catalyst is the iron-based that can be magnetized under the magnetic field, Ni-based or cobalt-base catalyst according to the method for claim 11.
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| CN103846161B (en) * | 2012-11-30 | 2017-02-08 | 中国石油化工股份有限公司 | Solid-liquid separation method |
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| CN103962069B (en) * | 2013-01-31 | 2017-03-08 | 中国科学院上海高等研究院 | A kind of paste state bed reactor |
| JP6071691B2 (en) * | 2013-03-26 | 2017-02-01 | 新日鉄住金エンジニアリング株式会社 | Hydrocarbon synthesis reactor |
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