CN107540498A - By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene - Google Patents

By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene Download PDF

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Publication number
CN107540498A
CN107540498A CN201610498266.2A CN201610498266A CN107540498A CN 107540498 A CN107540498 A CN 107540498A CN 201610498266 A CN201610498266 A CN 201610498266A CN 107540498 A CN107540498 A CN 107540498A
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China
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bed
catalyst
methanol
low
dimethyl ether
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钟思青
金永明
李晓红
王莉
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00Technologies relating to oil refining and petrochemical industry
    • Y02P30/20Technologies relating to oil refining and petrochemical industry using bio-feedstock
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00Technologies relating to oil refining and petrochemical industry
    • Y02P30/40Ethylene production

Abstract

The present invention relates to a kind of by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, mainly solve that regenerator temperature is higher in production process, make the gradual hydrothermal deactivation of catalyst, aromatics yield reduces, the problem of influenceing device continuous and steady operation.The present invention contacts generation low-carbon alkene and the effluent rich in aromatic hydrocarbons by using recirculating fluidized bed reaction-regeneration system, methanol and/or dimethyl ether by fluidized-bed reactor with one or more metal supported catalysts;The reclaimable catalyst of inactivation first passes through fast bed (8), control lower temperature mainly completes annealing in hydrogen atmosphere process, then entering back into the second dense-phase fluidized bed regenerator (11) controls higher temperature to complete the technical scheme made charcoal, the problem of preferably resolving catalyst hydrothermal deactivation, continuous and steady operation during methanol or dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, available for by methanol or the industrial production of dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene.

Description

By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene
Technical field
The present invention relates to a kind of by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene.Specifically, relate to It is and a kind of by methanol or the recirculating fluidized bed reaction-regeneration system of dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene.
Background technology
Ethene, propylene and aromatic hydrocarbons (especially triphen, benzene Benzene, toluene Toluene, dimethylbenzene Xylene, i.e. BTX) It is important basic organic synthesis raw material, at present, is mainly produced using petroleum path.In recent years, International Crude Oil is high always Position operation, the production technology to petroleum path bring very big cost pressure.
All the time, coal or producing synthesis gas from natural gas, synthesising gas systeming carbinol and alkene, separation technologies for aromatics have rule Modelling mature experience, but it is the breakpoint and difficult point of this industrial chain by the process of methanol to ethene, propylene and aromatic hydrocarbons, and be somebody's turn to do The solution of key technology can provide a new original to produce basic organic ethene, propylene and aromatic hydrocarbons by non-oil resource Expect route
In various existing methanol, dimethyl ether catalysis transformation technology, the product of methanol/dimethyl ether conversion aromatic hydrocarbons is simultaneously Including ethene, propylene and aromatic hydrocarbons.The technology initially sees Chang of Mobil companies in 1977 et al. (Journal of Catalysis, 1977,47,249) report methanol and its oxygenatedchemicals conversion preparation virtue on ZSM-5 molecular sieve catalyst The method of the hydrocarbons such as hydrocarbon.1985, Mobil companies disclosed first in its United States Patent (USP) applied US1590321 The result of study of methanol, dimethyl ether conversion aromatic hydrocarbons, the research use the phosphorous ZSM-5 molecular sieve for 2.7% (weight) to urge Agent, reaction temperature are 400~450 DEG C, methanol, dimethyl ether air speed 1.3 (Grams Per Hour)/gram catalyst.
The relevant report and patent in the field are more, but the purpose product of most of technologies is aromatic hydrocarbons, ethene, propylene category It is low in accessory substance, yield.Such as the patent in terms of methanol arenes catalytic agent:Chinese patent CN102372535, CN102371176、CN102371177、CN102372550、CN102372536、CN102371178、CN102416342、 CN101550051, United States Patent (USP) US4615995, US2002/0099249A1 etc..Such as in terms of methanol aromatics process Patent:United States Patent (USP) US4686312, Chinese patent ZL101244969, ZL1880288, CN101602646, CN101823929, CN101671226, CN102199069, CN102199446, CN1880288 etc..
In addition, while technology path disclosed in some patents is methanol aromatic hydrocarbons co-producing light olefins, gasoline etc. other Product, such as patent CN102775261, CN102146010, CN102531821, CN102190546, CN102372537.
Wherein, Multi-function methanol processing method disclosed in patent CN102775261 and device utilize methanol production low-carbon alkene Hydrocarbon, gasoline, aromatic hydrocarbons.This method uses two-step method production technology, and first step methanol feedstock produces low under the effect of special-purpose catalyst 1 Carbon olefin, second step by the reaction gas containing low-carbon alkene after heat exchange, chilling, carrying out washing treatment, in the presence of special-purpose catalyst 2 Synthesize aromatic hydrocarbons and/or gasoline.The reactor of two courses of reaction can be fixed bed or fluid bed.This method uses two-step method, technique Flow is complicated.
Patent CN102146010 discloses the work that low-carbon alkene and arene parallel cogeneration gasoline are produced using methanol as raw material Skill.Low-carbon alkene and aromatic hydrocarbons are produced using methanol as raw material and using molecular sieve catalyst through methanol alkylation reaction and aromatization Co-production gasoline.The reactor of methanol alkylation reaction and aromatization is various types of fixed bed reactors, pressure 0.01 ~0.5 MPa, 180~600 DEG C of temperature.Total liquid yield is more than 70 weight %, and triphen yield is more than 90% (weight).This method is also adopted It is complicated with two reactors, technological process.
Patent CN102531821 discloses methanol and the method for the co-feeding production low-carbon alkene of naphtha and/or aromatic hydrocarbons, Using load 2.2~6.0% (weight) La and 1.0~2.8% (weight) P ZSM-5 catalyst, fixed bed reactors can be used Or fluidized-bed reactor.Reaction temperature is 550~670 DEG C, air speed 1.0~5 (Grams Per Hour)/gram catalyst.The triolefin of this method Yield is higher, but BTX yields are low, only 5~17% (weight).
The method that patent CN102372537 and CN102190546 disclose preparing propylene by methanol transformation and aromatic hydrocarbons.This two specially Profit is developed on the basis of preparing propylene by methanol transformation technology, and propylene is main purpose product, and aromatics yield is relatively low.
The above-mentioned existing fluidization that aromatic hydrocarbons is produced using methanol and/or dimethyl ether as raw material all regenerates system using single System carries out catalyst circular response regeneration.For guarantee high activity of catalyst, it is necessary to which the carbon content of regenerated catalyst is as far as possible low, 0.5% (weight) below, therefore unavoidably needs high temperature regeneration, and general regeneration temperature is more than 650 DEG C.Jiao of reclaimable catalyst Hydrogeneous in charcoal, hydrogen and oxygen reaction can produce vapor., can be because dividing under this high temperature, hydro-thermal atmosphere for molecular sieve catalyst Son sieves framework dealumination and loses activity, and this inactivation is permanent and irreversible.For current regenerative system, in order to ensure The reproduction quality of catalyst, residence time of the catalyst in regenerator is longer, causes catalyst hydrothermal deactivation serious, uses the longevity Life reduces, and aromatics yield declines, production cost increase.
The content of the invention
The technical problems to be solved by the invention are that regenerator temperature is higher in the prior art, lose the gradual hydro-thermal of catalyst Living, aromatics yield reduces, the problem of influenceing device continuous and steady operation, there is provided a kind of to produce aromatic hydrocarbons and low by methanol or dimethyl ether The method of carbon olefin.This method is made charcoal using low temperature, incomplete regen-eration annealing in hydrogen atmosphere, higher temperature, oxygen-enriched regeneration completely, is had and protected Hold good catalyst hydrothermal stability simultaneously, obtain the low-carbon regenerative agent of high quality, the advantages of improving aromatics yield.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:One kind is by methanol or dimethyl ether conversion system The method for taking aromatic hydrocarbons and low-carbon alkene, using recirculating fluidized bed reaction-regeneration system, methanol and/or dimethyl ether pass through fluid bed Reactor contacts generation low-carbon alkene and the effluent rich in aromatic hydrocarbons with one or more metal supported catalysts;It is characterized in that Recirculating fluidized bed reaction-regeneration system used includes fluidized-bed reactor (1), and reactor cyclone (4), reactor takes Hot device (5), stripper (6), inclined tube (7) to be generated, fast bed (8), fast bed heat collector (9), outer circulating tube (10), the second close phase Fluid bed regenerator (11), Second reactivator cyclone separator (14), dilute phase conveying pipe (15), thick cyclone separator (16), tightly Connect formula direct coupled structure (17), degassing tank (18) and regenerator sloped tube (19);Decaying catalyst first passes through fast bed (8), and control is relatively low Temperature mainly completes annealing in hydrogen atmosphere process, then enters back into the second dense-phase fluidized bed regenerator (11) and controls higher temperature to complete to burn Charcoal, obtain the regenerated catalyst of high quality.
In above-mentioned technical proposal, it is preferable that metal supported catalyst is silica alumina ratio SiO2/Al2O3At least 10~100 Crystal aluminosilicate.
In above-mentioned technical proposal, it is highly preferred that catalyst is loaded with least one of Zn, Ag, P, Ga, Cu, Mn and Mg member Element or oxide.
In above-mentioned technical proposal, it is preferable that crystal aluminosilicate is ZSM-5 and/or ZSM-11.
In above-mentioned technical proposal, it is preferable that carried metal is preferably Zn and/or Bi;It is furthermore preferred that Zn and Bi weight ratio For (1:9)~(1:4).
In technical scheme, carried metal mainly exists in the form of the oxide in the catalyst, works as catalyst When being expressed as a%Zn/ZSM-5, the mass percentage content for illustrating Zn elements in catalyst is a%, except Zn or its oxide Remaining is ZSM-5 outside, contains other trace elements in catalyst because raw material or other reasonses ultimately result in preparation process The general component for being not counted in catalyst.
In above-mentioned technical proposal, it is preferable that the regenerated catalyst carbon content is less than 0.1%.
In above-mentioned technical proposal, it is preferable that methanol or dimethyl ether conversion reaction use turbulent fluid bed reactor (1), wrap Emulsion zone (2) and dilute-phase zone (3) are included, methanol or dimethyl ether enter emulsion zone (2) and catalyst from fluidized-bed reactor (1) bottom Contact carries out the reaction generation product such as aromatic hydrocarbons and low-carbon alkene, the reactor that the product gas of entrained catalyst passes through dilute-phase zone (3) Fluidized-bed reactor (1) is left after cyclone separator (4) progress gas solid separation and enters subsequent separation system, and the catalyst of recovery returns Return emulsion zone (2).
In above-mentioned technical proposal, it is preferable that fluidized-bed reactor (1) is by setting interior heat collector (5) or external warmer (5) Or set interior heat collector (5) and external warmer (5) to remove heat caused by reaction simultaneously, while control fluidized-bed reactor (1) Reaction temperature;The reclaimable catalyst of fluidized-bed reactor (1) interior carbon deposit is after stripper (6) removes micro hydro carbons, through treating Raw inclined tube (7) enters fast bed (8).
In above-mentioned technical proposal, it is preferable that use fast bed two-stage regeneration, including fast bed (8) in catalyst regeneration, soon Fast bed heat collector (9), outer circulating tube (10) and second dense-phase fluidized bed regenerator (11) emulsion zone (12), dilute-phase zone (13), the Two regenerator cyclone separators (14), dilute phase conveying pipe (15) and thick cyclone separator (16);Fluidized-bed reactor (1) with it is quick Bed (8) tied portion is put, and in fast bed (8) above, insertion second is close at the top of fast bed (8) for the second dense-phase fluidized bed regenerator (11) Phase fluid bed regenerator (11) bottom, both are by fast bed heat collector (9), and outer circulating tube (10) and dilute phase conveying pipe (15) are even It is logical;It is highly preferred that regenerator cyclone separator (14) and (21) are 1-5 levels, generally 2 or 3 grades.
In above-mentioned technical proposal, it is preferable that reclaimable catalyst carries out catalyst regeneration in fast bed (8) and air contact; Fast bed (8) carries out incomplete regen-eration based on annealing in hydrogen atmosphere, using relatively low regeneration temperature and appropriate oxygen content, controls flue gas Middle oxygen content is less than 1%;Semi regeneration catalyst and oxygen content in fast bed (8) less than 1% burn flue gas pass through it is dilute Phase delivery pipe (15), after thick cyclone separator (16) carries out gas solid separation, semi regeneration catalyst enters the second dense-phase fluidized bed again Raw device (11) emulsion zone (12), burns flue gas and is directly entered Second reactivator cyclonic separation through immediately formula direct coupled structure (17) upwards Device (14), avoid burning the vapor in flue gas and high temperature catalyst contact.
In above-mentioned technical proposal, it is preferable that oxygen content excessive two again main wind from second dense-phase fluidized bed regenerator (11) bottom Portion enters emulsion zone (12) and semi regeneration catalyst under the conditions of higher regeneration temperature, oxygen-enriched regeneration completely, obtains high quality Low-carbon regenerative agent;Flue gas of the oxygen content more than 1% is urged by regenerator cyclone separator (14) recovery of dilute-phase zone (13) After agent, leave the second dense-phase fluidized bed regenerator (11) and enter subsequent power recovery system.
In above-mentioned technical proposal, it is preferable that the high-temperature catalytic in the second dense-phase fluidized bed regenerator (11) emulsion zone (12) Agent enters fast bed (8) bottom after reducing temperature by fast bed external warmer (9), by controlling catalyst internal circulating load to adjust The temperature burnt.
In above-mentioned technical proposal, it is preferable that the catalyst of the second dense-phase fluidized bed regenerator (11) emulsion zone (12) passes through Outer circulating tube (10) enters fast bed device (8) to ensure the density of catalyst of fast bed device (8).
In above-mentioned technical proposal, it is preferable that the catalyst regenerated completely in the second dense-phase fluidized bed regenerator (11) passes through After the micro non-hydrocarbon gases of degassing tank (18) Removal of catalyst entrainment, into fluidized-bed reactor (1) emulsion zone (2).
In above-mentioned technical proposal, it is preferable that methanol or 400~550 DEG C of the reaction temperature of dimethyl ether conversion reaction, reaction pressure 0~1.0MPa of power, 200~550 kgs/m of reactor emulsion zone (2) catalyst averag density3, it is empty in fluidized-bed reactor (1) The meter per second of tower linear speed 0.1~1.0.
In above-mentioned technical proposal, it is preferable that 500~600 DEG C, 0~1.2MPa of regeneration pressure of fast bed (8) regeneration temperature, 30~150 kgs/m of fast bed (8) catalyst averag density3, average 1.0~3.0 meters of void tower linear speed in fast bed (8)/ Second.
In above-mentioned technical proposal, it is preferable that second 600~720 DEG C of dense-phase fluidized bed regenerator (11) regeneration temperature, regeneration 0~1.0MPa of pressure, 200~550 kgs/m of catalyst averag density3, average sky in the second dense-phase fluidized bed regenerator (11) The meter per second of tower linear speed 0.2~1.0.
In above-mentioned technical proposal, it is preferable that immediately formula direct coupled structure (17) by thick cyclone separator (16) tedge and Second reactivator cyclone separator (14) inlet tube forms, and the diameter of cyclone separator (14) inlet tube is straight slightly larger than tedge Footpath, and be enclosed on outside tedge, certain gap is left between two pipes and may be inhaled caused by the second dense-phase fluidized bed regenerator (11) Regenerated flue gas.
For by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is proposed that recirculating fluidized bed reaction- Regenerative system includes fluidized-bed reactor (1), reactor cyclone (4), reactor external warmer (5), stripper (6), Inclined tube (7) to be generated, fast bed (8), fast bed external warmer (9), the second dense-phase fluidized bed regenerator (11), Second reactivator rotation Wind separator (14), dilute phase conveying pipe (15), thick cyclone separator (16), immediately formula direct coupled structure (17), degassing tank (18) and Regenerator sloped tube (19)).Using technical scheme, by low regeneration temperature, incomplete regen-eration annealing in hydrogen atmosphere, higher regeneration temperature Degree, oxygen-enriched regeneration completely are made charcoal, and have the catalyst hydrothermal stability for keeping good simultaneously, obtain the low-carbon regeneration of high quality Agent, carbon content is less than 0.1% on regenerated catalyst, maintains higher aromatics yield, the carbon base absorption rate of its aromatic hydrocarbons is up to 60% More than, achieve good technique effect.
Brief description of the drawings
Fig. 1 is recirculating fluidized bed reaction-regeneration system of the present invention (fluidized-bed reactor setting interior heat collector) schematic diagram;
Fig. 2 is recirculating fluidized bed reaction-regeneration system of the present invention (fluidized-bed reactor setting external warmer) schematic diagram;
In Fig. 1, Fig. 2,1 is fluidized-bed reactor;2 be reactor emulsion zone;3 be reactor dilute-phase zone;4 be reactor Cyclone separator;5 be reactor external warmer;6 be stripper;7 be inclined tube to be generated;8 be fast bed;9 be fast bed outside heat removing Device;10 be outer circulating tube;11 be the second dense-phase fluidized bed regenerator;12 second dense-phase fluidized bed regenerator emulsion zones;13 be Two dense-phase fluidized bed regenerator dilute-phase zones;14 be second fluidized bed regenerator cyclone separator;15 be dilute phase conveying pipe;16 be thick Cyclone separator;17 be immediately formula direct coupled structure;18 be degassing tank;19 be regenerator sloped tube;20 be the main wind of fast bed;21 be second The main wind of fluid bed regenerator (two again main wind).
Below by embodiment, the invention will be further elaborated.
Specific embodiment
【Embodiment 1】
The device of 1800000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 470 DEG C, reaction pressure 0.2MPa, emulsion zone catalyst averag density 350 Kg/m3, the average meter per second of void tower linear speed 0.7.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 550 DEG C, Fast bed pressure is 0.21MPa, quick 80 kgs/m of bed catalyst averag density3, average 1.3 meters of the void tower linear speed of fast bed/ Second;Two again temperature be 660 DEG C, two again pressure be 0.2MPa, two 450 kgs/m of emulsion zone catalyst averag density again3, two again The average meter per second of void tower linear speed 0.8;Two main wind oxygen content 21% (volume) the again, (body of fast bed exhanst gas outlet oxygen content 0.5% Product), two exhanst gas outlet oxygen content 4.1% (volumes) again, carbon content 0.08% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 64.26%, ethene carbon base absorption rate 6.30%, propylene carbon base absorption rate 4.89%.
【Embodiment 2】
The device of 1800000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 450 DEG C, reaction pressure 0.3MPa, emulsion zone catalyst averag density 300 Kg/m3, the average meter per second of void tower linear speed 0.6.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 540 DEG C, Fast bed pressure is 0.31MPa, quick 50 kgs/m of bed catalyst averag density3, average 1.6 meters of the void tower linear speed of fast bed/ Second;Two again temperature be 690 DEG C, two again pressure be 0.3MPa, two 400 kgs/m of emulsion zone catalyst averag density again3, two again The average meter per second of void tower linear speed 0.6;Two main wind oxygen content 21% (volume) the again, (body of fast bed exhanst gas outlet oxygen content 0.8% Product), two exhanst gas outlet oxygen content 5.8% (volumes) again, carbon content 0.05% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 60.92%, ethene carbon base absorption rate 7.85%, propylene carbon base absorption rate 6.46%.
【Embodiment 3】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 2 reaction-again Raw system, fluidized-bed reactor sets external warmer, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 480 DEG C, reaction pressure 0.3MPa, emulsion zone catalyst averag density 380 Kg/m3, the average meter per second of void tower linear speed 0.8.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 560 DEG C, Fast bed pressure is 0.31MPa, quick bed catalyst averag density double centner/rice3, average 1.1 meters of the void tower linear speed of fast bed/ Second;Two again temperature be 680 DEG C, two again pressure be 0.3MPa, two 350 kgs/m of emulsion zone catalyst averag density again3, two again The average meter per second of void tower linear speed 0.8;Two main wind oxygen content 21% (volume) the again, (body of fast bed exhanst gas outlet oxygen content 0.6% Product), two exhanst gas outlet oxygen content 3.2% (volumes) again, carbon content 0.04% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 62.51%, ethene carbon base absorption rate 8.07%, propylene carbon base absorption rate 6.38%.
【Embodiment 4】
The device of 600000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 2 reaction-again Raw system, fluidized-bed reactor sets external warmer, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 490 DEG C, reaction pressure 0.2MPa, emulsion zone catalyst averag density 430 Kg/m3, the average meter per second of void tower linear speed 0.9.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 550 DEG C, Fast bed pressure is 0.21MPa, quick 75 kgs/m of bed catalyst averag density3, average 1.2 meters of the void tower linear speed of fast bed/ Second;Two again temperature be 680 DEG C, two again pressure be 0.2MPa, two 380 kgs/m of emulsion zone catalyst averag density again3, two again The average meter per second of void tower linear speed 0.7;Two main wind oxygen content 21% (volume) the again, (body of fast bed exhanst gas outlet oxygen content 0.9% Product), two exhanst gas outlet oxygen content 5.1% (volumes) again, carbon content 0.05% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 62.4%, ethene carbon base absorption rate 8.32%, propylene carbon base absorption rate 6.01%.
【Embodiment 5】
The device of 1800000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 2 reaction-again Raw system, fluidized-bed reactor sets external warmer, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 470 DEG C, reaction pressure 0.5MPa, emulsion zone catalyst averag density 300 Kg/m3, the average meter per second of void tower linear speed 0.5.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 580 DEG C, Fast bed pressure is 0.51MPa, quick 60 kgs/m of bed catalyst averag density3, average 1.5 meters of the void tower linear speed of fast bed/ Second;Two again temperature be 680 DEG C, two again pressure be 0.5MPa, two 350 kgs/m of emulsion zone catalyst averag density again3, two again The average meter per second of void tower linear speed 0.5;Two main wind oxygen content 21% (volume) the again, (body of fast bed exhanst gas outlet oxygen content 0.8% Product), two exhanst gas outlet oxygen content 4.4% (volumes) again, carbon content 0.06% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 63.3%, ethene carbon base absorption rate 6.17%, propylene carbon base absorption rate 4.94%.
【Embodiment 6】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 480 DEG C, reaction pressure 0.15MPa, emulsion zone catalyst averag density 480 kgs/m3, the average meter per second of void tower linear speed 0.5.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 540 DEG C, fast bed pressure is 0.16MPa, quick 86 kgs/m of bed catalyst averag density3, the average void tower linear speed 1.3 of fast bed Meter per second;Two again temperature be 670 DEG C, two again pressure be 0.15MPa, two 400 kgs/m of emulsion zone catalyst averag density again3, Two again be averaged the meter per second of void tower linear speed 0.6;Two main wind oxygen content 21% (volume) again, fast bed exhanst gas outlet oxygen content 0.4% (volume), two exhanst gas outlet oxygen content 2% (volumes) again, carbon content 0.07% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 60.3%, ethene carbon base absorption rate 9.17%, propylene carbon base absorption rate 7.94%.
【Embodiment 7】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 500 DEG C, reaction pressure 0.05MPa, emulsion zone catalyst averag density 550 kgs/m3, the average meter per second of void tower linear speed 0.8.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 550 DEG C, fast bed pressure is 0.06MPa, quick 86 kgs/m of bed catalyst averag density3, the average void tower linear speed 1.3 of fast bed Meter per second;Two again temperature be 680 DEG C, two again pressure be 0.05MPa, two 385 kgs/m of emulsion zone catalyst averag density again3, Two again be averaged the meter per second of void tower linear speed 0.7;Two main wind oxygen content 21% (volume) again, fast bed exhanst gas outlet oxygen content 0.8% (volume), two exhanst gas outlet oxygen content 4% (volumes) again, carbon content 0.08% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 53.83%, ethene carbon base absorption rate 14.02%, propylene carbon base absorption rate 10.17%.
【Embodiment 8】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Cu/SiO2.Fluidized-bed reaction The reaction process condition of device is:Reaction temperature is 480 DEG C, reaction pressure 0.15MPa, emulsion zone catalyst averag density 480 Kg/m3, the average meter per second of void tower linear speed 0.5.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 540 DEG C, Fast bed pressure is 0.16MPa, quick 86 kgs/m of bed catalyst averag density3, average 1.3 meters of the void tower linear speed of fast bed/ Second;Two again temperature be 670 DEG C, two again pressure be 0.15MPa, two 400 kgs/m of emulsion zone catalyst averag density again3, two again The average meter per second of void tower linear speed 0.6;Two main wind oxygen content 21% (volume) the again, (body of fast bed exhanst gas outlet oxygen content 0.4% Product), two exhanst gas outlet oxygen content 2% (volumes) again, carbon content 0.07% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 58.9%, ethene carbon base absorption rate 10.2%, propylene carbon base absorption rate 8.0%.
【Embodiment 9】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Ti/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 480 DEG C, reaction pressure 0.15MPa, emulsion zone catalyst averag density 480 kgs/m3, the average meter per second of void tower linear speed 0.5.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 540 DEG C, fast bed pressure is 0.16MPa, quick 86 kgs/m of bed catalyst averag density3, the average void tower linear speed 1.3 of fast bed Meter per second;Two again temperature be 670 DEG C, two again pressure be 0.15MPa, two 400 kgs/m of emulsion zone catalyst averag density again3, Two again be averaged the meter per second of void tower linear speed 0.6;Two main wind oxygen content 21% (volume) again, fast bed exhanst gas outlet oxygen content 0.4% (volume), two exhanst gas outlet oxygen content 2% (volumes) again, carbon content 0.07% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 61.3%, ethene carbon base absorption rate 9.05%, propylene carbon base absorption rate 7.5%.
【Embodiment 10】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Bi/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 500 DEG C, reaction pressure 0.05MPa, emulsion zone catalyst averag density 550 kgs/m3, the average meter per second of void tower linear speed 0.8.The technological condition of regeneration of fluid bed regenerator is:Quick bed tempertaure is 550 DEG C, fast bed pressure is 0.06MPa, quick 86 kgs/m of bed catalyst averag density3, the average void tower linear speed 1.3 of fast bed Meter per second;Two again temperature be 680 DEG C, two again pressure be 0.05MPa, two 385 kgs/m of emulsion zone catalyst averag density again3, Two again be averaged the meter per second of void tower linear speed 0.7;Two main wind oxygen content 21% (volume) again, fast bed exhanst gas outlet oxygen content 0.8% (volume), two exhanst gas outlet oxygen content 4% (volumes) again, carbon content 0.08% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 60.2%, ethene carbon base absorption rate 12.2%, propylene carbon base absorption rate 8.3%.
【Embodiment 11】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 0.4%Zn/3.6%Bi/ZSM-5.Fluidisation Bed reactor reaction process condition be:Reaction temperature is 500 DEG C, reaction pressure 0.05MPa, and emulsion zone catalyst is average close 550 kgs/m of degree3, the average meter per second of void tower linear speed 0.8.The technological condition of regeneration of fluid bed regenerator is:Quickly bed tempertaure is 550 DEG C, fast bed pressure is 0.06MPa, quick 86 kgs/m of bed catalyst averag density3, the average void tower linear speed of fast bed 1.3 meter per second;Two again temperature be 680 DEG C, two again pressure be 0.05MPa, two again 385 kilograms of emulsion zone catalyst averag density/ Rice3, two again be averaged the meter per second of void tower linear speed 0.7;Two main wind oxygen content 21% (volume) again, fast bed exhanst gas outlet oxygen content 0.8% (volume), two exhanst gas outlet oxygen content 4% (volumes) again, carbon content 0.08% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 64.2%, ethene carbon base absorption rate 8.4%, propylene carbon base absorption rate 7.8%.
【Embodiment 12】
The device of 1200000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 0.8%Zn/3.2%Bi/ZSM-5.Fluidisation Bed reactor reaction process condition be:Reaction temperature is 500 DEG C, reaction pressure 0.05MPa, and emulsion zone catalyst is average close 550 kgs/m of degree3, the average meter per second of void tower linear speed 0.8.The technological condition of regeneration of fluid bed regenerator is:Quickly bed tempertaure is 550 DEG C, fast bed pressure is 0.06MPa, quick 86 kgs/m of bed catalyst averag density3, the average void tower linear speed of fast bed 1.3 meter per second;Two again temperature be 680 DEG C, two again pressure be 0.05MPa, two again 385 kilograms of emulsion zone catalyst averag density/ Rice3, two again be averaged the meter per second of void tower linear speed 0.7;Two main wind oxygen content 21% (volume) again, fast bed exhanst gas outlet oxygen content 0.8% (volume), two exhanst gas outlet oxygen content 4% (volumes) again, carbon content 0.08% on regenerated catalyst.
Under conditions above and structural parameters, methanol aromatic hydrocarbons and alkene are carried out by method of the present invention, can obtain More satisfactory result, aromatic hydrocarbons carbon base absorption rate 64.0%, ethene carbon base absorption rate 10.1%, propylene carbon base absorption rate 9.0%.
【Comparative example 1】
The device of 1800000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene using recirculating fluidized bed as shown in Figure 1 reaction-again Raw system, fluidized-bed reactor sets interior heat collector, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.Fluid bed is anti- The reaction process condition for answering device is:Reaction temperature is 470 DEG C, reaction pressure 0.5MPa, emulsion zone catalyst averag density 330 Kg/m3, the average meter per second of void tower linear speed 0.5.The technological condition of regeneration of fluid bed regenerator is:Again and again temperature be 680 DEG C, one Pressure is 0.5MPa again, again and again 280 kgs/m of emulsion zone catalyst averag density3, the average meter per second of void tower linear speed 0.7 again and again; Two again temperature be 680 DEG C, two again pressure be 0.51MPa, two 310 kgs/m of emulsion zone catalyst averag density again3, put down again and again The equal meter per second of void tower linear speed 0.8, two main wind oxygen content 21% (volume) again, exhanst gas outlet oxygen content 1.8% (volume) again and again, two Exhanst gas outlet oxygen content 4.1% (volume) again, carbon content 0.08% on regenerated catalyst.
Under conditions above and structural parameters, available operation result, aromatic hydrocarbons carbon base absorption rate 50.95%, the carbon-based receipts of ethene Rate 13.21%, propylene carbon base absorption rate 9.52%.
【Comparative example 2】
The device of 1800000 tons/year of methanol production aromatic hydrocarbons and low-carbon alkene uses regular circulation fluidized-bed reaction-regeneration system System, regenerator is one section of regeneration, using metal supported catalyst 1%Zn/3%Cu/ZSM-5.The reaction work of fluidized-bed reactor Skill condition is:Reaction temperature is 470 DEG C, reaction pressure 0.5MPa, 300 kgs/m of emulsion zone catalyst averag density3, put down The equal meter per second of void tower linear speed 0.5.The technological condition of regeneration of fluid bed regenerator is:Temperature is 550 DEG C, regeneration pressure 0.5MPa, 380 kgs/m of regenerator emulsion zone catalyst averag density3, the average meter per second of void tower linear speed 0.6 of regenerator;Main wind oxygen content 21% (volume), exhanst gas outlet oxygen content 0.4% (volume), carbon content 1.8% on regenerated catalyst.
Under conditions above and structural parameters, available operation result, aromatic hydrocarbons carbon base absorption rate 47.71%, the carbon-based receipts of ethene Rate 16.63%, propylene carbon base absorption rate 11.82%.

Claims (10)

1. it is a kind of by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, react-regenerate using recirculating fluidized bed System, methanol and/or dimethyl ether contact generation low-carbon alkene by fluidized-bed reactor with one or more metal supported catalysts Hydrocarbon and the effluent rich in aromatic hydrocarbons;It is characterized in that recirculating fluidized bed reaction-regeneration system used includes fluidized-bed reactor (1), reactor cyclone (4), reactor heat collector (5), stripper (6), inclined tube (7) to be generated, fast bed (8), quickly Bed heat collector (9), outer circulating tube (10), the second dense-phase fluidized bed regenerator (11), Second reactivator cyclone separator (14) are dilute Phase delivery pipe (15), thick cyclone separator (16), immediately formula direct coupled structure (17), degassing tank (18) and regenerator sloped tube (19);Lose Catalyst living first passes through fast bed (8), and control lower temperature mainly completes annealing in hydrogen atmosphere process, then enters back into the second dense-phase fluidized bed Regenerator (11) controls higher temperature to complete to make charcoal, and obtains the regenerated catalyst of high quality.
2. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that Methanol or dimethyl ether conversion reaction use turbulent fluid bed reactor (1), including emulsion zone (2) and dilute-phase zone (3), methanol or two Methyl ether enters emulsion zone (2) from fluidized-bed reactor (1) bottom and catalyst contact carries out reaction generation aromatic hydrocarbons and low-carbon alkene Deng product, the product gas of entrained catalyst pass through dilute-phase zone (3) reactor cyclone (4) carry out gas solid separation after leave Fluidized-bed reactor (1) enters subsequent separation system, and the catalyst of recovery returns to emulsion zone (2).
3. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that Fluidized-bed reactor (1) is by setting interior heat collector (5) or external warmer (5) or setting interior heat collector (5) and outside heat removing simultaneously Device (5) removes heat caused by reaction, while controls the reaction temperature of fluidized-bed reactor (1).Fluidized-bed reactor (1) inner product The reclaimable catalyst of charcoal enters fast bed (8) after stripper (6) removes micro hydro carbons through inclined tube to be generated (7).
4. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that Catalyst regeneration uses fast bed two-stage regeneration, including fast bed (8), fast bed heat collector (9), outer circulating tube (10) and second Dense-phase fluidized bed regenerator (11) emulsion zone (12), dilute-phase zone (13), Second reactivator cyclone separator (14), dilute phase conveying pipe And thick cyclone separator (16) (15);Fluidized-bed reactor (1) is put with fast bed (8) tied portion, the regeneration of the second dense-phase fluidized bed In fast bed (8) above, second dense-phase fluidized bed regenerator (11) bottom of insertion at the top of fast bed (8), both pass through device (11) Fast bed heat collector (9), outer circulating tube (10) connect with dilute phase conveying pipe (15).
5. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that Reclaimable catalyst carries out catalyst regeneration in fast bed (8) and air contact;Fast bed (8) is based on annealing in hydrogen atmosphere, using relatively low Regeneration temperature and appropriate oxygen content carry out incomplete regen-eration, control oxygen content in flue gas to be less than 1%;In fast bed (8) Semi regeneration catalyst and oxygen content pass through dilute phase conveying pipe (15), thick cyclone separator (16) less than 1% flue gas that burns Carry out gas solid separation after, semi regeneration catalyst enters second dense-phase fluidized bed regenerator (11) emulsion zone (12), burn flue gas to On through immediately formula direct coupled structure (17) be directly entered Second reactivator cyclone separator (14), avoid burning the vapor in flue gas Contacted with high temperature catalyst.
6. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that Main wind enters emulsion zone (12) and semi regeneration catalyst to oxygen content excessive two from second dense-phase fluidized bed regenerator (11) bottom again Under the conditions of higher regeneration temperature, oxygen-enriched regeneration completely, the low-carbon regenerative agent of high quality is obtained;Oxygen content is more than 1% After flue gas reclaims catalyst by the regenerator cyclone separator (14) of dilute-phase zone (13), the second dense-phase fluidized bed regenerator is left (11) subsequent power recovery system is entered.
7. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that High temperature catalyst in second dense-phase fluidized bed regenerator (11) emulsion zone (12) reduces temperature by fast bed external warmer (9) Enter fast bed (8) bottom afterwards, the temperature burnt is adjusted by controlling catalyst internal circulating load.
8. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that The catalyst of second dense-phase fluidized bed regenerator (11) emulsion zone (12) enters fast bed device (8) to protect by outer circulating tube (10) Demonstrate,prove the density of catalyst of fast bed device (8).
9. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that The catalyst regenerated completely in second dense-phase fluidized bed regenerator (11) is micro by the entrainment of degassing tank (18) Removal of catalyst After non-hydrocarbon gases, into fluidized-bed reactor (1) emulsion zone (2).
10. according to claim 1 by methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene, it is characterised in that Immediately formula direct coupled structure (17) by thick cyclone separator (16) tedge and Second reactivator cyclone separator (14) inlet tube Composition, the diameter of cyclone separator (14) inlet tube are enclosed on outside tedge slightly larger than rising pipe diameter, and one is left between two pipes Fixed gap may be inhaled regenerated flue gas caused by the second dense-phase fluidized bed regenerator (11).
CN201610498266.2A 2016-06-29 2016-06-29 By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene Pending CN107540498A (en)

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Application publication date: 20180105