CN108654527B - Two-stage circulating fluidized bed reaction-regeneration system and method for preparing aromatic hydrocarbon from synthesis gas - Google Patents

Two-stage circulating fluidized bed reaction-regeneration system and method for preparing aromatic hydrocarbon from synthesis gas Download PDF

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CN108654527B
CN108654527B CN201810332927.3A CN201810332927A CN108654527B CN 108654527 B CN108654527 B CN 108654527B CN 201810332927 A CN201810332927 A CN 201810332927A CN 108654527 B CN108654527 B CN 108654527B
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catalyst
aromatization
reactor
gas
filling area
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CN108654527A (en
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骞伟中
宋文龙
侯一林
陈兆辉
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Tsinghua University
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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
    • B01J8/26—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 with two or more fluidised beds, e.g. reactor and regeneration installations
    • 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
    • B01J8/1809—Controlling processes
    • 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
    • B01J8/1845—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with particles moving upwards while fluidised
    • 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
    • C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
    • C10G3/54—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids characterised by the catalytic bed
    • C10G3/55—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids characterised by the catalytic bed with moving solid particles, e.g. moving beds
    • C10G3/57—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids characterised by the catalytic bed with moving solid particles, e.g. moving beds according to the fluidised bed technique
    • 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
    • C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
    • C10G3/62—Catalyst regeneration
    • 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
    • C10G2300/70—Catalyst aspects
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock

Abstract

A two-section circulating fluidized bed reaction-regeneration system and method for preparing aromatic hydrocarbon by synthesis gas comprises an aromatization reactor and a catalyst regeneration reactor which are connected with each other through a pipeline, wherein the aromatization reactor comprises a first catalyst filling area and a second catalyst filling area; the catalyst regeneration reactor comprises a fourth catalyst filling area and a third catalyst filling area, a hydrocarbon synthesis catalyst and an aromatization catalyst are filled in the aromatization reactor, the hydrocarbon synthesis catalyst mainly stays in a lower area and the aromatization catalyst mainly stays in an upper area under the action of air flow, and a regeneration method that the aromatization catalyst enters a low-temperature low-oxygen area of the catalyst regeneration reactor firstly and then enters a high-temperature high-oxygen area of the catalyst regeneration reactor after being inactivated is disclosed.

Description

Two-stage circulating fluidized bed reaction-regeneration system and method for preparing aromatic hydrocarbon from synthesis gas
Technical Field
The invention relates to the technical field of chemical process and equipment, in particular to a two-stage circulating fluidized bed reaction-regeneration system and a method for preparing aromatic hydrocarbon from synthesis gas.
Background
The technology of aromatizing synthetic gas is a new aromatic hydrocarbon production process, wherein one route is that hydrocarbon intermediates are firstly formed in the synthetic gas, and then the aromatic hydrocarbon is prepared by the hydrocarbon. The obvious advantage of combining the two reactions in one reactor is that the separation of the hydrocarbons from the complex hydrocarbon components and the preparation of high purity products are not necessary, so that the separation units of the two processes which were originally carried out separately can be effectively combined. The technical challenge is that the original hydrocarbon synthesis catalyst acts at the temperature of 300-380 ℃, and the hydrocarbon preparation aromatic hydrocarbon catalyst acts at the temperature of 350-500 ℃. At present, the preparation of multifunctional composite catalyst is reported, and the preparation of arene without generating hydrocarbon products is expected. However, at present, the catalyst is limited by chemical equilibrium, the conversion rate of the synthesis gas is not high, and CO is generated2The selectivity of (A) is relatively high. Meanwhile, the catalyst of the process needs to be regenerated at high temperature, and no technical report of the process exists at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a two-stage circulating fluidized bed reaction-regeneration system and a method for preparing aromatic hydrocarbon by synthesis gas, which realize a fluidized bed reactor structure of 'firstly generating hydrocarbon and regenerating aromatic hydrocarbon' by introducing a transverse porous baffle in the axial direction of a reactor, and establish a temperature difference and a concentration difference at the upper section and the lower section of a catalyst regeneration two-stage fluidized bed reactor to recover and protect the activity of a catalyst.
In order to achieve the purpose, the invention adopts the technical scheme that:
a two-section circulating fluidized bed reaction-regeneration system for preparing aromatic hydrocarbon by synthesis gas comprises an aromatization reactor 1 and a catalyst regeneration reactor 13 which are connected with each other through a pipeline, wherein the aromatization reactor 1 is divided into two end fluidized beds, a first catalyst filling area 1a is arranged below the aromatization reactor 1, a second catalyst filling area 1b is arranged above the aromatization reactor 1, a first gas inlet 2 is arranged at the bottom of the first catalyst filling area 1a, a first transverse porous distribution plate 3 is arranged between the first catalyst filling area 1a and the second catalyst filling area 1b, a first gas inlet 4 and a first catalyst outlet 5 are arranged at the lower part of the second catalyst filling area 1b, a first gas outlet 7 is arranged at the top of the second catalyst filling area 1b, and a first catalyst inlet 6 is arranged at the upper part of the second catalyst filling area 1 b;
the catalyst regeneration reactor 13 is divided into two end fluidized beds, and comprises an upper fourth catalyst filling area 13b and a lower third catalyst filling area 13a, the bottom of the third catalyst filling area 13a is provided with a second gas inlet 8, and a second catalyst outlet 12 is arranged below the third catalyst filling area 13 a;
a second transverse porous distribution plate 9 is arranged between the fourth catalyst loading area 13b and a third catalyst loading area 13a below the fourth catalyst loading area 13b, and a second catalyst inlet 11 and a second gas outlet 10 at the top are arranged at the upper part of the fourth catalyst loading area 13 b;
the output end of the first catalyst outlet 5 is connected with the input end of the second catalyst inlet 11, and the output end of the second catalyst outlet 12 is connected with the input end of the first catalyst inlet 6.
The first catalyst loading zone 1a is a hydrocarbon synthesis catalyst zone, the second catalyst loading zone 1b is a hydrocarbon aromatization catalyst zone, the first catalyst loading zone 1a is a low-temperature synthesis gas low-carbon hydrocarbon zone, the second catalyst loading zone 1b is a high-temperature hydrocarbon aromatization zone, the fourth catalyst loading zone 13b is a low-temperature low-oxygen zone, and the third catalyst loading zone 13a is a high-temperature high-oxygen zone.
The invention also provides a method for preparing aromatic hydrocarbon from the synthesis gas by using the device, which comprises the following steps:
(1) pre-installing a synthetic hydrocarbon catalyst and an aromatization catalyst in a first catalyst filling area 1a of an aromatization reactor 1, preheating synthesis gas, introducing the preheated synthesis gas from a first gas inlet 2 at the lower section of the aromatization reactor 1, blowing the aromatization catalyst to a second catalyst filling area 1b through a first transverse porous distribution plate 3, wherein the synthesis gas is mainly contacted with the catalyst for synthesizing hydrocarbons in the first catalyst filling area 1a to generate various hydrocarbons, passes through the first transverse porous distribution plate 3 and enters the second catalyst filling area 1 b;
(2) hydrocarbon gas contacts with the aromatization catalyst in the second catalyst filling area 1b to generate aromatic hydrocarbon and other organic products, the aromatic hydrocarbon and other organic products are discharged from the aromatization reactor 1 from a first gas outlet 7 of the reactor, and the C is subjected to heat exchange, separation and other steps3-C8The non-aromatic hydrocarbon is recycled and enters the second catalyst filling area 1b from the first gas inlet 4 for recycling;
(3) a portion of the catalyst is pre-charged in a third catalyst charge zone 13a of the catalyst regeneration reactor 13 and an oxygen-containing gas (e.g., air, oxygen, or oxygen-containing CO) is introduced through the bottom second gas inlet 82One of nitrogen or argon, the volume content of oxygen is 2% -100%), and the generated gas in the third catalyst filling area 13a enters the fourth catalyst filling area 13b through the second transverse porous distribution plate 9;
(4) after carbon deposition of the catalyst in the second catalyst filling region 1b in the aromatization reactor 1, moving out from the first catalyst outlet 5 of the aromatization reactor 1, conveying the carbon deposition through a pipeline, entering a fourth catalyst filling region 13b of a catalyst regeneration reactor 13 through a second catalyst inlet 11, allowing the coke-containing catalyst entering from the second catalyst inlet 11 to enter a third catalyst filling region 13a through a second transverse porous distribution plate 9 after part of coke is burned off in the fourth catalyst filling region 13b, and allowing the gas to exit the catalyst regeneration reactor 13 through a second gas outlet 10;
(5) in the third catalyst loading zone 13a, most of the coke on the catalyst is burned off and transported through the second catalyst outlet 12, through the pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6;
(6) repeating the above steps to continuously carry out the process.
The temperature of the first catalyst loading area 1a is 250-380 ℃, the temperature of the second catalyst loading area 1b is 450-550 ℃, and the pressure is 0.1-3.5 MPa.
The temperature of the third catalyst loading area 13a is 550-650 ℃, the temperature of the fourth catalyst loading area 13b is 480-600 ℃, and the pressure is 0.1-3.5 MPa.
The main active components of the low-carbon hydrocarbon synthesis catalyst in the first catalyst loading zone 1a in the aromatization reactor 1 are Fe, Cr, Co, Mo, Ni, Mn and one or more of the carbonization state and the nitridation state thereof, the carrier is one or more of aluminum oxide, zirconium oxide and silicon oxide, the active components account for 1-50% of the total mass of the hydrocarbon synthesis catalyst, and the rest is the carrier; the average particle size of the catalyst was 200-350. mu.m.
The hydrocarbon aromatization catalyst in the second catalyst filling zone 1b is a metal or metal oxide-molecular sieve + carrier three-function catalyst, and the metal or metal oxide is Cu, Zn, Cr, Fe, Co, Ni, ZnO, CeO2, La2O3, Ga2O3、Fe2O3And MoO3One or more of ZSM-5, ZSM-12, one or more of Y molecular type and beta molecular sieve, and one or more of alumina, kaolin and silicon oxide as carrier; wherein: the mass fraction of the molecular sieve in the total mass of the hydrocarbon aromatization catalyst is 20-40%, the mass fraction of the carrier in the total mass of the hydrocarbon aromatization catalyst is 45-65%, and the metal or metal oxygenThe mass fraction of the compound in the total mass of the hydrocarbon aromatization catalyst is 1-15%, and the average particle size of the catalyst is 40-120 micrometers.
The invention has the beneficial effects that:
the synthetic hydrocarbons and the generated aromatic hydrocarbons react in a subarea manner, so that the control of different temperatures can be realized, different types of catalysts can be used, and the design difficulty of the catalysts is reduced. By arranging two reaction areas, the back mixing of intermediate products can be reduced, and CO can be generated2The yield is reduced by 80%. Compared with other processes, the cost is reduced by 30 percent.
The catalyst regeneration reactor adopts a two-stage fluidized bed with variable temperature, and has controllable heat compared with the single-stage fluidized bed, the service life of the catalyst is prolonged by 50-65%, and the pulverization of the catalyst is reduced by 5%. After the catalyst is regenerated, the catalyst is introduced into an aromatization reaction region, the temperature difference is small, and the catalyst pulverization is reduced by 10-20% compared with the condition that the catalyst is directly introduced into a synthetic hydrocarbon region.
C is to be3-C8The non-aromatic hydrocarbon is circularly converted, and the aromatic hydrocarbon yield can be improved by 10-20%.
Drawings
FIG. 1 is a two-stage circulating fluidized bed reaction system for producing aromatic hydrocarbons from synthesis gas.
Detailed Description
The present invention will be described in further detail with reference to examples.
As shown in FIG. 1, the two-stage circulating fluidized bed reaction-regeneration system for preparing aromatic hydrocarbon from synthesis gas of the present invention comprises an aromatization reactor 1 and a catalyst regeneration reactor 13 which are connected with each other through a pipeline, the aromatization reactor 1 is divided into two end fluidized beds, the lower part is a first catalyst filling area 1a, the upper part is a second catalyst filling area 1b, a first gas inlet 2 is arranged at the bottom of the first catalyst loading area 1a, a first transverse porous distribution plate 3 is arranged between the first catalyst loading area 1a and the second catalyst loading area 1b, the lower part of the second catalyst loading area 1b is provided with a first gas inlet 4 and a first catalyst outlet 5, the top of the second catalyst filling area 1b is provided with a first gas outlet 7, and the upper part is provided with a first catalyst inlet 6;
the catalyst regeneration reactor 13 is divided into two end fluidized beds, and comprises an upper fourth catalyst filling area 13b and a lower third catalyst filling area 13a, the bottom of the third catalyst filling area 13a is provided with a second gas inlet 8, and a second catalyst outlet 12 is arranged below the third catalyst filling area 13 a;
a second transverse porous distribution plate 9 is arranged between the fourth catalyst loading area 13b and the third catalyst loading area 13a below the fourth catalyst loading area 13b, and a second catalyst inlet 11 and a second gas outlet 10 at the top are arranged at the upper part of the fourth catalyst loading area 13 b.
The first catalyst loading zone 1a is a hydrocarbon synthesis catalyst zone, the second catalyst loading zone 1b is a hydrocarbon aromatization catalyst zone, the first catalyst loading zone 1a is a low-temperature synthesis gas low-carbon hydrocarbon zone, the second catalyst loading zone 1b is a high-temperature hydrocarbon aromatization zone, the fourth catalyst loading zone 13b is a low-temperature low-oxygen zone, and the third catalyst loading zone 13a is a high-temperature high-oxygen zone.
Example 1
Mixing hydrocarbon synthesis catalyst (iron nitride/alumina, iron nitride mass fraction is 50%, the rest is alumina, catalyst average grain size is 350 micrometer) and aromatization catalyst (Ga)2O3Molecular sieve/alumina type, wherein alumina, molecular sieve Y, Ga2O360%, 30%, 10% by mass, respectively, the average particle diameter of the catalyst being 120 μm) is packed in the first catalyst packing section 1a region of the aromatization reactor 1. The lower region of the aromatization reactor 1 was preheated to 250 ℃, synthesis gas (CO and hydrogen) was fed, the pressure was controlled to 3MPa, the aromatization catalyst was blown from the first catalyst loading zone 1a into the second catalyst loading zone 1b, and the temperature of the second catalyst loading zone 1b was controlled to 550 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. After the gas out of the aromatization reactor 1 is subjected to heat exchange and cooling,sequentially separating water, aromatic hydrocarbon, light hydrocarbon and synthesis gas, wherein C is contained in the light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the circulating first gas inlet 4 to continue to react.
The partially aromatized catalyst is pre-filled in the third catalyst filling zone 13a in the catalyst regeneration reactor 13, air is introduced from the second gas inlet 8 at the bottom, and the generated gas in the third catalyst filling zone 13a passes through the second transverse porous distribution plate 9 and enters the fourth catalyst filling zone 13 b. The temperatures of the third catalyst-packed section 13a and the fourth catalyst-packed section 13b were controlled at 620 ℃ and 530 ℃, respectively.
When the carbon deposition of the catalyst in the second catalyst loading region 1b in the aromatization reactor is inactivated, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline and enters the fourth catalyst loading region 13b of the catalyst regeneration reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regenerator 13 through a second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.
Example 2
Hydrocarbon synthesis catalyst (Fe/Cr/alumina catalyst, alumina, Fe, Cr mass fractions of 5%, 20%, 75%, respectively, average particle size of catalyst is 200 μm) and aromatization catalyst (ZnO/Ga)2O3ZSM-5/alumina, wherein the alumina, ZSM-5 molecular sieve, Ga2O3ZnO mass fractions of 50%, 35%, 5%, 10%, respectively, and an average particle diameter of the catalyst of 40 μm) is packed in the first catalyst packing section 1a region in the reactor. The lower region of the reactor was preheated to 380 ℃ and synthesis gas (CO and hydrogen) was fed in, the pressure being controlled at 2 MPa. Blowing the aromatization catalyst from the first catalyst loading zone 1a to the second catalyst loading zone1b, the temperature of the second catalyst-packed section 1b is controlled to 450 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. The gas out of the aromatization reactor 1 is subjected to heat exchange and cooling, and then water, aromatic hydrocarbon, light hydrocarbon and synthesis gas are sequentially separated, wherein C is contained in the light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the first gas inlet 4 for continuous reaction.
Partially aromatized catalyst is pre-charged in a third catalyst charging zone 13a of the catalyst regeneration two-stage fluidized bed reactor 13, and CO containing 15% oxygen is introduced from a bottom second gas inlet 82The generated gas in the third catalyst loading zone 13a passes through the second horizontal porous distribution plate 9 and enters the fourth catalyst loading zone 13 b. The temperatures of the third catalyst-packed section 13a and the fourth catalyst-packed section 13b were controlled to 580 deg.C and 490 deg.C, respectively.
When the catalyst in the second catalyst loading zone 1b in the aromatization reactor is deactivated by carbon deposition, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline and enters the fourth catalyst loading zone 13b of the reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regenerator 13 through a second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.
Example 3
Hydrocarbon synthesis catalyst (Co/Mn/alumina/silica catalyst (Co, Mn, alumina, silica mass fractions of 0.6%, 0.4%, 70%, 29%, respectively, catalyst average particle size of 270-micron) and aromatization catalyst (MoO)3Fe/beta molecular sieve/alumina, wherein alumina, beta molecular sieve, MoO3Fe mass fractions of 58%, 36%, 3%, 3%, respectively, and an average particle diameter of the catalyst of 80 μm) are packed in the first catalyst packing zone 1a region in the reactor. The lower region of the reactor was preheated to 280 ℃ and synthesis gas (CO and hydrogen) was fed in at a pressure of 0.1 MPa. The aromatization catalyst was blown from the first catalyst loading zone 1a into the second catalyst loading zone 1b, and the temperature of the second catalyst loading zone 1b was controlled to 480 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. The gas out of the aromatization reactor 1 is subjected to heat exchange and cooling, and then water, aromatic hydrocarbon, light hydrocarbon and synthesis gas are sequentially separated, wherein C is contained in the light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the first gas inlet 4 for continuous reaction.
The partially aromatized catalyst is pre-filled in a third catalyst filling area 13a in the catalyst regeneration two-stage fluidized bed reactor 13, argon containing 8 percent of oxygen is introduced from a second gas inlet 8 at the bottom, and generated gas in the third catalyst filling area 13a enters a fourth catalyst filling area 13b through a second transverse porous distribution plate 9. The temperatures of the third catalyst loading zone 13a and the fourth catalyst loading zone 13b were controlled at 620 ℃ and 550 ℃, respectively.
When the catalyst in the second catalyst loading zone 1b in the aromatization reactor is deactivated by carbon deposition, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline and enters the fourth catalyst loading zone 13b of the reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regenerator 13 through a second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.
Example 4
Hydrocarbon synthesis catalyst (molybdenum nitride/alumina, molybdenum nitride and alumina fractions are respectively 10% and 90%, and average particle size of catalyst is 250 micrometers) and aromatization catalyst (Fe)2O3ZnO/ZSM-5/kaolin/silica, kaolin, silica, ZSM-5 molecular sieves, Fe2O3ZnO mass fractions of 30%, 30%, 30%, 6%, 4%, respectively, and an average particle diameter of the catalyst of 75 μm) is packed in the region of the first catalyst packing zone 1a in the reactor. The lower region of the reactor was preheated to 320 ℃, synthesis gas (CO and hydrogen) was introduced, the pressure was controlled at 3.5MPa, the aromatization catalyst in the first catalyst loading zone 1a was blown into the second catalyst loading zone 1b, and the temperature of the second catalyst loading zone 1b was controlled at 400 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. The gas out of the aromatization reactor 1 is subjected to heat exchange and cooling, and then water, aromatic hydrocarbon, light hydrocarbon and synthesis gas are sequentially separated, wherein C is contained in the light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the first gas inlet 4 for continuous reaction.
The partially aromatized catalyst is pre-filled in a third catalyst filling area 13a in the catalyst regeneration two-stage fluidized bed reactor 13, oxygen is introduced from a second gas inlet 8 at the bottom, and generated gas in the third catalyst filling area 13a enters a fourth catalyst filling area 13b through a second transverse porous distribution plate 9. The temperatures of the third catalyst loading zone 13a and the fourth catalyst loading zone 13b were controlled to 550 ℃ and 480 ℃, respectively.
When the catalyst in the second catalyst loading zone 1b in the aromatization reactor is deactivated by carbon deposition, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline and enters the fourth catalyst loading zone 13b of the reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regenerator 13 through a second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.
Example 5
Mixing a synthetic hydrocarbon catalyst (molybdenum carbide/Ni/Cr/alumina, wherein the mass fractions of molybdenum carbide, Ni and Cr are respectively 10%, 15% and 18%, the rest is alumina, and the average particle size of the catalyst is 280 micrometers) and an aromatization catalyst (Bi/Ga)2O3ZSM-5/alumina type, in which Bi, Ga2O3ZSM-5, alumina in an amount of 6%, 5%, 35%, 54%, respectively, and the average particle diameter of the catalyst was 90 μm) was packed in the first catalyst packing region 1a region of the reactor. The lower region of the reactor was preheated to 280 ℃ and synthesis gas (CO and hydrogen) was fed in at a pressure of 2.5 MPa. The aromatization catalyst in the first catalyst loading zone 1a was blown into the second catalyst loading zone 1b, and the temperature of the second catalyst loading zone 1b was controlled to 450 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. The gas out of the aromatization reactor 1 is subjected to heat exchange and cooling, and then water, aromatic hydrocarbon, light hydrocarbon and synthesis gas are sequentially separated, wherein C is contained in the light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the first gas inlet 4 for continuous reaction.
The partially aromatized catalyst is pre-filled in a third catalyst filling area 13a in the catalyst regeneration two-stage fluidized bed reactor 13, nitrogen with oxygen content of 50 percent is introduced from a second gas inlet 8 at the bottom, and the generated gas in the third catalyst filling area 13a enters a fourth catalyst filling area 13b through a second transverse porous distribution plate 9. The temperatures of the third catalyst loading zone 13a and the fourth catalyst loading zone 13b were controlled to 600 ℃ and 500 ℃, respectively.
When the catalyst in the second catalyst loading zone 1b in the aromatization reactor is deactivated by carbon deposition, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline and enters the fourth catalyst loading zone 13b of the reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regenerator 13 through a second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.
Example 6
Synthesizing hydrocarbon catalyst (iron carbide/chromium oxide/alumina/zirconia, wherein the weight fractions of iron carbide, chromium oxide, alumina and zirconia are respectively 5%, 10%, 60% and 25%, and the average particle size of the catalyst is 300 micrometers) and aromatization catalyst (ZnO/Fe/CeO)2ZSM-12/silica type, in which ZnO, Fe CeO2ZSM-12, silica in mass fractions of 0.3%, 0.5%, 0.2%, 40%, 59%, and the average particle diameter of the catalyst was 100 μm) was packed in the first catalyst packing zone 1a region of the reactor. The lower region of the reactor was preheated to 350 ℃, synthesis gas (CO and hydrogen) was introduced, the pressure was controlled to 3MPa, the aromatization catalyst was blown from the first catalyst loading zone 1a into the second catalyst loading zone 1b, and the temperature of the second catalyst loading zone 1b was controlled to 500 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. The gas out of the aromatization reactor 1 is subjected to heat exchange and cooling, and then water, aromatic hydrocarbon,Light hydrocarbon and synthetic gas are separated in sequence, C is contained in light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the first gas inlet 4 for continuous reaction.
The partially aromatized catalyst is pre-filled in a third catalyst filling area 13a in the catalyst regeneration two-stage fluidized bed reactor 13, air is introduced from a second gas inlet 8 at the bottom, and generated gas in the third catalyst filling area 13a enters a fourth catalyst filling area 13b through a second transverse porous distribution plate 9. The temperatures of the third catalyst-packed section 13a and the fourth catalyst-packed section 13b were controlled to 650 deg.c and 600 deg.c, respectively.
When the catalyst in the second catalyst loading zone 1b in the aromatization reactor is deactivated by carbon deposition, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline and enters the fourth catalyst loading zone 13b of the reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regeneration reactor 13 through the second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.
Example 7
Synthesizing hydrocarbon into catalyst (cobalt carbide/Cr/ZSM-5/Al)2O3Wherein the cobalt carbide, Cr, ZSM-5 molecular sieve and Al2O310 percent, 30 percent and 50 percent respectively, the average grain diameter of the catalyst is 200 microns) and an aromatization catalyst (Fe2O3/MoO3/Cr/CeO2ZSM-5/Kaolin/Al2O3Type, Fe2O3, MoO3, Cr, La2O3ZSM-5, kaolin, Al2O33%, 2%, 5%, 5%, 20%, 30%, 35%, respectively, of the catalyst having an average particle diameter of 60 μm) is packed in the first catalyst packing zone 1a region in the reactor. The lower region of the reactor was preheated to 300 ℃ and synthesis gas (CO and hydrogen) was fed inThe aromatization catalyst was blown from the first catalyst loading zone 1a to the second catalyst loading zone 1b under a controlled pressure of 2.5MPa, and the temperature of the second catalyst loading zone 1b was controlled at 520 ℃.
The synthesis gas generates hydrocarbons in the first catalyst-packed section 1a, and the hydrocarbons further react in the second catalyst-packed section 1b to generate aromatic hydrocarbons. The aromatic hydrocarbons and the byproduct light hydrocarbons, water and unreacted synthesis gas are discharged out of the aromatization reactor 1 through the first gas outlet 7. The gas out of the aromatization reactor 1 is subjected to heat exchange and cooling, and then water, aromatic hydrocarbon, light hydrocarbon and synthesis gas are sequentially separated, wherein C is contained in the light hydrocarbon3-C8The components are circulated back to the second catalyst filling area 1b of the aromatization reactor 1 through the light hydrocarbon inlet of the first gas inlet 4 for continuous reaction.
The partially aromatized catalyst is pre-filled in a third catalyst filling area 13a in the catalyst regeneration two-stage fluidized bed reactor 13, 2 percent of nitrogen of oxygen is introduced from a second gas inlet 8 at the bottom, and the generated gas in the third catalyst filling area 13a enters a fourth catalyst filling area 13b through a second transverse porous distribution plate 9. The temperatures of the third catalyst-packed section 13a and the fourth catalyst-packed section 13b were controlled to 650 ℃ and 480 ℃, respectively.
When the catalyst in the second catalyst loading zone 1b in the aromatization reactor 1 is deactivated by carbon deposition, the catalyst is removed from the first catalyst outlet 5 of the upper section of the aromatization reactor 1, conveyed by a pipeline, and enters the fourth catalyst loading zone 13b of the reactor 13 through the second catalyst inlet 11. After burning off part of the coke, the coke passes through the second transverse porous distribution plate 9 and enters the third catalyst loading area 13 a. The gas exits the catalyst regeneration reactor 13 through the second gas outlet 10. In the third catalyst charge zone 13a, most of the coke on the catalyst is burned off. And is transported from the second catalyst outlet 12, through a pipeline, and returned to the aromatization reactor 1 through the first catalyst inlet 6.
Repeating the above steps to continuously carry out the process.

Claims (3)

1. A method for preparing aromatic hydrocarbon from synthetic gas by using a two-stage circulating fluidized bed reaction-regeneration system is characterized in that,
(1) pre-installing a synthetic hydrocarbon catalyst and an aromatization catalyst in a first catalyst loading area (1 a) of an aromatization reactor (1), preheating synthesis gas, introducing the preheated synthesis gas from a first gas inlet (2) at the lower section of the aromatization reactor (1), blowing the aromatization catalyst to a second catalyst loading area (1 b) through a first transverse porous distribution plate (3), wherein the synthesis gas mainly contacts with the catalyst for synthesizing hydrocarbons in the first catalyst loading area (1 a) to generate various hydrocarbons, passes through the first transverse porous distribution plate (3), and enters the second catalyst loading area (1 b);
(2) hydrocarbon gas contacts with the aromatization catalyst in the second catalyst filling area (1 b) to generate aromatic hydrocarbon, the aromatic hydrocarbon is discharged from the aromatization reactor (1) from a first gas outlet (7) of the reactor, and C is subjected to heat exchange and separation steps3-C8The non-aromatic hydrocarbon is recycled and enters a second catalyst filling area (1 b) from a first gas inlet (4) for recycling;
(3) pre-charging a portion of catalyst in a third catalyst loading zone (13 a) in a catalyst regeneration reactor (13), introducing an oxygen-containing gas from a bottom second gas inlet (8), passing the generated gas in the third catalyst loading zone (13 a) through a second transverse porous distribution plate (9) and into a fourth catalyst loading zone (13 b);
(4) after the carbon deposition of the catalyst in the second catalyst filling area (1 b) in the aromatization reactor (1), the carbon deposition is removed from a first catalyst outlet (5) of the aromatization reactor (1), the carbon deposition is conveyed through a pipeline and enters a fourth catalyst filling area (13 b) of a catalyst regeneration reactor (13) through a second catalyst inlet (11), the carbon deposition-containing catalyst entering from the second catalyst inlet (11) is burnt off part of the carbon deposition in the fourth catalyst filling area (13 b), the carbon deposition-containing catalyst enters a third catalyst filling area (13 a) through a second transverse porous distribution plate (9), and the gas exits the catalyst regeneration reactor (13) through a second gas outlet (10);
(5) in the third catalyst loading zone (13 a), carbon deposits on the catalyst are burnt and are conveyed from the second catalyst outlet (12), through a pipeline and returned to the aromatization reactor (1) through the first catalyst inlet (6);
(6) repeating the above steps to continuously perform the process;
the main active components of the synthetic hydrocarbon catalyst in the first catalyst filling area (1 a) in the aromatization reactor (1) are Fe, Cr, Co, Mo, Ni, Mn and one or more of the carbonization state and the nitridation state thereof, the carrier is one or more of aluminum oxide, zirconium oxide, silicon oxide and molecular sieve, the mass fraction of the active components in the total mass of the synthetic hydrocarbon catalyst is 1-50%, and the balance is the carrier; the average particle size of the catalyst is 200-350 microns;
the hydrocarbon aromatization catalyst in the second catalyst filling zone (1 b) is a catalyst of metal or metal oxide, molecular sieve and carrier, and the metal or metal oxide is Cu, Zn, Cr, Fe, Co, Ni, ZnO and CeO2，La2O3，Ga2O3、Fe2O3、MoO3One or more of ZSM-5, ZSM-12, Y molecular type and beta molecular sieve, and one or more of alumina, kaolin and silicon oxide as carrier; wherein: the mass fraction of the molecular sieve in the total mass of the hydrocarbon aromatization catalyst is 20-40%, the mass fraction of the carrier in the total mass of the hydrocarbon aromatization catalyst is 45-65%, the mass fraction of the metal or metal oxide in the total mass of the hydrocarbon aromatization catalyst is 1-15%, and the average particle size of the catalyst is 40-120 microns;
the system comprises an aromatization reactor (1) and a catalyst regeneration reactor (13) which are connected with each other through a pipeline, the aromatization reactor (1) is divided into two sections of fluidized beds, a first catalyst filling area (1 a) is arranged below the two sections of fluidized beds, a second catalyst filling area (1 b) is arranged above the two sections of fluidized beds, the bottom of the first catalyst filling area (1 a) is provided with a first gas inlet (2), a first transverse porous distribution plate (3) is arranged between the first catalyst loading area (1 a) and the second catalyst loading area (1 b), the lower part of the second catalyst filling area (1 b) is provided with a first gas inlet (4) and a first catalyst outlet (5), the top of the second catalyst filling area (1 b) is provided with a first gas outlet (7), and the upper part of the second catalyst filling area is provided with a first catalyst inlet (6);
the catalyst regeneration reactor (13) is divided into two sections of fluidized beds, and comprises a fourth catalyst filling area (13 b) at the upper part and a third catalyst filling area (13 a) at the lower part, a second gas inlet (8) is arranged at the bottom of the third catalyst filling area (13 a), and a second catalyst outlet (12) is arranged below the third catalyst filling area (13 a); a second transverse porous distribution plate (9) is arranged between the fourth catalyst loading area (13 b) and a third catalyst loading area (13 a) below the fourth catalyst loading area, and a second catalyst inlet (11) and a second gas outlet (10) at the top are arranged at the upper part of the fourth catalyst loading area (13 b);
the output end of the first catalyst outlet (5) is connected with the input end of the second catalyst inlet (11), and the output end of the second catalyst outlet (12) is connected with the input end of the first catalyst inlet (6).
2. The method for preparing aromatic hydrocarbons from synthesis gas according to claim 1, wherein the temperature of the first catalyst loading zone (1 a) is 250-380 ℃, the temperature of the second catalyst loading zone (1 b) is 450-550 ℃, and the pressure is 0.1-3.5 MPa.
3. The method for preparing aromatic hydrocarbons from synthesis gas according to claim 1, wherein the temperature of the third catalyst loading zone (13 a) is 550-650 ℃, the temperature of the fourth catalyst loading zone (13 b) is 480-600 ℃, and the pressure is 0.1-3.5 MPa.
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