CN1739846A - Separation process of synthetic oil catalyst prepared in slurry bed reactor - Google Patents
Separation process of synthetic oil catalyst prepared in slurry bed reactor Download PDFInfo
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Abstract
In the conventional Fischer-Tropsch process, synthetic gas is led into slurry bed reactor for catalyzed reaction, the suspended material is fed from the reactor to the inorganic film separator to separate synthetic oil with the inorganic film from the suspended material to obtain purified oil, and concentrated oil slurry with rich catalyst is returned to the slurry bed reactor for further reaction or further separated. The present invention adopts ceramic and/or metal film of pores in the size from 2 nm to 100 micron to separate the fine solid catalyst particles, and makes it possible to apply micron level, submicron level or even nm level solid catalyst in oil synthesizing industry.
Description
Technical field
The present invention relates to a kind of separation process of synthetic oil catalyst, relate in particular to a kind of Separation Process for Making Synthetic Catalyst with Slurry Bed Reactor, being used for coal or natural gas is raw material is produced artificial oil through the Fischer-Tropsch synthetic method process.
Project background
Because the contradiction between the limited petroleum reserves of the oil demand that increases day by day and the earth, people press for a kind of energy approach that can take over oil of searching.With coal or natural gas is that the feedstock production artificial oil can effectively utilize higher coal of reserves and natural gas, replenish the deficiency of world petroleum resource, and owing to sulphur (S), nitrogen (N) and heavy metal equal size in the artificial oil are low, can satisfy environmental protection requirement, so be subjected to the extensive concern of world's chemical industry.
No matter be that coal or natural gas are produced artificial oil and will be realized that all the first step is synthesis gas H through three processes
2With the preparation of CO, second step was synthesis gas (the 3rd step became oil product to the oil refining process of artificial oil by routine for Fischer-Tropsch, FT) synthetic artificial oil and the water of being converted into through the low temperature Fischer-Tropsch.Fischer-Tropsch synthesis device type has the branch of fixed bed, fluid bed and slurry attitude bed, and it is more advanced wherein to starch the attitude bed, comes into operation in industry.South Africa Sasol company has developed this reactor the eighties in 20th century, and builds up the industrialized unit of 2500 barrels/d of a cover in May, 1993.This reactor advantage is: (1) is simple in structure, is easy to amplify; (2) but isothermal operation, thereby available higher operating temperature and obtain higher reaction rate; (3) can online loading and unloading catalyst; (4) pressure drop of reactor is low, can save the compression expense; (5) CO conversion per pass height, the hydrocarbon-selective height that C5 is above.Main medium is artificial oil, synthesis gas (H in the reactor
2+ CO) and catalyst, the particle diameter that requires catalyst is between 1～100 μ m.Can artificial oil be separated from the synthetic slurry oil that contains solid catalyst effectively in the paste state bed reactor, and make catalyst obtain recycling, is that can device the key of moving steady in a long-term.
The separation method of catalyst mainly contains sedimentation, filtration, centrifugation, magnetic separation technique, supercritical extract separation or the like in the paste state bed reactor.Sedimentation-separation technology is to utilize gravity that catalyst granules sedimentation separation from slurries is come out, and shifts out artificial oil continuously or off and on, finishes separating of oil and catalyst.The examination of the mould of U.S. Mobil company, the La Bote pilot scale of DOE, the mould of the pilot scale of Britain fuel experimental center and China's Shanxi coalification institute tries, and when handling oil and catalyst separation, has all adopted the gravity settling separation operation.Chinese patent CN03118581.9 has proposed to contain the slurry oil of catalyst and has imported a component from the unit, carries out the method for sedimentation with separating catalyst in separative element.Its used separative element comprises housing, be positioned at the housing middle part the slurry oil distributor pipe, be positioned at the last division board on housing top and be positioned at the following division board of lower housing portion.The slurry oil distributor pipe is the porous coil pipe, and the porous coil pipe is provided with the slurry oil inlet, and following division board and last division board are porous plates, following division board and below form down gathering room, following gathering room is provided with and concentrates the slurry oil outlet, and last division board and top form gathering room, and last gathering room is provided with the clean oil outlet.During use, slurry oil to be separated enters separative element inside by the slurry oil inlet, radially be uniformly distributed in the separative element through the slurry oil distributor pipe, because the sedimentation of catalyst, form concentrated slurry oil in the separative element bottom, concentrated slurry oil warp division board down enters down gathering room, exports the extraction separative element through concentrating slurry oil again.Clean oil upwards enters gathering room through last division board, under the effect of external and internal pressure difference, discharges separative element through the clean oil outlet.The deficiency of gravitational settling is that disengaging time is long, and the small particle diameter catalyst separation efficient that produces for catalyst breakage is low, and is lower to the separative efficiency of superfine catalyst, can't be used for submicron order, nano level catalyst separation.
Separate required time in order to shorten catalyst with oil, particularly in separating the decaying catalyst operation, it is the preferential separation method that adopts that centrifuge separates.Mobil company adopts the centrifugation operation to remove most of catalyst in the suspension in its conceptual design, and clean oil is delivered to storage tank again and used for further filtering.DOE proposes to adopt the scheme of hydrocyclone in the design of its industrial reactor that carries out, promptly continuously extract a part of slurries to hydrocyclone, and top stream part is used for reclaiming artificial oil, and underflow is Returning reactor then.
Filter operation is a common method of obtaining high separating efficiency.The cross-flow filter that U.S. DOE adopts on the pilot-plant of La Bote is to be made of four filter elements that are five feet long of connecting.Filter element is 5/8 inch of an internal diameter, the stainless steel tube of 1 μ m level.With the clean oil blowback once practical operation was promptly lost efficacy after one day in 30 minutes at interval although filter element is designed to.The filtration and separation techniques of South Africa Sasol company is the unique artificial oil in the paste state bed reactor and isolation technics of catalyst of successfully being used in industrial production, and this technology still is in confidential state at present.
Magnetic separation technique mainly contains two kinds of implementation methods, and a kind of is to utilize high-gradient magnetic field to produce magnetic field force, and ferromagnetic substance is separated; Another kind method is to utilize high magnetic field intensity to promote the flocculation of ferromagnetic material, thereby increases particle sinking speed, reaches the separation purpose.This technology is to the catalyst requirement that is magnetic.The supercritical extract separation method is actual to be to utilize supercritical fluid as a kind of solvent Fischer-Tropsch synthesis oil to be extracted, and reaches the purpose with catalyst separation.The concrete facilities and equipments complexity of this method, plant investment and operating cost are all bigger.
Summary of the invention
The purpose of this invention is to provide Fischer-Tropsch synthetic method separation process of synthetic oil catalyst prepared in a kind of paste state bed reactor; it solves the separation problem of liquid artificial oil and solid catalyst; avoid catalyst fines to sneak in the artificial oil, guarantee degree of purity of production, make catalyst obtain recycling simultaneously.
Technical scheme of the present invention is: a kind of Separation Process for Making Synthetic Catalyst with Slurry Bed Reactor, Fischer-Tropsch synthesis method routinely, synthesis gas is fed paste state bed reactor 1 carry out catalytic reaction, the separation process that it is characterized in that the suspended state material is conveyed into inoranic membrane separator 4 for the slurry oil that paste state bed reactor 1 is included catalyst, utilize the sieving actoion of inoranic membrane, liquid artificial oil is wherein separated from slurry oil through inoranic membrane, be purified oil; The concentrated slurry oil that is rich in catalyst returns the reaction zone participation reaction of paste state bed reactor or continues separation.
Wherein above-mentioned inoranic membrane separator 4 is made up of tubular type inoranic membrane and outer tube; It is the symmetry or the asymmetric membrane of pottery, metal or its composite formation of 2nm-100 μ m that inoranic membrane adopts average pore size.
Wherein said separation process is to be undertaken or realize by the membrane separator that places inside reactor by the external membrane separator.When separation process is undertaken by the external membrane separation, be provided with gas-liquid separator 2 and relay reservoir 3 between paste state bed reactor 1 and the membrane separator 4; The slurry oil that flows out paste state bed reactor 1 makes it pass through inoranic membrane separator 4 by product pump 5-1 pressurization, and concentrated slurry returns relay reservoir 3, forms recycle stream; Clean oil constantly sees through film and exports from clean oil outlet conduit 4-1, catalyst concn is by continuous enrichment in the slurry oil that does not see through, when the weight percentage of solid-phase catalyst reaches 0.1-30% in recycle stock, stop separation process, concentrated slurry returns paste state bed reactor 1 from middle basin 3 by pipeline 3-1; The concentrated slurry oil that flows out from inoranic membrane separator 4 returns pans or extracts a part of recirculation separation from the slurry oil that middle basin 3 is extracted out that directly imports by circulating pump 5-2.
When the separation process of slurry oil realizes by the membrane separator that places inside reactor, slurry oil aspirates under reaction self pressure or by negative pressure in the reactor, make the continuous inoranic membrane separator 4 back outflow reactors that place in the reactor that see through of liquid phase wherein, concentrate slurry oil and continue to participate in reaction by the reaction zone 7 that concentrated slurry oil pipeline 3-1 returns paste state bed reactor.
Separation process of the present invention can be divided into batch (-type) and continous way.Batch (-type) is that the film separation process is carried out after the reactor internal reaction finishes, in this cyclic process, liquid phase material is constantly exported from the side that sees through of film, the material that does not see through is by continuous enrichment, the solid catalysis agent content reaches 0.1-30% (weight) in recycle stock, stops separation process when filtering rate die-offs; This situation can feed reactor content a relay reservoir and carry out temperature-adjustment pressure-adjustment, also can directly carry out temperature-adjustment pressure-adjustment by reactor, makes material carry out aforesaid separation process subsequently between intermediate storage tank and membrane separator.
Continous way is that the film separation process of catalyst and the charging of reactor are carried out simultaneously continuously, promptly carry out synthetic reaction to the reactor continuous feed on one side, from reactor, extract material on one side and enter relay reservoir, the film that circulates separates, constantly separate liquid-phase product, constantly with isolated catalyst Returning reactor, continue to participate in synthetic reaction simultaneously.This method is by regulating the mean residence time that inoranic membrane sees through the interior material of rate of outflow control reactor of liquid.
Continuity method is applicable to generally and need growing quantity-produced occasion in one period that separation process stops with the end of catalytic reaction process.
, reduces the fenestra that prevents inoranic membrane membrane filtration efficient for stopping up, the present invention's timing or not timing ground adopt clean oil (or solvent naphtha) interval backflushing membrane separator, to come off attached to the catalyst on the face, import in the material that flows, thereby prevent that effectively film from polluting.
The present invention is coupled in the separation process and the catalytic reaction process of catalyst in the same system, promptly utilize the screening principle of inorganic separating film, the catalyst granules of solid phase is trapped within the reactor, and the liquid phase artificial oil continuously sees through the inoranic membrane outflow system, thereby realizes Separation of Solid and Liquid.
Beneficial effect
1, the present invention is on pop-jumpization of the raw material funds system artificial oil basis at existing coal or natural gas, does not change original reaction condition, adopts the inoranic membrane separating technology to separate and reclaims catalyst, makes in the material continuous-flow process and finishes Separation of Solid and Liquid.
2, solid catalyst in system, reacts-separates recovery-cyclic process of reaction more all the time, and technology is simple, the automaticity height, and energy consumption is low, environmentally safe.
3, owing to introduced the inoranic membrane isolation technics, solved the Separation of Solid and Liquid problem of fine powder suspension effectively, make the application in the artificial oil reaction of micron, sub-micron even nano level ultrafine solids catalyst become possibility, it is the solid catalyst of 2nm-100 μ m that thereby Fischer-Tropsch synthesis can adopt particle diameter, and the miniaturization of catalyst more helps the abundant dispersion in reaction mass, and the efficient of reaction is improved greatly.
4, greater than 99.5%, for example the inoranic membrane average pore size is 50nm to the rate of recovery of catalyst in the present invention, is that the rate of recovery of 100nm catalyst is 100% for average grain diameter; The inoranic membrane average pore size is 200nm; for average grain diameter be the rate of recovery of 800nm catalyst be 99.99% (the gravitational settling yield about 50～98%, the more little difficult more sedimentation of catalyst particle size, yield is low more; small size particle can be lost in the product, has a strong impact on product quality.), help the long-term stability operation of commercial plant.
Description of drawings
Fig. 1 is the flow chart of the Separation Process for Making Synthetic Catalyst with Slurry Bed Reactor of separated type.
Fig. 2 is the flow chart of the Separation Process for Making Synthetic Catalyst with Slurry Bed Reactor of integral type.
1 is paste state bed reactor among the figure, and 1-1 is a heater; 2 is gas-liquid separator, and 2-1 is a gas pipeline; 3 is pans, and 3-1 is for concentrating the slurry oil pipeline; 4 is membrane separator, and 4-1 is the clean oil outlet conduit; 5-1 feed pump, 5-2 are circulating pump; 6-1,6-2,6-3,6-4 are valve; The 7-reaction zone; The 8-gas-liquid separation zone; 9-slurry oil inlet; The 10-gas channel; A is a synthesis gas, and B is a gaseous products, and C is a clean oil.
The specific embodiment
As shown in Figure 1, paste state bed reactor 1 and membrane separator 4 be separated type, are provided with gas-liquid separator 2 and relay reservoir 3 therebetween; Synthesis gas enters and carries out preheating among the heater 1-1, enters then in the reactor 1 and reacts under 1.0～3.0MPa, and major product is gasoline and alkene under high temperature (300～350 ℃), and low temperature (180～250 ℃) is major product city diesel oil and wax down.During the normal running, slurries autoreactor are continuously extracted out, the reaction end gas of carrying secretly separates in gas-liquid separator 2, tail gas is back to reactor head through pipeline 2-1, the slurries that do not contain gas enter into pans 3 and carry out the temperature-adjustment pressure-adjustment processing, when pressure drop to 5 below the atmospheric pressure after, open valve 6-1,6-2,6-3,6-4, material enters in the membrane separator 4 under the effect of delivery pump 5-1 and circulating pump 5-2 and separates.Material circulation in the circulatory system that pans 3 and membrane separator 4 formed repeatedly, concentrate, when being concentrated to solid content when reaching 30%, separation process is finished, this moment first termination of pumping 5-1, termination of pumping 5-2 again, last shut off valve 6-1,6-2,6-3,6-4.The slurries that are rich in catalyst in the pans 3 are through pipeline 3-1 Returning reactor; Can be purified oil from membrane separator 4 per-meate side through pipeline 4-1, this clean oil can obtain oil product through conventional oil refining process.
As shown in Figure 2, membrane separator 4 places the inside of paste state bed reactor 1.Synthesis gas enters and carries out preheating among the heater 1-1, the reaction zone 7 that enters then in the reactor reacts, under the effect of catalyst, synthesis gas generation fischer-tropsch reaction generates artificial oil and carbon dioxide, product is being carried the part catalyst secretly through being distributed in reactor gas channel 10 all around, rise to gas-liquid separation zone 8, carbon dioxide and light component overflow from liquid, discharge from reactor head and obtain gaseous products.And the slurry oil of carrying catalyst secretly after the degassing 9 enters in the membrane separator 4 from entering the mouth, the solid catalyst tunicle is held back, reaction zone through pipeline 1-3 Returning reactor, liquid oils then sees through film, be purified oil through pipeline 4-1 outflow reactor, when membrane flux descends greatly, use clean oil (or solvent naphtha) that film is recoiled, the solid catalyst filter cake on film surface is come off, flux is got a promotion.Control valve 6-4 can control the clean oil flow, changes the pressure that can adjust the clean oil side according to reactor pressure, and the transmembrane pressure that changes the diffusion barrier both sides is poor.
Claims (8)
1. Separation Process for Making Synthetic Catalyst with Slurry Bed Reactor, Fischer-Tropsch synthesis method routinely, synthesis gas is fed paste state bed reactor (1) carry out catalytic reaction, the separation process that it is characterized in that the suspended state material is conveyed into inoranic membrane separator (4) for the slurry oil that paste state bed reactor (1) is included catalyst, utilize the sieving actoion of inoranic membrane, liquid artificial oil is wherein separated from slurry oil through inoranic membrane, be purified oil; The concentrated slurry oil that is rich in catalyst returns the reaction zone participation reaction of paste state bed reactor or continues separation.
2. separating technology according to claim 1 is characterized in that inoranic membrane separator (4) is made up of tubular type inoranic membrane and outer tube.
2. separating technology according to claim 1 is characterized in that it is the symmetry or the asymmetric membrane of pottery, metal or its composite formation of 2nm-100 μ m that said inoranic membrane adopts average pore size.
3. separating technology according to claim 1 is characterized in that separation process is to be undertaken or realize by the membrane separator that places inside reactor by the external membrane separator.
4. separating technology according to claim 3 is characterized in that reaction and separates when carrying out continuously, and separates when carrying out by external membrane, is provided with gas-liquid separator (2) and relay reservoir (3) between paste state bed reactor (1) and the inoranic membrane separator (4).
5. separating technology according to claim 4, the slurry oil that it is characterized in that flowing out paste state bed reactor (1) makes it pass through inoranic membrane separator (4) by product pump (5-1) pressurization, and concentrated slurry returns relay reservoir (3), forms recycle stream; Clean oil constantly sees through film and exports from clean oil outlet conduit 4-1, the slurry oil that does not see through is by continuous enrichment, when the weight percentage of solid-phase catalyst reaches 0.1-30% in recycle stock, stop separation process, concentrated slurry returns paste state bed reactor (1) from middle basin (3) by pipeline (3-1); The concentrated slurry oil that flows out from inoranic membrane separator (4) returns pans or extracts a part of recirculation separation from the slurry oil that middle basin (3) is extracted out that directly imports by circulating pump (5-2).
6. separating technology according to claim 3, it is characterized in that when the separation process of slurry oil realizes by the membrane separator that places inside reactor, slurry oil makes liquid phase wherein continuous in inoranic membrane separator (4) the back outflow reactor that places in the reactor under reaction self pressure or by the negative pressure suction in the reactor, concentrates slurry oil by concentrating reaction zone (7) the continuation participation reaction that slurry oil pipeline (3-1) returns paste state bed reactor.
7. separating technology according to claim 1 is characterized in that adopting clean oil or solvent naphtha interval backflushing membrane separator, will come off attached to the catalyst on the face, imports in the artificial oil that flows.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102151520A (en) * | 2010-12-21 | 2011-08-17 | 湘潭大学 | Gas-liquid-solid or liquid-solid heterogeneous catalytic reaction method |
| CN102728286A (en) * | 2012-07-17 | 2012-10-17 | 神华集团有限责任公司 | Slurry bed reaction equipment |
| CN101583405B (en) * | 2006-12-29 | 2012-12-19 | 雪佛龙美国公司 | A process for recovering ultrafine solids from a hydrocarbon liquid |
| CN103747861A (en) * | 2011-06-24 | 2014-04-23 | 安格斯化学公司 | Process and apparatus for production and filtration of aminoalcohols using a continuous stirred tank slurry reactor |
| CN102165042B (en) * | 2008-09-30 | 2014-05-07 | 日本石油天然气·金属矿物资源机构 | Catalyst separation system |
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| CN102009003B (en) * | 2009-09-07 | 2013-02-06 | 中国石油化工股份有限公司 | Slurry-bed reaction and separation system and method as well as application thereof in Fischer-Tropsch synthesis technology |
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| US5253403A (en) * | 1992-05-04 | 1993-10-19 | Mcdermott International, Inc. | On-stream time for ebullating bed reactor |
| CN1201842C (en) * | 2003-01-28 | 2005-05-18 | 中国石油化工集团公司 | Method and equipment for separating synthetic oil and catalyst in slurry reactor |
| CN1219569C (en) * | 2004-03-19 | 2005-09-21 | 中国科学院山西煤炭化学研究所 | Method of separating and reclaiming spent cobalt based catalyst and heavy hydrocarbon throuth Fishcher-Tropsch synthesis in slurry bed |
| CN100532974C (en) * | 2004-03-26 | 2009-08-26 | 陈新祥 | Air conditioner and water heater integrated machine having double compressor |
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| CN101583405B (en) * | 2006-12-29 | 2012-12-19 | 雪佛龙美国公司 | A process for recovering ultrafine solids from a hydrocarbon liquid |
| CN102165042B (en) * | 2008-09-30 | 2014-05-07 | 日本石油天然气·金属矿物资源机构 | Catalyst separation system |
| US9139779B2 (en) | 2008-09-30 | 2015-09-22 | Japan Oil, Gas And Metals National Corporation | Catalyst separation system |
| CN102151520A (en) * | 2010-12-21 | 2011-08-17 | 湘潭大学 | Gas-liquid-solid or liquid-solid heterogeneous catalytic reaction method |
| CN103747861A (en) * | 2011-06-24 | 2014-04-23 | 安格斯化学公司 | Process and apparatus for production and filtration of aminoalcohols using a continuous stirred tank slurry reactor |
| US9211518B2 (en) | 2011-06-24 | 2015-12-15 | Angus Chemical Company | Process and apparatus for production and filtration of aminoalcohols using a continuous stirred tank slurry reactor |
| CN103747861B (en) * | 2011-06-24 | 2016-08-31 | 安格斯化学公司 | Use the method and apparatus being used for producing and filter amino alcohol of continuous stirred tank slurry reactor |
| CN102728286A (en) * | 2012-07-17 | 2012-10-17 | 神华集团有限责任公司 | Slurry bed reaction equipment |
| CN102728286B (en) * | 2012-07-17 | 2015-06-17 | 神华集团有限责任公司 | Slurry bed reaction equipment |
| CN103846162A (en) * | 2012-11-30 | 2014-06-11 | 中国石油化工股份有限公司 | Liquid solid magnetic separation method |
| CN103846162B (en) * | 2012-11-30 | 2016-12-21 | 中国石油化工股份有限公司 | A kind of liquid-solid magnetism separate method |
| CN111996026A (en) * | 2020-07-30 | 2020-11-27 | 国家能源集团宁夏煤业有限责任公司 | Method and system for catalyst distribution in slurry bed reactor |
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| CN1319635C (en) | 2007-06-06 |
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Assignee: NANJING JIUSI HIGH-TECH Co.,Ltd. Assignor: Nanjing Tech University Contract fulfillment period: 2007.7.1 to 2017.7.1 Contract record no.: 2008320000317 Denomination of invention: Separation process of synthetic oil catalyst prepared in slurry bed reactor Granted publication date: 20070606 License type: Exclusive license Record date: 20080924 |
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Free format text: EXCLUSIVE LICENCE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.7.1 TO 2017.7.1 Name of requester: NANJING JIUSI HIGH-TECH CO., LTD. Effective date: 20080924 |