CN104593047A - Adsorption desulphurization reaction apparatus and adsorption desulphurization method - Google Patents
Adsorption desulphurization reaction apparatus and adsorption desulphurization method Download PDFInfo
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- CN104593047A CN104593047A CN201310528725.3A CN201310528725A CN104593047A CN 104593047 A CN104593047 A CN 104593047A CN 201310528725 A CN201310528725 A CN 201310528725A CN 104593047 A CN104593047 A CN 104593047A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/14—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing with moving solid particles
- C10G45/20—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing with moving solid particles according to the "fluidised-bed" technique
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00761—Discharging
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Combustion & Propulsion (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention provides an adsorption desulphurization reaction apparatus and an adsorption desulphurization method. The adsorption desulphurization reaction apparatus comprises a fluidized bed reactor, a filter arranged outside the fluidized bed reactor, and a spent-catalyst regeneration unit; a cyclone separator arranged in the fluidized bed reactor possesses at least two material introduction channels, and a ratio of the total area of a cross section of each material introduction channel along a direction perpendicular to the material flow direction to the area of a horizontal cross section of a separation segment of the fluidized bed reactor is 1:3-30. The adsorption desulphurization reaction apparatus is capable of timely transferring out a catalyst fine powder in the fluidized bed reactor, avoiding accumulation of the catalyst fine powder in the fluidized bed reactor and keeping stable long-term operation, thereby obtaining good and stable reaction effect. Also, the cyclone separator employed in the fluidized bed reactor is small in wearing on the catalyst particle, and is capable of obviously reducing consumption of the catalyst, thereby reducing operation cost of the apparatus.
Description
Technical field
The present invention relates to a kind of adsorption desulfurize reaction unit, the invention still further relates to a kind of desulfurizing method by adsorption.
Background technology
Raising along with people's living standard and the pay attention to day by day to environment protection, the standard-required of countries in the world to clean fuel is more and more higher, also more and more stricter to the sulphur content restriction in fuel.Therefore, domestic and international researchist develops the technology of sulphur content in various deep removal hydrocarbon ils one after another.
The main method of traditional fuel oil desulfurization is hydrogenating desulfurization, but along with the increasingly stringent of standard of fuel, hydrogenation depth improves, and needs harsher reaction conditions, as higher reaction pressure etc.Meanwhile, for gasoline, due to containing a large amount of alkene, improving hydrogenation severity will cause higher loss of octane number, and therefore some new sulfur methods continue to bring out, wherein especially of greatest concern with adsorption desulfurize.The industrial application of adsorption desulfurize (as S Zorb technique) shows, this technology has the features such as desulfurization depth is high, hydrogen consumption is low, loss of octane number is little, oil refining enterprise can be met and produce the demand meeting the gasoline blending component of Europe V, even higher standard, make this technology have vast potential for future development.
CN1323749C discloses a kind of hydrocarbon sweetening system using renewable solid sorbent particles in fluid-bed sweetening reactor.Take out continuously from reactor and be loaded with the absorbent particles of sulphur, and transferred in revivifier and regenerate, the sorbent material after regeneration returns in reactor after reduction, realizes carrying out continuously of adsorption desulfurize.Solid Conveying and Melting mechanism disclosed in CN1323749C to provide the absorbent particles of sulfur-loaded through locking hopper from the high pressure hydrocarbon environment of reactor to the safety of the low pressure oxygen environment of revivifier and effectively transfer.But, in actual application, there is the problem that adsorbent fines is assembled in reactor head, affect operational stability and the long-term operation of device.
CN101780389A and CN201454508U discloses a kind of fluidized-bed reactor for gasoline absorbing desulfurization, the strainer with automatic back-flushing device is provided with at the top of this fluidized-bed reactor, dust settler is provided with below strainer, the use of this dust settler can effectively reduce need fine powder content in the gas of filter process, thus reduce the load of strainer, effectively extend the recoil interval of automatic back-flushing device, reduce investment and the maintenance cost of equipment.The dust settler used can be adopt the blocking type of conical structure or adopt the whirlwind-type of twisted blade structure.Adsorbent fines content that gas in fluidized-bed carries is about 30% to adopt blocking type dust settler to reduce, and whirlwind-type dust settler can reduce the adsorbent fines content that gas in fluidized-bed carries and is about 22%.Although the use of dust settler can reduce the blowback frequency of strainer to a certain extent, but adsorbent fines major part is still detained the middle and upper part of sorbent material wound layer in the reactor, and accumulate along with the increase of plant running time, thus the efficiency of dust settler is constantly declined, the blowback interval of strainer shortens thereupon, affects the plant running cycle.
Conventional fluidization bed bioreactor arranges cyclonic separator usually to reclaim solid particulate at top.But generally revolve point separator requirement and enter the gas speed of cyclonic separator in the scope of 15-25m/s, height enters implication speed and is no doubt conducive to improving gas-solid efficiency, but can increase the wearing and tearing of particle.And gasoline absorbing desulfurization used catalyst physical strength is lower, if arrange traditional cyclonic separator in fluidized absorption reactor, then comparatively large because entering implication speed, the wearing and tearing of granules of catalyst can be aggravated, and then greatly improve the running cost of device.
Therefore, need to provide a kind of new adsorption desulfurize reaction unit, this device can not only realize adsorption desulfurize, and the adsorbent fines formed in reactor can be shifted out reaction system in time, reduce the adsorbent fines amount in reactor, the wearing and tearing of absorbent particles can not be aggravated, stable, the long-term operation of implement device simultaneously.
Summary of the invention
The object of the invention is to overcome existing adsorption desulfurize reaction unit be difficult in time adsorbent fines be shifted out fluidized-bed reactor, affect stability and the security of plant running, shorten the technical problem of device stable operation cycle, a kind of adsorption desulfurize reaction unit is provided, adsorbent fines in fluidized-bed reactor can be shifted out fluidized-bed reactor by this device in time, the stable operation cycle of extension fixture, also can not aggravate the wearing and tearing of absorbent particles simultaneously.
The invention provides a kind of adsorption desulfurize reaction unit, this device comprises fluidized-bed reactor, is arranged on strainer and the spent agent regeneration unit of described fluidized-bed reactor outside, and described fluidized-bed reactor is used for sulfur-bearing hydrocarbon feed and hydrogen and the adsorbent contact with adsorption desulfurize effect;
Described fluidized-bed reactor comprises the reactor body of sealing, air outlet tube and the spent agent be arranged in described reactor body upper portion side wall exports inclined tube, the internal space of described reactor body comprises segregation section, settling section, conversion zone and feed zone from top to bottom successively, is provided with at least one cyclonic separator in described segregation section;
Described cyclonic separator comprises the hollow body of sealing, solid materials derives passage and at least two material introduction channels, the internal space of described hollow body comprises straight tube district and pyramidal area from top to bottom successively, described material introduction channel is tangentially arranged in the exterior side wall in described straight tube district, enter in described straight tube district to make the oil agent mixture in described segregation section by described material introduction channel, described material introduction channel is 1:3-30 along the ratio of the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of described segregation section, the bottom that passage is positioned at described pyramidal area derived by described material,
Described air outlet tube is arranged on the top of at least one cyclonic separator, the two ends of described air outlet tube are communicated with the air flow inlet of described strainer with the internal space of this cyclonic separator respectively, so that isolated for this cyclonic separator gas-oil mixture is sent fluidized-bed reactor, and in described strainer, the adsorbent fines in described gas-oil mixture is separated;
Described spent agent regeneration unit is used for the spent agent being exported inclined tube output by spent agent to carry out regenerating and reducing, and is sent back in described fluidized-bed reactor by reductive agent.
The invention still further relates to a kind of desulfurizing method by adsorption, the method is carried out in adsorption desulfurize reaction unit provided by the invention, comprising:
Contact containing sulfur-bearing hydrocarbon feed in the conversion zone of described fluidized-bed reactor with the sorbent material with adsorption desulfurize effect with the oil gas raw material of hydrogen, to remove at least part of element sulphur in described sulfur-bearing hydrocarbon feed;
The oil agent mixture that fluidized-bed reactor exports is separated in the filter, to isolate the adsorbent fines in described oil agent mixture, obtains oil gas product;
The spent agent being exported inclined tube output by spent agent is carried out regenerating and reducing in spent agent regeneration unit, and reductive agent is sent back in the conversion zone of described fluidized-bed reactor.
Catalyst fines in fluidized-bed reactor can be shifted out in time according to adsorption desulfurize reaction unit of the present invention, avoid catalyst fines accumulation in a fluidized bed reactor, make reaction unit to stablize long-term operation, thus obtain good and stable reaction effect.
Further, the wearing and tearing of the cyclonic separator used in fluidized-bed reactor of the present invention to granules of catalyst are little, obviously can reduce the consumption of catalyzer, thus reduce the running cost of device.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
Fig. 1 is for illustration of a kind of embodiment of adsorption desulfurize reaction unit according to the present invention.
Fig. 2 is for illustration of a kind of embodiment of the cyclonic separator used in adsorption desulfurize reaction unit according to the present invention.
Description of reference numerals
1: reactor body 101: segregation section
102: settling section 103: conversion zone
104: feed zone 2: air outlet tube
3: spent agent exports inclined tube 4: cyclonic separator
41: hollow body 411: straight tube district
412: pyramidal area 42: material introduction channel
43: solid materials derives passage 44: the first cyclonic separator
45: the second cyclonic separators 441: solid materials derives passage
451: solid materials derives passage 5: oil gas feed(raw material)inlet
6: gas distribution dish 7: reductive agent input inclined tube
8: bunker for collecting 9: collection chamber
10: spent agent receptor 11: feeder
12: collection chamber 100: fluidized-bed reactor
200: strainer 201: air flow inlet
202: agent structure 203: fillter section
204: collection section 205: filtering element
206: oil gas product exit 207: reclaim sorbent material output tube
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of adsorption desulfurize reaction unit, as shown in Figure 1, this adsorption desulfurize reaction unit comprises fluidized-bed reactor 100, is arranged on the strainer 200 of described fluidized-bed reactor outside and spent agent regeneration unit (not shown).
Described fluidized-bed reactor is used for sulfur-bearing hydrocarbon feed and hydrogen and the adsorbent contact with adsorption desulfurize effect.As shown in Figure 1, fluidized-bed reactor 100 comprises the reactor body 1 of sealing, air outlet tube 2 and the spent agent be arranged in reactor body 1 upper portion side wall exports inclined tube 3, and the internal space of reactor body 1 comprises segregation section 101, settling section 102, conversion zone 103 and feed zone 104 from top to bottom successively.
Described reactor body can be conventional shape, is generally cylindrical shape.The size of described segregation section, settling section and conversion zone can be conventional selection.Usually, the aspect ratio of described segregation section and described conversion zone can be 0.1-0.2:1.The area ratio of the area of the horizontal section of described segregation section and the horizontal section of described conversion zone can be 1.2-2.5:1.Angle between the outer contour of described settling section and horizontal plane can be 60-75 °.
Described spent agent exports inclined tube and is used for the sorbent material reduced active in conversion zone to send fluidized-bed reactor, to carry out regenerating and reducing.As shown in Figure 1, spent agent exports the conversion zone 103 that one end of inclined tube 3 is positioned at fluidized-bed reactor 100, and the sidewall of the reactor body 1 of the other end hermetically passing fluidized-bed reactor 100 also extends to the outside of fluidized-bed reactor 100.Spent agent is exported inclined tube 3 and is generally communicated with revivifier (not shown) by spent agent receptor 10.From the further angle improving the conveying smoothness of spent agent receptor, as shown in Figure 1, the passage be communicated with the internal space of fluidized-bed reactor 100 is preferably set at the top of spent agent receptor 10, the internal space of the internal space of spent agent receptor 10 with fluidized-bed reactor 100 is communicated with.
As shown in Figure 1, at least one cyclonic separator 4 is provided with in segregation section 101.As shown in Figure 2, cyclonic separator 4 comprises the hollow body 41 of sealing, solid materials derives passage 43 and at least two material introduction channels 42, the internal space of hollow body 41 comprises straight tube district 411 and pyramidal area 412 from top to bottom successively, material introduction channel 42 is tangentially arranged in the exterior side wall in straight tube district 411, is entered in straight tube district 411 by material introduction channel 42 to make the oil agent mixture in segregation section 101.Described " tangentially " refers to the tangential direction of the exterior side wall along straight tube district.
The quantity of described material introduction channel is at least two, is preferably 3-6.Described material introduction channel is evenly arrange at the circumferential direction of the exterior side wall in described straight tube district.Each material introduction channel along being identical perpendicular to the area in the cross section of flow direction of material.The height of passage in straight tube district derived by described material can be conventional selection, is not particularly limited.
Described material introduction channel is 1:3-30 along the ratio of the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of described segregation section.Can be lower speed by the speed control entering the air-flow of cyclonic separator like this, thus reduce the degree of wear to sorbent material.Guaranteeing under the prerequisite that the separation efficiency of cyclonic separator can meet the demands, from the angle reduced further the degree of wear of sorbent material, described material introduction channel is preferably 1:5-25 along the ratio of the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of described segregation section.Along the total area perpendicular to the cross section of air flow direction, described material introduction channel refers to that whole material introduction channel is along the summation perpendicular to the area in the cross section of air flow direction.
In the preferred embodiment of the present invention, each material introduction channel is A along the area perpendicular to the cross section of flow direction of material
1, the area of the horizontal section in described straight tube district is A
2, A
2/ A
1=1-10.Better separating effect can either be obtained like this, the degree of wear of solid particulate in sepn process can be reduced again further.Preferably, A
2/ A
1=2-8.
The shape in the cross section along flow direction of material of material introduction channel is not particularly limited, and can be conventional selection, be generally square.
As shown in Figure 2, cyclonic separator 4 also comprises the solid materials be arranged on bottom pyramidal area 412 derives passage 43.From the isolated solid particulate of cyclonic separator, as the case may be, can again send in conversion zone, also can export inclined tube by spent agent and send in spent agent regeneration unit and carry out regenerating, send in the conversion zone of fluidized-bed reactor after sorting and reduction.Therefore, the solid materials of described cyclonic separator is derived passage and can be extended in conversion zone, also can export inclined tube with spent agent and be communicated with.
The quantity of described cyclonic separator can be 1, also can be multiple.Preferably, the quantity of described cyclonic separator is 2-6.When the quantity of described cyclonic separator is multiple, preferably cyclonic separator series connection is used, the separating effect improved further can be obtained like this.
Described air outlet tube is used for isolated for described cyclonic separator gas-oil mixture to send fluidized-bed reactor, and the adsorbent fines in described gas-oil mixture is separated in described strainer.Described air outlet tube can be arranged on the top of described cyclonic separator, and the two ends of air outlet tube are communicated with the air flow inlet of described strainer with the internal space of cyclonic separator respectively.When the quantity of described cyclonic separator is multiple, quantity and the position of airduct can be determined according to the annexation of cyclonic separator.Particularly, multiple cyclonic separator be plural serial stage connect time, described air outlet tube can be set for the top of in the end primary cyclone.
Conventional various methods can be adopted to be communicated with the air flow inlet of strainer with the internal space of cyclonic separator respectively at the two ends of air outlet tube.In one embodiment of the invention, as shown in Figure 1, collection chamber 9 can be set at the top of fluidized-bed reactor, collection chamber 9 is communicated with the air flow inlet 201 of strainer 200 with air outlet tube 2 respectively, and the gas-oil mixture exported from air outlet tube 2 so just can be entered the air flow inlet 201 of strainer 200 by collection chamber 9.
The output speed of cross-sectional area on isolated oil gas product of described air outlet tube has impact, also has certain regulating effect to the movement velocity of air-flow in strainer simultaneously.In the preferred embodiment of the present invention, the area of the horizontal section in described straight tube district is A
2, described air outlet tube along being A perpendicular to the area in the cross section of air flow direction
3, A
3/ A
2=0.2-0.8.Like this while isolated for cyclonic separator gas-oil mixture can being sent fluidized-bed reactor in time, reduce the degree of wear to solid particulate further.Preferably, A
3/ A
2=0.3-0.5.
One of the present invention preferred embodiment in, as shown in Figure 1, cyclonic separator 4 comprises the first cyclonic separator 44 and the second cyclonic separator 45, the air stream outlet of the first cyclonic separator 44 is communicated with the material introduction channel of the second cyclonic separator 45, the solid materials of the first cyclonic separator 44 is derived passage 441 and is extended downward in conversion zone 103, the solid materials derivation passage 451 of the second cyclonic separator 45 exports inclined tube 3 with spent agent and is communicated with, and air outlet tube 2 is positioned at the top of the second cyclonic separator 45 and is connected with the internal space of the second cyclonic separator 45.Can return in conversion zone 103 by the isolated larger-size absorbent particles of the first cyclonic separator 44 like this, then can export inclined tube 3 by spent agent by the absorbent particles that the isolated size of the second cyclonic separator 45 is less to export, thus can the size distribution of sorbent material in fluid bedreactors regulate.
This preferred embodiment in, the quantity of described first cyclonic separator is preferably identical with the quantity of the material introduction channel of described second cyclonic separator, and more preferably each material introduction channel of described second cyclonic separator is respectively communicated with the air stream outlet of first cyclonic separator.Particularly, the material introduction channel of described second cyclonic separator and the quantity of described first cyclonic separator are 2, and each material introduction channel of described second cyclonic separator respectively connects with first cyclonic separator.
This preferred embodiment in, as shown in Figure 1, bunker for collecting 8 can be set on the upper inner wall of the conversion zone 103 of fluidized-bed reactor 100, bunker for collecting 8 and spent agent export inclined tube 3 and are communicated with, bunker for collecting 8 is for receiving from the less absorbent particles of the size of solid materials derivation passage 451 output of the second cyclonic separator 45, and the absorbent particles of reception is sent in spent agent receptor 10 by spent agent output inclined tube 3, the material outlet of spent agent receptor 10 is communicated with the spent agent entrance of revivifier.
As shown in Figure 1, the bottom of the feed zone 104 of reactor body 1 is provided with oil gas feed(raw material)inlet 5 and gas distributing disc 6.Described oil gas feed(raw material)inlet is used for oil gas raw material to send in fluidized-bed reactor, and described gas distribution dish enters conversion zone equably for making the oil gas raw material entered by oil gas feed(raw material)inlet.The specific form of described gas distribution dish can be the routine selection of this area, no longer describes in detail herein.
As shown in Figure 1, the lower outside wall of reactor body 1 is also provided with reductive agent input inclined tube 7, the sidewall of reductive agent input inclined tube 7 hermetically passing reactor body 1 is communicated with conversion zone 103, for being sent in conversion zone 103 by reductive agent.
Described strainer, for separating of going out the adsorbent fines of carrying secretly in the gas-oil mixture of fluidized-bed reactor output, obtains oil gas product, and isolated adsorbent fines is sent in adsorbent fines holding tank.Described strainer can for the conventional various strainers can isolating oil gas product from the gas-oil mixture being entrained with adsorbent fines.
Particularly, as shown in Figure 1, strainer 200 can comprise the agent structure 202 for sealed hollow structure, the internal space of this agent structure 202 comprises fillter section 203 and collection section 204 from top to bottom, the top (preferred top) of fillter section 203 is provided with filtering element 205, adsorbent fines is wherein separated by filtering element 205 by the gas-oil mixture entering strainer 200, the oil gas product obtained is sent in follow-up processing unit by the oil gas product exit 206 being arranged on agent structure 202 top, isolated adsorbent fines then falls in collection section 204 under gravity, and send in adsorbent fines holding tank (not shown) eventually through the recovery sorbent material output tube 207 be arranged on bottom collection section 204.
Described filtering element can be the various element can isolating solid fines from air-flow, as wire cloth or metal filter candle.
Preferably, described strainer also has blow device, purges for the regular filtering element to strainer, to make the fine powder be deposited on described filtering element blow off, prevents filtering element blocked.Described blow device can for the common various devices that can realize above-mentioned functions, such as: when inside and outside filtering element, resistance drop reaches certain value, the dust blowback concussion be deposited on filtering element to pulse backblowing pressurized air in filtering element, can remove by described blow device.
As shown in Figure 1, collection chamber 12 can be set at the top of strainer 200, and oil gas product exit 206 is communicated with collection chamber 12, collection chamber 12 for collecting from the isolated oil gas product of filtering element 205, and makes oil gas product be exported by oil gas product exit 206 further.
Described spent agent regeneration unit is used for the spent agent being exported inclined tube output by spent agent to carry out regenerating and reducing, and is sent back in described fluidized-bed reactor by reductive agent.Usually, described spent agent regeneration unit can comprise revivifier and reducer.
Spent agent entrance and the described spent agent of described revivifier export inclined tube and are communicated with, the regenerator outlet of described revivifier is communicated with described reducer, for the spent agent regeneration that described fluidized-bed reactor is exported, and at least part of regenerator obtained is sent in described reducer.
The reductive agent outlet of described reducer is communicated with the feed zone of described fluidized-bed reactor, for being reduced by regenerator, and is sent into by least part of reductive agent in the conversion zone of described fluidized-bed reactor.In actual mechanical process, can be as shown in Figure 1, feeder 11 can be set, by the sorbent material entrance of feeder 11 and the reductive agent outlet of reducer, the adsorbent outlet of feeder 11 and reductive agent are inputted inclined tube 7 be communicated with, thus the reductive agent circulation exported by reducer is sent in fluidized-bed reactor.
The structure of described revivifier and reducer can be the routine selection of this area, no longer describes in detail herein.
Present invention also offers a kind of desulfurizing method by adsorption, the method is carried out in adsorption desulfurize reaction unit provided by the invention, comprising:
Contact containing sulfur-bearing hydrocarbon feed in the conversion zone of described fluidized-bed reactor with the sorbent material with adsorption desulfurize effect with the oil gas raw material of hydrogen, to remove at least part of element sulphur in described sulfur-bearing hydrocarbon feed;
The oil agent mixture that fluidized-bed reactor exports is separated in the filter, to isolate the adsorbent fines in described oil agent mixture, obtains oil gas product;
The spent agent being exported inclined tube output by spent agent is carried out regenerating and reducing in spent agent regeneration unit, and reductive agent is sent back in the conversion zone of described fluidized-bed reactor.
Described adsorption desulfurize reaction unit and structure thereof have been described in detail above, no longer describe in detail herein.
Described sulfur-bearing hydrocarbon feed can need for common various in this area the sulfur-bearing hydrocarbon feed carrying out adsorption desulfurize.Preferably, described sulfur-bearing hydrocarbon feed is one or more in straight-run spirit, catalytic gasoline and coker gasoline.
The various sorbent materials with adsorption desulfurize effect that the described sorbent material with adsorption desulfurize effect can be commonly used for this area, are preferably the sorbent material with adsorption desulfurize effect using zinc oxide as active ingredient.Such as can for having the sorbent material of adsorption desulfurize effect disclosed in CN1208124C and CN1331591C.
The described granularity with the sorbent material of adsorption desulfurize effect can be selected for conventional, is as the criterion can realize fluidisation.Usually, the granularity described in the sorbent material of adsorption desulfurize effect can be 20-150 micron.In the present invention, the granularity of sorbent material is volume average particle sizes, adopts laser particle size analyzer to measure.
Described sulfur-bearing hydrocarbon feed and the described contact with the sorbent material of adsorption desulfurize effect are carried out in the atmosphere of hydrogen.Hydrogen can be sent into the conversion zone of fluidized-bed reactor from the oil gas feed(raw material)inlet bottom described fluidized-bed reactor together with sulfur-bearing hydrocarbon feed.The consumption of described hydrogen can be the routine selection of this area.Usually, in described oil gas raw material, the mol ratio of hydrogen and sulfur-bearing hydrocarbon feed can be 0.1-2:1, is preferably 0.15-1.5:1, is more preferably 0.2-1:1.
Enter oil gas raw material in fluidized-bed reactor in the process risen, hold up adsorbent bed and fully react with it.The riser speed of oil gas raw material is preferably 0.01-1 meter per second, be more preferably 0.1-0.8 meter per second, the air-flow in segregation section can be made like this to enter cyclonic separator (when cyclonic separator is plural serial stage connection with the linear velocity of 2-10 meter per second (as 3-8 meter per second) by material introduction channel, for entering first step cyclonic separator), the degree of wear of the low absorbent particles of a step-down thus the separating effect obtaining raising is further gone forward side by side.
Sulfur-bearing hydrocarbon feed is not particularly limited with the condition of the adsorbent contact with adsorption desulfurize effect, can carry out, be as the criterion the element sulphur in described sulfur-bearing hydrocarbon feed can be removed to meet the demands under the normal condition of this area.Usually, the temperature of described contact can be 300-500 DEG C, is preferably 320-480 DEG C; In gauge pressure, the pressure in described fluidized-bed reactor can be 0.5-5MPa, is preferably 1-4.5MPa.
Sorbent material to be generated can be regenerated under normal conditions, such as, method can regenerate disclosed in CN1323137C.Particularly, sorbent material to be generated can be regenerated in oxygen-containing atmosphere, the condition of described regeneration comprises: temperature can be 350-650 DEG C; In absolute pressure, pressure can be 240-1134kPa; The superficial linear vilocity of oxygen-containing gas can be 0.3-1.5m/s.
Regenerator can be reduced under normal conditions.Usually, can contact with the gas of hydrogen by making regenerator, thus regenerator is reduced, obtain reductive agent.The condition of described reduction comprises: temperature can be 300-550 DEG C; In absolute pressure, pressure can be 800-3000kPa; The superficial linear vilocity of hydrogen-containing gas can be 0.1-2m/s.The consumption of described hydrogen is can be as the criterion the sorbent material reduction after regeneration.
The present invention is described in detail below in conjunction with embodiment.
In following examples and comparative example, if not otherwise specified, use the adsorpting desulfurization device shown in Fig. 1, wherein, the reactor body of fluidized-bed reactor is cylindric, the segregation section of fluidized-bed reactor and the aspect ratio of conversion zone are 0.1:1, and the area ratio of the area of the horizontal section of segregation section and the horizontal section of conversion zone is 1.5:1, and the angle between the outer contour of settling section and horizontal plane is 70 °.
In following examples and comparative example, adopt the laser particle size analyzer be purchased from Malvern company to measure granularity and mean particle size, wherein, mean particle size is volume average particle sizes.
Embodiment 1-2 is for illustration of the present invention.
Embodiment 1
In the present embodiment, cyclonic separator comprises the first cyclonic separator and the second cyclonic separator, the material introduction channel of described second cyclonic separator and the quantity of the first cyclonic separator are 2, and each material introduction channel of the first cyclonic separator respectively connects with first cyclonic separator.
In the cyclonic separator used, the cross section of material introduction channel is square, and along the tangential setting of the hollow body of cyclonic separator, and the quantity of material introduction channel is 3,3 material introduction channels along the circumference of the exterior side wall in straight tube district for being symmetrical arranged; The ratio along the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of segregation section of material introduction channel is 1:5; Each material introduction channel along being A perpendicular to the area in the cross section of air flow direction
1, the area of the horizontal section in straight tube district is A
2, A
2/ A
1=3; The area in the cross section along vertical and air flow direction of air outlet tube is A
3, A
3/ A
2=0.3.
As shown in Figure 1, (be sour gasoline by sulfur-bearing hydrocarbon feed, character is listed in Table 1) and hydrogen enter in fluidized-bed reactor with the mol ratio of 4:1 by oil gas feed(raw material)inlet 5, and enter in conversion zone 103 by gas distribution dish 6, (produced by Research Institute of Petro-Chemical Engineering of China Petrochemical Industry with the sorbent material with adsorption desulfurize effect, its character is listed in table 2) contact reacts, to remove at least part of element sulphur in hydrocarbon feed.Wherein, the temperature of contact is 430 DEG C, and in gauge pressure, pressure is 0.25MPa, and the riser speed of mixture in conversion zone of sulfur-bearing hydrocarbon feed and hydrogen is 0.3m/s.
From conversion zone 103 export oil agent mixture through settling section 102 carry out settlement separate after, enter in the first cyclonic separator 44 and be separated, isolated absorbent particles returns in conversion zone 103; The air-flow exported by the first cyclonic separator 44 then enters in the second cyclonic separator 45 and is separated further, by the isolated adsorbent fines of the second cyclonic separator 45 by spent agent export inclined tube 3 enter carry out regeneration and sorting in revivifier after enter in reducer and reduce, and again in feeding fluidized-bed reactor.Entered in strainer 200 by air outlet tube 2 by the isolated gas-oil mixture of the second cyclonic separator 45, filter out the adsorbent fines in gas-oil mixture, obtain oil gas product, isolated adsorbent fines is sent in adsorbent fines holding tank.
Wherein, oil agent mixture is 4.5m/s in the linear velocity at the material introduction channel place of the first cyclonic separator.
Wherein, the condition of regeneration comprises: temperature is 510 DEG C; In absolute pressure, pressure is 400kPa; The superficial linear vilocity of oxygen-containing gas is 0.45m/s; The condition of reduction comprises: temperature is 400 DEG C; In absolute pressure, pressure is 3000kPa; The superficial linear vilocity of hydrogen-containing gas is 0.4m/s.
Carry out 500 hours continuously.In reaction process, monitor the composition of the oil gas product obtained, result is listed in table 3.React after 500 hours, the amount being gathered in the adsorbent fines at fluidized-bed reactor top is 15kg, and in the catalyzer in the sorbent material dense-phase bed in fluidized-bed reactor, the content that granularity is less than the catalyzer of 30 μm is 8 % by weight.Load 2000kg catalyzer altogether in a fluidized bed reactor before reaction starts, in reaction process, in fluidized-bed reactor, supplement 50kg catalyzer altogether; 35kg catalyst fines is collected in 500 hours rear catalyst fine powder storage tanks.
Table 1
Table 2
Table 3
*: using the anti-knock index of the sour gasoline as hydrocarbon feed for benchmark, wherein, anti-knock index=(RON+MON)/2
Embodiment 2
Adopt the method identical with embodiment 1 to carry out adsorption desulfurize, unlike: the quantity of material introduction channel is 2,2 material introduction channels along the circumference of the exterior side wall in straight tube district for being symmetrical arranged; The ratio along the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of segregation section of material introduction channel is 1:24, A
2/ A
1=6, A
3/ A
2=0.5;
The linear velocity of mixture in conversion zone of sulfur-bearing hydrocarbon feed and hydrogen is 0.5m/s;
Oil agent mixture is 8m/s in the linear velocity at the material introduction channel place of the first cyclonic separator.
Carry out 500 hours continuously.In reaction process, monitor the composition of the oil gas product obtained, result is listed in table 4.
React after 500 hours, the amount being gathered in the adsorbent fines at fluidized-bed reactor top is 12kg, and in the catalyzer in the sorbent material dense-phase bed in fluidized-bed reactor, the content that granularity is less than the catalyzer of 30 μm is 9 % by weight.Load 2000kg catalyzer altogether in a fluidized bed reactor before reaction starts, in reaction process, in fluidized-bed reactor, supplement 50kg catalyzer altogether; 38kg catalyst fines is collected in 500 hours rear catalyst fine powder storage tanks.
Table 4
*: using the anti-knock index of the sour gasoline as hydrocarbon feed for benchmark, wherein, anti-knock index=(RON+MON)/2
Comparative example 1
The method identical with embodiment 2 is adopted to carry out adsorption desulfurize, unlike: the ratio 1:35 along the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of segregation section of material introduction channel, A
2/ A
1=12:1, A
3/ A
2=0.1;
Oil agent mixture is 15m/s in the linear velocity at the material introduction channel place of the first cyclonic separator.
Carry out 500 hours continuously.In reaction process, monitor the composition of the oil gas product obtained, result is listed in table 5.React after 500 hours, the amount being gathered in the adsorbent fines at fluidized-bed reactor top is 50kg, and in the catalyzer in the sorbent material dense-phase bed in fluidized-bed reactor, the content that granularity is less than the catalyzer of 30 μm is 25 % by weight.Load 2000kg catalyzer altogether in a fluidized bed reactor before reaction starts, in reaction process, in fluidized-bed reactor, supplement 150kg catalyzer altogether; 100kg catalyst fines is collected in 500 hours rear catalyst fine powder storage tanks.
Table 5
*: using the anti-knock index of the sour gasoline as hydrocarbon feed for benchmark, wherein, anti-knock index=(RON+MON)/2
The result of embodiment 1 and 2 and comparative example 1 confirms, adsorption desulfurize reaction unit of the present invention is adopted to carry out adsorption desulfurize, in time the adsorbent fines in fluidized-bed reactor can be shifted out, and little to the wearing and tearing of sorbent material, and device can long period safe and stable operation.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (15)
1. an adsorption desulfurize reaction unit, this device comprises fluidized-bed reactor, is arranged on strainer and the spent agent regeneration unit of described fluidized-bed reactor outside, and described fluidized-bed reactor is used for sulfur-bearing hydrocarbon feed and hydrogen and the adsorbent contact with adsorption desulfurize effect;
Described fluidized-bed reactor comprises the reactor body of sealing, air outlet tube and the spent agent be arranged in described reactor body upper portion side wall exports inclined tube, the internal space of described reactor body comprises segregation section, settling section, conversion zone and feed zone from top to bottom successively, is provided with at least one cyclonic separator in described segregation section;
Described cyclonic separator comprises the hollow body of sealing, solid materials derives passage and at least two material introduction channels, the internal space of described hollow body comprises straight tube district and pyramidal area from top to bottom successively, described material introduction channel is tangentially arranged in the exterior side wall in described straight tube district, enter in described straight tube district to make the oil agent mixture in described segregation section by described material introduction channel, described material introduction channel is 1:3-30 along the ratio of the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of described segregation section, the bottom that passage is positioned at described pyramidal area derived by described material,
Described air outlet tube is arranged on the top of at least one cyclonic separator, the two ends of described air outlet tube are communicated with the air flow inlet of described strainer with the internal space of this cyclonic separator respectively, so that isolated for this cyclonic separator gas-oil mixture is sent fluidized-bed reactor, and in described strainer, the adsorbent fines in described gas-oil mixture is separated;
Described spent agent regeneration unit is used for the spent agent being exported inclined tube output by spent agent to carry out regenerating and reducing, and is sent back in described fluidized-bed reactor by reductive agent.
2. adsorption desulfurize reaction unit according to claim 1, wherein, each material introduction channel is A along the area perpendicular to the cross section of flow direction of material
1, the area of the horizontal section in described straight tube district is A
2, A
2/ A
1=1-10.
3. adsorption desulfurize reaction unit according to claim 1 and 2, wherein, the area of the horizontal section in described straight tube district is A
2, described air outlet tube along being A perpendicular to the area in the cross section of air flow direction
3, A
3/ A
2=0.2-0.8.
4. adsorption desulfurize reaction unit according to claim 1 and 2, wherein, described material introduction channel is 1:5-25 along the ratio of the area perpendicular to the total area in the cross section of flow direction of material and the horizontal section of described segregation section.
5. adsorption desulfurize reaction unit according to claim 1 and 2, wherein, the quantity of described material introduction channel is 2-6.
6. adsorption desulfurize reaction unit according to claim 1 and 2, wherein, described material introduction channel is evenly arrange along the circumferential direction of the exterior side wall in described straight tube district.
7. adsorption desulfurize reaction unit according to claim 1 and 2, wherein, described cyclonic separator comprises the first cyclonic separator and the second cyclonic separator, the air stream outlet of described first cyclonic separator is communicated with the material introduction channel of described second cyclonic separator, and described air outlet tube is positioned at the top of described second cyclonic separator and is communicated with the internal space of described second cyclonic separator;
The solid materials of described first cyclonic separator is derived passage and is extended downward in described conversion zone, sending back in described conversion zone by the isolated absorbent particles of described first cyclonic separator; The solid materials derivation passage of described second cyclonic separator exports inclined tube with described spent agent and is communicated with, with the outside by being delivered to fluidized-bed reactor by the isolated absorbent particles of described second cyclonic separator.
8. adsorption desulfurize reaction unit according to claim 7, wherein, the quantity of described first cyclonic separator is identical with the quantity of the material introduction channel of described second cyclonic separator, and each material introduction channel of described second cyclonic separator is respectively communicated with the air stream outlet of first cyclonic separator.
9. adsorption desulfurize reaction unit according to claim 1, wherein, described strainer has blow device, purges for the regular filtering element to strainer, to be blown off by the fine powder be deposited on described filtering element.
10. a desulfurizing method by adsorption, carries out in the adsorption desulfurize reaction unit of the method in claim 1-9 described in any one, comprising:
Contact containing sulfur-bearing hydrocarbon feed in the conversion zone of described fluidized-bed reactor with the sorbent material with adsorption desulfurize effect with the oil gas raw material of hydrogen, to remove at least part of element sulphur in described sulfur-bearing hydrocarbon feed;
The oil agent mixture that fluidized-bed reactor exports is separated in the filter, to isolate the adsorbent fines in described oil agent mixture, obtains oil gas product;
The spent agent being exported inclined tube output by spent agent is carried out regenerating and reducing in spent agent regeneration unit, and reductive agent is sent back in the conversion zone of described fluidized-bed reactor.
11. methods according to claim 10, wherein, the riser speed of described oil gas raw material in described conversion zone is 0.01-1 meter per second.
12. methods according to claim 11, wherein, the riser speed of described oil gas raw material in described conversion zone is 0.1-0.8 meter per second.
13. methods according to claim 10, wherein, oil gas raw material comprises with the condition of the adsorbent contact with adsorption desulfurize effect: temperature is 300-500 DEG C; And in gauge pressure, the pressure in fluidized-bed reactor is 0.5-5MPa.
14. according to the method in claim 10-13 described in any one, and wherein, in described oil gas raw material, the mol ratio of hydrogen and described sulfur-bearing hydrocarbon feed is 0.1-2:1.
15. according to the method in claim 10-13 described in any one, and wherein, described sulfur-bearing hydrocarbon feed is one or more in straight-run spirit, catalytic gasoline and coker gasoline.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106140036A (en) * | 2016-08-31 | 2016-11-23 | 安徽金禾实业股份有限公司 | Fluid bed air outlet segregation apparatus in a kind of Melamine Production |
| CN106226408A (en) * | 2016-07-22 | 2016-12-14 | 北京赛普泰克技术有限公司 | A kind of cycle rate computational methods of the adsorbent of gasoline absorbing desulfurization device |
| CN109603695A (en) * | 2019-01-10 | 2019-04-12 | 清华大学 | A kind of separation system of paste state bed reactor |
| CN115368937A (en) * | 2022-08-12 | 2022-11-22 | 北京中瀚能源有限公司 | Pretreatment device, combustion device and combustion method for low-calorific-value solid fuel |
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| CN102839011A (en) * | 2011-06-23 | 2012-12-26 | 中国石油化工股份有限公司 | Adsorption desulfurization method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102839011A (en) * | 2011-06-23 | 2012-12-26 | 中国石油化工股份有限公司 | Adsorption desulfurization method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106226408A (en) * | 2016-07-22 | 2016-12-14 | 北京赛普泰克技术有限公司 | A kind of cycle rate computational methods of the adsorbent of gasoline absorbing desulfurization device |
| CN106226408B (en) * | 2016-07-22 | 2019-01-08 | 北京赛普泰克技术有限公司 | A kind of cycle rate calculation method of the adsorbent of gasoline absorbing desulfurization device |
| CN106140036A (en) * | 2016-08-31 | 2016-11-23 | 安徽金禾实业股份有限公司 | Fluid bed air outlet segregation apparatus in a kind of Melamine Production |
| CN109603695A (en) * | 2019-01-10 | 2019-04-12 | 清华大学 | A kind of separation system of paste state bed reactor |
| CN115368937A (en) * | 2022-08-12 | 2022-11-22 | 北京中瀚能源有限公司 | Pretreatment device, combustion device and combustion method for low-calorific-value solid fuel |
| CN115368937B (en) * | 2022-08-12 | 2023-04-18 | 北京中瀚能源有限公司 | Pretreatment device, combustion device and combustion method for low-calorific-value solid fuel |
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