CN203018065U - Slurry-bed loop reactor and continuous separation equipment - Google Patents
Slurry-bed loop reactor and continuous separation equipment Download PDFInfo
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- CN203018065U CN203018065U CN 201220538498 CN201220538498U CN203018065U CN 203018065 U CN203018065 U CN 203018065U CN 201220538498 CN201220538498 CN 201220538498 CN 201220538498 U CN201220538498 U CN 201220538498U CN 203018065 U CN203018065 U CN 203018065U
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Abstract
The utility model relates to a slurry-bed loop reactor and continuous separation equipment. The slurry-bed loop reactor comprises a slurry-bed loop reactor, a sedimentation tank (8) and a filtration assembly (12), wherein the slurry-bed loop reactor comprises a riser (2), a riser top expanding segment (20), a downcomer (6) and a downcomer top expanding segment (4), the riser top expanding segment (20) is communicated with the downcomer top expanding segment (4) through a down pipe (5), and the downcomer (6) is communicated with the bottom of the riser (2); and the downcomer top expanding segment (4) is communicated with the sedimentation tank (8), the upper part of the sedimentation tank (8) is communicated with the filtration assembly (12), a slurry outlet of the filtration assembly (12) is communicated with the lower part of the sedimentation tank (8) through a pipeline, and a liquid outlet (17) of the filtration assembly (12) is a liquid product outlet. Compared with the prior art, the slurry-bed reactor has the characteristics of being reasonable in structure, high in separation efficiency and capable of operating in a long-period, continuous and stable manner.
Description
Technical field
The utility model relates to a kind of slurry reactor and slurries liquid-solid separation equipment, more particularly, relate to a kind of slurry bed circulatory flow reactor and follow-up liquid solid particle continuous separate thereof from equipment.
Background technology
Paste state bed reactor is a kind of gas-liquid commonly used (slurry) haptoreaction equipment, has high liquid storage amount.For the very large catalytic reaction process of reaction heat, use paste state bed reactor can effectively remove reaction heat, the isothermal operation of realization response device guarantees the normal operation of reactor, therefore is widely used in chemical process.Slurry bed circulatory flow reactor is a kind of efficient heterophase reactor that grows up on the basis of slurry attitude bed bubbling reactor.Slurry bed circulatory flow reactor is except all advantages that has slurry attitude bed bubbling reactor and have, can also rely on its inner fluid of density official post of reactive agent district and circulating-area to do well-regulated circulating, thereby strengthen mixing, diffusion, heat transfer and mass transfer between reactant.
In order to eliminate the impact of diffusion, generally adopt tens microns even more fine grain catalyst in paste state bed reactor, but also brought liquid reaction product to separate this difficult problem with catalyst granules thereupon.How effectively to realize liquid-solid separation, become the key technology in using the slurry reactor process.
The liquid-solid separation of paste state bed reactor catalyst slurry is generally carried out outside reactor, and the slurries that contain catalyst must use specific pump to carry, and the catalyst of separating still need to send back in reactor with the slurries form.This process is easy to cause the breakage of catalyst granules, thereby the long-time continuous operation of reactor is brought problem.
Filtering technique is the common method of obtaining high separating efficiency.Press liquid form, filtration is divided into dead-end filtration and cross-flow filtration, compares traditional dead-end filtration, and the cross-flow filtration filter cake is difficult for piling up, and filter cycle is long, is the emphasis of studying at present.
US6068760, WO02/097007A2 all disclose and have adopted sedimentation techniques to realize the method for liquid-solid separation in paste state bed reactor, reacted slurries are drawn reactor, after a sedimentation pipe, slurries enter settling tank 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 EP1405664A1 is that reacted slurries are directly introduced settling tank, sedimentation is provided with baffle plate in filling with, and height of baffle plate is higher than liquid level in settling tank, therefore after slurry stream is crossed the gap of baffle plate and tank base, the clear liquid rising flows out above settling tank, and contains the underflow of particle in the outlet Returning reactor main body of settling tank bottom.
CN1600412A discloses a kind of liquid-solid separation system, and one or more layers equipment for separating liquid from solid as in reactor, is realized the purpose of Separation of Solid and Liquid by filtration.Taken so a large amount of space reactors, and solid-liquid separation unit energy and the quality transmission of reaction, poor effect have been affected in the reactor body zone.
US2005/0027021 discloses a kind of liquid-solid separation system, realize liquid-solid separation by the filter element that vertical placement is set outside reactor, what play main filtration is the filter cake that is deposited on filter element, regulates the thickness of filter cake by regulating the slurries flowing velocity.But because element space size of living in is that design has been determined, come controlled filter speed to make adjustable range very limited by the outside slurry flow rate of regulating element merely, and fine grained easily stop up screen pipe and do not have effective back-flushing method to make filter process be difficult to realize serialization.
US2005/0000861 discloses a kind of filter element that can be placed on inside reactor and/or outside, this element is divided into coarse filtration district and fine filtering district, and both coaxially vertically place with the footpath, block oarse-grained catalyst outside filtering area in coarse filtration district, top, Returning reactor recycles again again, carries out further isolated by filtration and can directly enter through the filtrate of coarse filtration the fine filtering district that is located at below the coarse filtration district.This solid separation method need to be by exterior power, and detailed back-flushing method is not provided, and is difficult to realize that liquid-solid continuous effective separates.
Utilize merely as can be known the method for filtering to be difficult to realize continued operation by above analysis, even realized that continued operation also can cause the catalyst solid abrasion of particles serious, affect separative efficiency, also can make equipment complicated, investment and operating cost increase.
The utility model content
The purpose of this utility model is to provide a kind of continued operation, and can discharge slurry bed circulatory flow reaction and the liquid-solid continuous separation equipment of the broken catalyst granules of wearing and tearing.
The slurry reactor that the utility model provides and separation equipment comprise slurry bed circulatory flow reactor, settling tank 8 and filter assemblies 12; Wherein slurry bed circulatory flow reactor comprises tedge 2, tedge top expanded section 20, down-comer 6 and down-comer top expanded section 4, tedge top expanded section 20 is communicated with down-comer top expanded section 4 through down-pipe 5, and down-comer 6 bottoms are communicated with tedge 2 bottoms; Down-comer top expanded section 4 is communicated with settling tank 8, and settling tank 8 upper clear supernate outlets are communicated with filter assemblies 12, and the slurries outlet of filter assemblies 12 is through pipeline connection settling tank 8 bottoms, and the liquid outlet opening of filter assemblies is the fluid product outlet.
The slurry reactor that the utility model provides and the beneficial effect of separation equipment are:
The slurry reactor that the utility model provides and separation equipment in the outer setting of reaction zone tedge down-comer top expanded section, settling tank and filter assemblies and the blowback system that is used for filter medium regeneration, simple in structure, separative efficiency is high, and filter medium is easy to regeneration, and is practical.Can realize that solid catalyst particle separates with the continuous high-efficient of liquid form product, can also make and discharge continuously reaction system, convenient and flexible operation because of the broken solid catalyst particle of wearing and tearing.
Description of drawings
The slurry reactor that accompanying drawing provides for the utility model and the structural representation of separation equipment.
In figure, the 1-gas distributor; The 2-tedge; The 3-discharging opening; 4-down-comer top expanded section; The 5-down-pipe; The 6-down-comer; The 8-settling tank; The outlet of 11-concentrated slurry; The 12-filter assemblies; The 13-filter medium; The 15-pump; The 17-liquid outlet opening; 18-blowback entrance; 19-slurries charge door; 20-tedge top expanded section; 7,9,10,14,16-pipeline.
The specific embodiment
Below illustrate slurry reactor that the utility model provides and the specific embodiment of separation equipment, in this manual, involved term " top " refers to the top part of this container; " top " refers to the part of the 70%-100% of container total height from top to bottom, " middle part " refers to the part between container total height 30%～70% from top to bottom, " bottom " refers to the part of container total height 0-30% from top to bottom, and " bottom " refers to this container lowermost end part.
The slurry reactor that the utility model provides and separation equipment comprise slurry bed circulatory flow reactor, settling tank 8 and filter assemblies 12; Wherein slurry bed circulatory flow reactor comprises tedge 2, tedge top expanded section 20, down-comer 6 and down-comer top expanded section 4, tedge top expanded section 20 is communicated with down-comer top expanded section 4 through down-pipe 5, and down-comer 6 bottoms are communicated with tedge 2 bottoms; Down-comer top expanded section 4 is communicated with settling tank 8, and settling tank 8 upper clear supernate outlets are communicated with filter assemblies 12, and the slurries outlet of filter assemblies 12 is through pipeline connection settling tank 8 bottoms, and the liquid outlet opening of filter assemblies is the fluid product outlet.
In slurry reactor and separation equipment that the utility model provides, described down-comer top expanded section is communicated with through pipeline with described tedge top expanded section top.
In slurry reactor and separation equipment that the utility model provides, can be between tedge and down-comer for guaranteeing solid particle, and deposition in the pipeline between tedge top expanded section and down-comer top expanded section.Preferred down-pipe 5 and the tedge connecting line bottom down-comer is and is obliquely installed, with the angle of level reference all greater than the angle of repose of solid particle.
The ratio of the caliber of the caliber of described down-pipe 5 and down-comer 6 is 0.5～6:1, preferred 1～5:1, more preferably 1.5～3:1.Preferentially select larger-diameter down-pipe 5, being convenient to thicker particle relies on gravitational settling slowly to flow to down-comer top expanded section bottom along the lower wall of down-pipe herein, bubble can gather and float herein simultaneously, make major part can return to tedge 2, play certain gas-liquid (slurry) and separate, eliminate the effect of bubble.
In slurry reactor and separation equipment that the utility model provides, described tedge expanding reach and tedge caliber ratio are 1.1～8.0:1, are preferably 1.2～2.5:1.Adopt the advantage of the structure of tedge top expanded section to be on tedge top, after described reaction mixture slurry is reacted in tedge on the supreme riser top expanded section rear slurry that flows flow and ease up, be convenient to gas-liquid (slurry) and separate, improved the removal effect of bubble in slurries.
In slurry reactor and separation equipment that the utility model provides, the bottom of tedge 2 is provided with gas distributor 1, and vapor-phase reactant enters in tedge through gas distributor 1, and the top of tedge top expanded section is provided with exhaust outlet 3.
Be provided with slurries charge door 19 on connecting pipeline bottom described down-comer and tedge.
In slurry reactor and separation equipment that the utility model provides, described slurry bed circulatory flow reactor comprises tedge 2, tedge top expanded section 20, down-comer 6 and down-comer top expanded section 4, wherein, described down-comer and down-comer top expanded section are one or more.When being a plurality of, a plurality of down-comer top expanded section can be arranged in level tedge top expanded section surrounding, so that the pressure between balance down-comer top expanded section and tedge and tedge top expanded section when down-comer and down-comer top expanded section.In use, can realize the initial gross separation of gas-liquid-solid three-phase due to settlement action down-comer top expanded section, described down-comer top expanded section inside can be divided into gas enrichment region, reduction paste liquid zone and thickened pulp liquid zone from the top to the bottom.Preferably, in order to realize the better separating effect of gas-liquid-solid three-phase in the down-comer top expanded section, the down-comer top expanded section is 1.0～50:1 with the ratio of the caliber of down-comer, preferred 1.5～25:1, more preferably 2～15:1.
In slurry reactor and separation equipment that the utility model provides, described down-comer top expanded section middle part is communicated with settling tank 8 middle parts; Described settling tank 8 tops are communicated with down-comer top expanded section top; The bottom of described settling tank 8 is provided with discharge gate 11.In use, due to settlement action, described settling tank 8 inside from the top on earth part be gas enrichment region, reduction paste liquid zone and thickened pulp liquid zone.The gas at settling tank 8 tops can enter down-comer top expanded section section through pipeline, then through tedge top gas phase discharging opening discharge.The discharge gate 11 of described settling tank bottom is in order to discharge the high concentration slurries after sedimentation concentration.Described discharge gate 11 and slurries charge door 19 are used for processing more neatly catalyst.Replenish by slurries charge door 19 slurries that are mixed with fresh solid particle catalyst.Simultaneously,, can discharge by discharge gate 11 during in the enrichment of the bottom of settling tank 8 due to drawing small when the catalyst granules in reactor.
In slurry reactor and separation equipment that the utility model provides, the reduction paste liquid zone on described settling tank 8 tops is connected with described filter assemblies 12, and the slurries district of described filter assemblies 12 is connected with settling tank 8 bottoms.Clear liquid after sedimentation in settling tank is introduced in filter assemblies filtered, further remove solid granule, obtain liquid-phase product, simultaneously, the slurries after concentrated are sent back in settling tank 8.Being provided with filter medium in filter assemblies 12, is slurries district and filtrate district by filter medium with the spatial separation in filter assemblies, and wherein the filtrate district is connected with liquid outlet opening 17, and the liquid after filtering is sent as product.Described filtrate district also is connected with for filter medium being carried out blowback entrance 18 and the valve of backwash, with the switching between controlled filter and backwash.On the connecting line of settling tank 8 and filter assemblies, pump can be set, to increase liquid stream mobilization dynamic.
In slurry reactor and separation equipment that the utility model provides, described filter medium is selected from 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 materials or other type.The material not restriction of the utility model to filter medium.
The slurry reactor that the utility model provides and the application process of separation equipment, unstripped gas enters tedge 2 after being distributed by gas distributor 1, with the slurries mixing afterreaction in tedge 2, then upwards flow into tedge top expanded section 20, slurries ease up owing to changing flow direction and flowing herein, can remove most of bubble, the slurries that are mingled with part minor diameter bubble flow in down-comer top expanded section 4 through down-pipe 5; In the tedge top expanded section, be gas enrichment space on the aperture position of down-pipe 5, be used for the gas that the unreacted gas of enrichment and reaction generate.In down-comer top expanded section 4, be mingled with alveolate slurries and rely on the preliminary sedimentation of Action of Gravity Field, in the down-comer top expanded section space from the top on earth part be gas enrichment region, reduction paste liquid zone and thickened pulp liquid zone; Wherein the gas enrichment space at gas enrichment region and tedge top expanded section 20 tops is connected.The catalyst of larger particles along with the slurries main body flows downward through down-comer, returns to sustainable participation reaction in tedge 2 after the enrichment of down-comer top expanded section.A small amount of broken subparticle can rise along with slurries are slow and the final settling tank 8 that flows into.In this process, owing to containing a large amount of bubbles in tedge, its internal density is reduced, thereby formed a density contrast with the slurries in down-comer, cause slurries to form circulating of nature between tedge and down-comer, thereby guaranteed the continuous displacement of concentrated slurry in the down-comer top expanded section, guaranteed simultaneously carrying out continuously of multi-phase separation process.
In settling tank 8, contain the slurries of a small amount of broken subparticle can further sedimentation with space in settling tank 8 from the top on earth part be gas enrichment region, reduction paste liquid zone and thickened pulp liquid zone.Wherein the gas enrichment region is connected with down-comer top expanded section top; The slurries of reduction paste liquid zone are introduced in filter assemblies 12 through pump 15 and are carried out isolated by filtration, and the concentrated slurry after filtration returns to the bottom thickened pulp liquid zone enrichment of settling tank through pipeline 16, and finally discharges through discharge gate 11.
In filter assemblies 12, slurries from settling tank 8 axially flow downward along filter assemblies, wherein a part of liquid by filter medium, and is finally drawn as product under the promotion of filter medium both sides pressure reduction, and the micro-solid particle flows back to settling tank 8 bottoms with slurries.Carry out filtering medium layer both sides pressure reduction thickening and rise along with filter cake with reaction, when pressure reduction higher than when setting value, backwashing system is started working, this moment, the liquid outlet opening late gate was closed, valve opening on blowback lines, liquid outlet opening and recoil pipeline are communicated with, the backwash medium is the back flush filtering medium layer under the reverse differential pressure that adds promotes, the reverse differential pressure that removes with filter cake constantly reduces, when setting value lower than another, flushing process finishes, the valve closing on this moment blowback lines, and system returns to normal operating state.Wherein said backwash medium can be the product clear liquid, can be also distillate, the preferred product clear liquid.
The applicable gas, liquid, solid phase reaction of the method that the utility model provides also need to be isolated the chemical reaction process of solid particle from slurries, (Fischer-Tropsch) process as synthetic in the hydrocarbon oil hydrogenation, certain embodiments and the Fischer-Tropsch that adopt suspension bed or oar state bed reactor.
Illustrate below in conjunction with accompanying drawing the continuous separation method that paste state bed reactor that the utility model provides is used for Fischer-Tropsch building-up process liquid and solid particle, but therefore the utility model is not restricted.
As shown in drawings: the reactant synthesis gas enters in tedge with wherein slurries through gas distributor 1 from the bottom of tedge 2 and mixes, contact with catalyst granules in slurries, complete chemical reaction in uphill process, product and unnecessary reactant rise to reactor head expanding reach 20 together with catalyst; Unreacted gas reactant separates with slurries herein with gaseous product, discharges from the gas vent 3 at top, and solid particle catalyst enters in down-comer top expanded section 4 through pipeline 5 with the form of liquid with slurries; In down-comer top expanded section 4, gas-liquid-solid three-phase due to the density difference be subjected to depositional affect with space in tank from the top on earth part be gas enrichment region, reduction paste liquid zone and thickened pulp liquid zone, the gas of enrichment is sent into down-comer top expanded section 4 top gas enrichment spaces through pipeline 7, the slurries of thickened pulp liquid zone can flow downward and return to tedge 2 through down-comer 6, the dilution slurries that contain micro-minute bubbles and crushed particles can be introduced into settling tank 8, and carry out herein secondary settlement, realize further gas-liquid-solid three-phase separation; Wherein, gas is introduced down-comer top expanded section 4 by pipeline 9, the slurries that are rich in solid particle can be got rid of by discharge gate 11, the slurries that contain micro-broken solid particle can flow through filter assemblies through pump 15 from top to bottom by pipeline 14, under filter medium 13 inside and outside differential pressures promote, liquid can radially pass filter medium, and finally draws as product.Solid particle is arrested on the filter medium inwall, souring due to liquid flow, part filter cake on the filter medium inwall constantly comes off and flows downward with slurries and turns back in settling tank 8, the filter cake of part difficult drop-off can be trapped on the inwall of filter medium, along with constantly thickening of filter cake, pressure reduction between filter medium is inside and outside rises, and during higher than 0.35MPa, backwashing system is started working when pressure reduction.Under the promotion that adds reverse differential pressure, the backwash medium introduce in the filtrate district of filter assemblies and radially ecto-entad pass through filter medium, the filter cake that is attached on the filter medium inwall is sprung back in slurries, and returns to settling tank 8 along with slurries flow downward.During lower than 0.1MPa, flushing process finishes when the pressure reduction inside and outside filter medium, and system returns to normal operating state.
The following examples are further described the method that the utility model provides, but therefore do not limit the utility model.
Embodiment
The tedge top expanded section that adopts in force is 1.4:1 with the caliber of tedge ratio, the Area Ratio of down-comer top expanded section and tedge is 1:1, down-pipe 5 is 2:1 with the diameter ratio of down-comer 6, the down-comer top expanded section is 3.5:1 with the caliber ratio of down-comer, down-pipe 5 is 45 degree with the placement angle of down-comer 6 and level reference, and chimney filter is one sintered porous metal chimney filter, its external diameter 50mm, long 1000mm, average pore size 2 μ m.The particle size range of the catalyst that adopts is 20～100 μ m, and synthesis gas enters bed by reactor bottom with the form of bubbling in this process, under operating condition, generates liquid hydrocarbon.Unreacted synthesis gas separates with slurries fully with gas products after slurries rise to reactor head, and is discharged by exhaust outlet; The part slurries are introduced the down-comer top expanded section through down-pipe 5, unworn thicker catalyst granules be settled down to down-comer top expanded section bottom and with slurries through the down-comer Returning reactor, the slurries that contain damaged catalyst granules enter settling tank.In settling tank, the slurries that are rich in broken solid particle can be discharged by discharge gate 11, and the slurries that contain micro-broken solid particle can flow through filter assemblies from top to bottom by pump 15, after media filtration, finally draw as product after filtration.In this process, the slurry solid content that the down-comer top expanded section is discharged is 700 μ g/ml, and in liquid form product, solid content is 3 μ g/ml, and the maximum gauge of particle is 2 μ m.Separative efficiency is more than 99%.Wherein in slurries, solid content adopts weight method to measure.Separative efficiency is calculated by following formula:
η=（S
m-S
f）/S
m
Wherein: S
mSolid content in=raw material (slurries before filtering); S
fSolid content in=product (cleaner liquid).
Claims (11)
1. a slurry bed circulatory flow reactor and continuous separation equipment, is characterized in that, comprises slurry bed circulatory flow reactor, settling tank (8) and filter assemblies (12); Wherein slurry bed circulatory flow reactor comprises tedge (2), tedge top expanded section (20), down-comer (6) and down-comer top expanded section (4), tedge top expanded section (20) is communicated with down-comer top expanded section (4) through down-pipe (5), and down-comer (6) bottom is communicated with bottom tedge (2); Down-comer top expanded section (4) is communicated with settling tank (8), settling tank (8) top is communicated with filter assemblies (12), the slurries outlet of filter assemblies (12) is through pipeline connection settling tank (8) bottom, and the liquid outlet opening (17) of filter assemblies (12) is the fluid product outlet.
2. according to reactor and the continuous separation equipment of claim 1, it is characterized in that, the top of described down-comer top expanded section is communicated with through pipeline with the top of described tedge top expanded section.
3. according to reactor and the continuous separation equipment of claim 1, it is characterized in that, the connecting line of described down-pipe (5) and tedge and down-comer bottom is and is obliquely installed, with the angle of level reference all greater than the angle of repose of solid particle.
4. according to reactor and the continuous separation equipment of claim 1, it is characterized in that, the ratio of the caliber of the caliber of described down-pipe (5) and down-comer (6) is 0.5～6:1.
5. according to reactor and the continuous separation equipment of claim 4, it is characterized in that, the ratio of the caliber of the caliber of described down-pipe (5) and down-comer (6) is 1～5:1.
6. according to reactor and the continuous separation equipment of claim 5, it is characterized in that, the ratio of the caliber of the caliber of described down-pipe (5) and down-comer (6) is 1.5～3:1.
7. according to reactor and the continuous separation equipment of claim 1, it is characterized in that, described tedge expanding reach and tedge caliber ratio are 1.1～8.0:1.
8. according to reactor and the continuous separation equipment of claim 7, it is characterized in that, described tedge expanding reach and tedge caliber ratio are 1.2～2.5:1.
9. according to reactor and the continuous separation equipment of claim 1, it is characterized in that, be provided with slurries charge door (19) on the connecting pipeline of described down-comer and tedge bottom.
10. according to reactor and the continuous separation equipment of claim 1, it is characterized in that, described down-comer top expanded section is 1.0～50:1 with the ratio of the caliber of down-comer.
11. reactor and continuous separation equipment according to claim 10 is characterized in that, described down-comer top expanded section is 1.5～25:1 with the ratio of the caliber of down-comer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220538498 CN203018065U (en) | 2012-10-19 | 2012-10-19 | Slurry-bed loop reactor and continuous separation equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220538498 CN203018065U (en) | 2012-10-19 | 2012-10-19 | Slurry-bed loop reactor and continuous separation equipment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203018065U true CN203018065U (en) | 2013-06-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201220538498 Expired - Lifetime CN203018065U (en) | 2012-10-19 | 2012-10-19 | Slurry-bed loop reactor and continuous separation equipment |
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| Country | Link |
|---|---|
| CN (1) | CN203018065U (en) |
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2012
- 2012-10-19 CN CN 201220538498 patent/CN203018065U/en not_active Expired - Lifetime
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Granted publication date: 20130626 |
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