CN104557363B - Methanol and/or the reaction unit of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons and reaction method thereof - Google Patents

Methanol and/or the reaction unit of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons and reaction method thereof Download PDF

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CN104557363B
CN104557363B CN201310512279.7A CN201310512279A CN104557363B CN 104557363 B CN104557363 B CN 104557363B CN 201310512279 A CN201310512279 A CN 201310512279A CN 104557363 B CN104557363 B CN 104557363B
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catalyst
reactor
methanol
conversion zone
propylene
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CN104557363A (en
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李晓红
王菊
俞志楠
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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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    • 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
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • 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
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts
    • 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
    • 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
    • Y02P30/40—Ethylene production

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Abstract

The present invention relates to a kind of methanol and/or dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons reaction unit and reaction method thereof, mainly solve the problem that in prior art, ethylene, propylene and aromatics yield are low.The present invention is by including reactor (1), regenerator (2), the system of stripper (3), raw material (6) enters reactor (1) first conversion zone (12), recycle stock (7) enters reactor (1) second conversion zone (14) and catalyst haptoreaction, the product generated and carbon deposited catalyst enter stripper (3), carbon deposited catalyst after stripping enters regenerator (2) regeneration through inclined tube to be generated (4), catalyst after regeneration enters the technical scheme of reactor (1) through regenerator sloped tube (5), preferably solve this problem, can be used for ethylene, in propylene and arene industrial production.

Description

Methanol and/or the reaction unit of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons and reaction method thereof
Technical field
The present invention relates to a kind of methanol and/or the reaction unit of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons and reaction method thereof.
Background technology
Ethylene, propylene and aromatic hydrocarbons (especially triphen, benzene Benzene, toluene Toluene, dimethylbenzene Xylene, i.e. BTX) are important basic organic synthesis raw materials.Driven by downstream derivative thing demand, the market demand sustainable growth of ethylene, propylene and aromatic hydrocarbons.
It is the main production of ethylene, propylene and aromatic hydrocarbons with the liquid hydrocarbon (such as Petroleum, diesel oil, the secondary operations oil) steam cracking process as raw material.This technique belongs to petroleum path production technology, and in recent years, the supply limited due to petroleum resources and higher price, cost of material is continuously increased.The factor being subject to, alternative materials is prepared ethylene, propylene and aromatic hydrocarbons technology and is caused and pay close attention to more and more widely.Wherein, for coal-based methanol, dimethyl ether raw material, due to rich coal resources in China, it is increasingly becoming a kind of important Chemical Manufacture raw material, becomes the important supplement of petroleum.Accordingly, it is considered to prepare ethylene, propylene and aromatic hydrocarbons with methanol and/or dimethyl ether for raw material.
In various existing methanol, dimethyl ether catalysis transformation technology, the product of methanol/dimethyl ether conversion aromatic hydrocarbons includes ethylene, propylene and aromatic hydrocarbons simultaneously.This technology initially sees Chang of Mobil company in 1977 et al. (Journal of Catalysis, 1977,47,249) and reports the method that the Hydrocarbon such as aromatic hydrocarbons are prepared in methanol and oxygenatedchemicals conversion thereof on ZSM-5 molecular sieve catalyst.1985, Mobil company is in its United States Patent (USP) US1590321 applied for, disclose methanol, the result of study of dimethyl ether conversion aromatic hydrocarbons first, this research use phosphorous be the ZSM-5 molecular sieve of 2.7 weight % be catalyst, reaction temperature is 400 ~ 450 DEG C, methanol, dimethyl ether air speed 1.3 (Grams Per Hour)/gram catalyst.
Relevant report and the patent in this field are more, but the purpose product of most of technology is aromatic hydrocarbons, and ethylene, propylene belong to by-product, and yield is low.Such as, 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, patent in terms of methanol aromatics process: United States Patent (USP) US4686312, Chinese patent ZL101244969, ZL1880288, CN101602646, CN101823929, CN101671226, CN102199069, CN102199446, CN1880288 etc..
It addition, technology path disclosed in some patent is other products such as co-producing light olefins, gasoline while methanol aromatic hydrocarbons, such as patent CN102775261, CN102146010, CN102531821, CN102190546, CN102372537 etc..
Wherein, disclosed in patent CN102775261, Multi-function methanol processing method and device utilize preparing low carbon olefin hydrocarbon with methanol, gasoline, aromatic hydrocarbons.The method uses two-step method production technology, and first step methanol feedstock produces low-carbon alkene under special-purpose catalyst 1 acts on, and the reaction gas containing low-carbon alkene after heat exchange, chilling, carrying out washing treatment, is synthesized aromatic hydrocarbons and or gasoline under the effect of special-purpose catalyst 2 by second step.The reactor of two courses of reaction can be fixed bed or fluid bed.The method uses two-step method, and technological process is complicated.
Patent CN102146010 is disclosed that with methanol for raw material production low-carbon alkene and the technique of arene parallel cogeneration gasoline.With methanol as raw material and use molecular sieve catalyst to produce low-carbon alkene and arene parallel cogeneration gasoline through methanol alkylation reaction and aromatization.The reactor of methanol alkylation reaction and aromatization is various types of fixed bed reactors, pressure 0.01 ~ 0.5 MPa, temperature 180 ~ 600 DEG C.Total liquid yield is more than 70 weight %, and triphen yield is more than 90 weight %.The method is also adopted by two reactors, and technological process is complicated.
Patent CN102531821 is disclosed that methanol and Petroleum co-fed production low-carbon alkene and/or the method for aromatic hydrocarbons, uses load 2.2 ~ 6.0 weight %La and the ZSM-5 catalyst of 1.0 ~ 2.8 weight %P, can use fixed bed reactors or fluidized-bed reactor.Reaction temperature is 550 ~ 670 DEG C, air speed 1.0 ~ 5 (Grams Per Hour)/gram catalyst.The triolefin yield of the method is higher, but BTX yield is low, only 5 ~ 17 weight %.
Patent CN102372537 and CN102190546 disclose the method for preparing propylene by methanol transformation and aromatic hydrocarbons.These two patents are to develop on the basis of preparing propylene by methanol transformation technology, and propylene is the product of argument, and aromatics yield is relatively low.
Above-mentioned patented technology all exists the problem that ethylene, propylene and aromatics yield are low.Propose technical scheme to the property of the present invention is directed to, solve the problems referred to above.
Summary of the invention
One of the technical problem to be solved is the technical problem that ethylene in prior art, propylene and aromatics yield are low, it is provided that a kind of methanol and/or dimethyl ether conversion ethylene and propylene and the reaction unit of aromatic hydrocarbons.This system has ethylene, propylene, advantage that aromatics yield is high.
The two of the technical problem to be solved are to provide a kind of reaction method corresponding with solving one of technical problem.
For solving one of the problems referred to above, the technical solution used in the present invention is as follows: a kind of methanol and/or the reaction unit of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, including reactor 1, regenerator 2, stripper 3；Reactor 1 is the first conversion zone 12, First Transition section the 13, second conversion zone the 14, second changeover portion the 15, the 3rd conversion zone 16 the most according to this；It is internal that 3rd conversion zone 14 is positioned at stripper 3；The height of reactor the first conversion zone 12 accounts for the 17 ~ 70% of reactor 1 total height；The diameter ratio of the second conversion zone 14 diameter and the first conversion zone 12 is 0.3 ~ 2:1, and it highly accounts for the 20 ~ 75% of reactor 1 total height；The diameter ratio of the 3rd conversion zone 16 diameter and the first conversion zone 12 is 0.3 ~ 1:1, and it highly accounts for the 3 ~ 5% of reactor 1 total height；Raw material 6 enters reactor 1 first conversion zone 12, recycle stock 7 enters reactor 1 second conversion zone 14 and catalyst haptoreaction.
In technique scheme, under maximum ethylene, propylene operator scheme, the height of reactor the first conversion zone 12 accounts for the 40 ~ 70% of total reactor height；The diameter ratio of the second conversion zone 14 diameter and the first conversion zone 12 is 0.3 ~ 1:1, and it highly accounts for the 20 ~ 50% of total reactor height；The diameter ratio of the 3rd conversion zone 16 diameter and the first conversion zone 12 is 0.3 ~ 1:1, and it highly accounts for the 3 ~ 5% of total reactor height.Under maximum aromatic hydrocarbons operator scheme, the height of reactor the first conversion zone 12 accounts for the 17 ~ 40% of total reactor height；The diameter ratio of the second conversion zone 14 diameter and the first conversion zone 12 is 1 ~ 2:1, and it highly accounts for the 50 ~ 75% of total reactor height；The diameter ratio of the 3rd conversion zone 16 diameter and the first conversion zone 12 is 0.3 ~ 1:1, and it highly accounts for the 3 ~ 5% of total reactor height.Under coproduction ethylene, propylene and aromatic hydrocarbons pattern, the height of reactor the first conversion zone 12 accounts for the 30 ~ 60% of total reactor height；The diameter ratio of the second conversion zone 14 diameter and the first conversion zone 12 is 0.3 ~ 2:1, and it highly accounts for the 30 ~ 65% of total reactor height；The diameter ratio of the 3rd conversion zone 16 diameter and the first conversion zone 12 is 0.3 ~ 1:1, and it highly accounts for the 3 ~ 5% of total reactor height.
In technique scheme, the total height of reactor First Transition section 13 and the second changeover portion 15 accounts for the 5% of reactor 1 total height.
In technique scheme, raw material 6 enters the first conversion zone 12 of reactor 1, and recycle stock 7 enters the second conversion zone 14 and the catalyst haptoreaction of reactor 1；The product generated and carbon deposited catalyst enter stripper 3, and the carbon deposited catalyst after stripping enters regenerator 2 through inclined tube 4 to be generated and regenerates, and the catalyst after regeneration enters reactor the first conversion zone 12 through regenerator sloped tube 5.
In technique scheme, reactor 1, for being converted into the product based on ethylene, propylene and aromatic hydrocarbons by raw material 6, recycle stock 7 and catalyst haptoreaction；Regenerator 2, for removing the coke on carbon deposited catalyst by the way of burning；Stripper 3, for being stripped off the product carried on carbon deposited catalyst.
In technique scheme, reactor 1 interiorly or exteriorly arranges heat collector, and heat collector height accounts for the 30% ~ 95% of height for reactor；Regenerator 2 interiorly or exteriorly arranges heat collector, and heat collector height accounts for the 30% ~ 80% of regenerator height.
In technique scheme, regenerator 2 and stripper 3 inside are equipped with one group of gas-solid cyclone separator, are 1 ~ 3 grade.
For solving the two of the problems referred to above, the technical solution used in the present invention is as follows: a kind of methanol and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, uses above-mentioned reaction unit, described reaction method to include following step:
A) raw material 6 enters the first conversion zone 12 of reactor 1, and recycle stock 7 is at the second conversion zone 14 of reactor 1, and catalyst haptoreaction, reaction of formation product and carbon deposited catalyst；
B) product and carbon deposited catalyst enter stripper 3, carbon deposited catalyst contacts stripping with stripping fluid 9, carbon deposited catalyst after the stripping afterproduct 8 obtained and stripping, stripped product 8 enters subsequent separation system after gas-solid cyclone separator separation carbon deposited catalyst；
C) carbon deposited catalyst after stripping enters regenerator 2 through inclined tube 4 to be generated and contacts with regenerating medium 10 and burn, the catalyst after being regenerated and flue gas 11；
D) catalyst after regeneration enters reactor 1 through regenerator sloped tube 5；
E) part ethane and/or propane and/or C4 and/or C5 and/or C6 is non-aromatic proceeds reaction as recycle stock 7 in the product that separated system separates, remaining using ethylene, propylene, BTX aromatics product as output of products system.
In technique scheme, raw material 6 is methanol or dimethyl ether or both mixture, preferably methanol.
In technique scheme, in raw material 6, the weight/mass percentage composition of water is 0 ~ 30 weight %, preferably shorter than 10 weight %.
In technique scheme, the temperature of reactor 1 is 400 ~ 550 DEG C, the weight space velocity of raw material 6 is 2 ~ 10 (Grams Per Hours)/gram catalyst, in terms of gauge pressure, reaction pressure is 0 ~ 0.5 MPa, the mass ratio of catalyst circulating load and raw material 6 inlet amount is 3～40: 1, average gas superficial velocity 0.7 ~ 5.0 meter per second.Under maximum ethylene, propylene operator scheme, temperature is 480 ~ 550 DEG C, the weight space velocity of raw material 6 is 4 ~ 10 (Grams Per Hours)/gram catalyst, in terms of gauge pressure, reaction pressure is 0 ~ 0.3 MPa, the mass ratio of catalyst circulating load and raw material 6 inlet amount is 10～40: 1, average gas superficial velocity 1.3 ~ 4.0 meter per second；Under maximum aromatic hydrocarbons operator scheme, temperature is 400 ~ 500 DEG C, the weight space velocity of raw material 6 is 2 ~ 4 (Grams Per Hours)/gram catalyst, in terms of gauge pressure, reaction pressure is 0.1 ~ 0.5 MPa, the mass ratio of catalyst circulating load and raw material 6 inlet amount is 3～30: 1, average gas superficial velocity 0.7 ~ 1.3 meter per second；Under coproduction ethylene, propylene and aromatic hydrocarbons pattern, temperature is 440 ~ 520 DEG C, the weight space velocity of raw material 6 is 2 ~ 7 (Grams Per Hours)/gram catalyst, in terms of gauge pressure, reaction pressure is 0.1 ~ 0.4 MPa, the mass ratio of catalyst circulating load and raw material 6 inlet amount is 5～35: 1, average gas superficial velocity 0.7 ~ 2.3 meter per second.
In technique scheme, the temperature of regenerator 2 is 580 ~ 720 DEG C, preferably 600 ~ 700 DEG C, further preferred 630 ~ 680 DEG C.
In technique scheme, the charcoal on catalyst after regeneration, with the mass percent of catalyst, content is less than 0.1 weight %.
In technique scheme, catalyst activity component is ZSM-5, ZSM-23, ZSM-11, beta-molecular sieve, Y molecular sieve or the composite molecular screen formed each other, preferably ZSM-5；Carrier is Kaolin, aluminium oxide, silicon dioxide；The mass ratio of active component and carrier is (10 ~ 50): (50 ~ 90), preferably (20 ~ 40): (60 ~ 80).
In technique scheme, catalyst is loaded with in Zn, Ag, P, Ga, Cu, Mn, Mg one or more elements or oxide, preferably Zn, P；With the mass percent of catalyst, the element of load content on a catalyst is 0.01 ~ 15 weight %, preferably 0.02 ~ 8 weight %.
In technique scheme, the active component of catalyst is selected from ZSM-5 molecular sieve, in terms of the percentage by weight of catalyst, catalyst loads Zn element or oxide, the P element of 0.1 ~ 8 weight % or the oxide of 0.01 ~ 5 weight %.
In technique scheme, stripping fluid 9 is water vapour or N2Or water vapour and N2Mixture, regenerating medium 10 is air or air and O2Mixture or air and N2Mixture.
The present invention is recycled with by-product by the separation of product during methanol and/or dimethyl ether catalysis conversion reaction, it is achieved the purpose of the yield of maximum ethylene, propylene and aromatic hydrocarbons.And reactor reducing, raw material of different nature and recycle stock can be made to react under the most suitable reaction condition respectively, improve purpose product yield further.
The technical scheme that the present invention provides, optional different reaction condition realizes maximum ethylene, propylene, maximum aromatic hydrocarbons and coproduction ethylene, the propylene operator scheme that produce purpose different with three kinds of aromatic hydrocarbons.
Use technical scheme, operate under maximum ethylene, propylene pattern, raw material 6 is methanol, the reaction temperature of reactor 1 is 500 DEG C, in terms of gauge pressure, reaction pressure is 0.2 MPa, the weight space velocity of methanol is 5 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 15:1, average gas superficial velocity 1.6 meter per second；Use Cu-ZSM-5 catalyst；Ethylene carbon base absorption rate be 25.7 weight %, propylene carbon base absorption rate be 20.3 weight %, aromatic hydrocarbons carbon base absorption rate be 40.2 weight %, BTX carbon base absorption rate is 27.9 weight %.
Use technical scheme, operate under maximum aromatic hydrocarbons pattern, raw material 6 is methanol, the reaction temperature of reactor 1 is 475 DEG C, in terms of gauge pressure, reaction pressure is 0.25 MPa, the weight space velocity of methanol is 2 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 7:1, average gas superficial velocity 0.7 meter per second；Use Zn-P-ZSM-5 catalyst；Ethylene carbon base absorption rate be 12.1 weight %, propylene carbon base absorption rate be 7.8 weight %, aromatic hydrocarbons carbon base absorption rate be 70.5 weight %, BTX carbon base absorption rate is 55.4 weight %.
Use technical scheme, operate under coproduction ethylene, propylene and aromatic hydrocarbons pattern, raw material 6 is methanol, the reaction temperature of reactor 1 is 460 DEG C, in terms of gauge pressure, reaction pressure is 0.2 MPa, the weight space velocity of methanol is 3 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 12:1, average gas superficial velocity 1 meter per second；Use Zn-Mg-P-ZSM-5 catalyst；Methanol feeds；Ethylene carbon base absorption rate be 17.5 weight %, propylene carbon base absorption rate be 12.0 weight %, aromatic hydrocarbons carbon base absorption rate be 58.5 weight %, BTX carbon base absorption rate is 45.7 weight %.
Accompanying drawing explanation
Fig. 1 is the reaction unit schematic diagram of the present invention,
Fig. 2 is the schematic diagram of reactor.
In Fig. 1 ~ 2,1 is reactor；2 is regenerator；3 is stripper；4 is inclined tube to be generated；5 is regenerator sloped tube；6 is raw material；7 is recycle stock；8 is product；9 is stripping fluid；10 is regenerating medium；11 is flue gas；12 is reactor the first conversion zone；13 is reactor First Transition section；14 is reactor the second conversion zone；15 is reactor the second changeover portion；16 is reactor the 3rd conversion zone.
In Fig. 1, raw material 6 enters the first conversion zone 12 of reactor 1, and recycle stock 7 is at the second conversion zone 14 of reactor 1, and catalyst haptoreaction, reaction of formation product and carbon deposited catalyst；Product and carbon deposited catalyst enter stripper 3, and carbon deposited catalyst contacts stripping with stripping fluid 9, and the carbon deposited catalyst after the stripping afterproduct 8 obtained and stripping, stripped product 8 enters subsequent separation system after gas-solid cyclone separator separation carbon deposited catalyst；Carbon deposited catalyst after stripping enters regenerator 2 through inclined tube 4 to be generated and contacts with regenerating medium 10 and burn, the catalyst after being regenerated and flue gas 11；Catalyst after regeneration enters reactor 1 through regenerator sloped tube 5；Part ethane and/or propane and/or C4 and/or C5 and/or C6 is non-aromatic proceeds reaction as recycle stock 7 in the product that separated system separates, remaining using ethylene, propylene, BTX aromatics product as output of products system.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1]
Use device as shown in Figure 1.
A diameter of 4 meters of reactor the first conversion zone, highly account for the 50% of total reactor height；The diameter ratio of the second conversion zone diameter and the first conversion zone is 0.5:1, and it highly accounts for the 40% of total reactor height；The diameter ratio of the 3rd conversion zone diameter and the second conversion zone is 0.3:1, and it highly accounts for the 5% of total reactor height.The height of First Transition section accounts for the 3% of total reactor height, and the height of the second changeover portion accounts for the 2% of total reactor height.Arranging heat collector outside reactor, heat collector height accounts for the 85% of height for reactor.Arranging heat collector outside regenerator, heat collector height accounts for the 80% of regenerator height.
The reaction condition of reactor is: temperature is 500 DEG C, in terms of gauge pressure, reaction pressure is 0.2 MPa, the weight space velocity of methanol is 5 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 15: 1, average gas superficial velocity 1.3 meter per second.The temperature of regenerator is 650 DEG C.
Stripping fluid is water vapour.Regenerating medium is air.
With methanol as raw material, water content is 5 weight %.Mass ratio non-aromatic for ethane propane C4 and C5 and C6 in recycle stock is 2:3:5.Methanol and recycle stock charge-mass ratio are 15:1.
Use Cu-ZSM-5 catalyst.
The preparation process of Cu-ZSM-5 catalyst: by ZSM-5 molecular sieve, carrier and binding agent mechanical mixture, adds suitable quantity of water, HCl, controls pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the ZSM-5 catalyst intermediate of 60 ~ 300 mesh.The mass ratio of ZSM-5 molecular sieve and substrate is 4:6；The silicoaluminophosphate molecular ratio of ZSM-5 molecular sieve is 25；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 7:3.It is the solution of 5% by Cu mass of ion percentage composition, impregnates for 1.74:1 with the weight ratio of solution and catalyst, be dried 5 hours at 120 DEG C, place into Muffle furnace roasting at 550 DEG C and within 6 hours, be prepared as the Cu-ZSM-5 catalyst that Cu constituent content is 8 weight %.
Reaction result is shown in Table 1.
[embodiment 2]
Use device as shown in Figure 1.
A diameter of 1.5 meters of reactor the first conversion zone, highly account for the 17% of total reactor height；The diameter ratio of the second conversion zone diameter and the first conversion zone is 2:1, and it highly accounts for the 75% of total reactor height；The diameter ratio of the 3rd conversion zone diameter and the second conversion zone is 1:1, and it highly accounts for the 3% of total reactor height.The height of First Transition section accounts for the 2% of total reactor height, and the height of the second changeover portion accounts for the 3% of total reactor height.Arranging heat collector outside reactor, heat collector height accounts for the 95% of height for reactor.Arranging heat collector outside regenerator, heat collector height accounts for the 30% of regenerator height.
The reaction condition of reactor is: temperature is 400 DEG C, in terms of gauge pressure, reaction pressure is 0.5 MPa, the weight space velocity of methanol is 4 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 3: 1, average gas superficial velocity 1.3 meter per second.The temperature of regenerator is 680 DEG C.
Stripping fluid is N2.Regenerating medium is air.
With methanol as raw material, water content is 30 weight %.Mass ratio non-aromatic for ethane propane C4 and C5 and C6 in recycle stock is 1:1:8.Methanol and recycle stock charge-mass ratio are 12:1.
Use Ag-Y-ZSM-23 catalyst.
The preparation process of Ag-Y-ZSM-23 catalyst: by Y molecular sieve, ZSM-23 molecular screen, carrier and binding agent mechanical mixture, add suitable quantity of water, HCl, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the Y-ZSM-23 catalyst intermediate of 60 ~ 300 mesh.The mass ratio of molecular sieve and substrate is 1:9；Y molecular sieve and ZSM-23 molecular screen mass ratio are 3:7；The silicoaluminophosphate molecular ratio of Y molecular sieve is 10；The silicoaluminophosphate molecular ratio of ZSM-23 molecular screen is 60；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 8:2.It is the solution of 1% by Ag mass of ion percentage composition, impregnate with solution and catalyst weight than for 0.1:1, it is dried 5 hours at 120 DEG C, places into Muffle furnace roasting at 550 DEG C and within 6 hours, be prepared as the Ag-Y-ZSM-23 catalyst that Ag constituent content is 0.1 weight %.
Reaction result is shown in Table 1.
[embodiment 3]
Use device as shown in Figure 1.
A diameter of 6 meters of reactor the first conversion zone, highly account for the 70% of total reactor height；The diameter ratio of the second conversion zone diameter and the first conversion zone is 0.3:1, and it highly accounts for the 20% of total reactor height；The diameter ratio of the 3rd conversion zone diameter and the second conversion zone is 0.3:1, and it highly accounts for the 5% of total reactor height.The height of First Transition section accounts for the 2.5% of total reactor height, and the height of the second changeover portion accounts for the 2.5% of total reactor height.Arranging heat collector in reactor, heat collector height accounts for the 30% of height for reactor.Arranging heat collector in regenerator, heat collector height accounts for the 30% of regenerator height.
The reaction condition of reactor is: temperature is 550 DEG C, in terms of gauge pressure, reaction pressure is 0 MPa, the weight space velocity of methanol is 10 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 40: 1, average gas superficial velocity 4 meter per second.The temperature of regenerator is 580 DEG C.
Stripping fluid is water vapour.Regenerating medium is air and O2Mixture, volume ratio is 8: 2.
With methanol as raw material, water content is 10 weight %.Mass ratio non-aromatic for propane C4 and C5 and C6 in recycle stock is 2:8.Methanol and recycle stock charge-mass ratio are 10:1.
Use Ga-beta catalyst.
The preparation process of Ga-beta catalyst: by beta-molecular sieve, carrier and binding agent mechanical mixture, adds suitable quantity of water, HCl, controls pH value not less than 4, serosity stir after at 500 DEG C spray shaping, make the beta catalyst intermediate of 60 ~ 300 mesh.The mass ratio of beta-molecular sieve and substrate is 5:5；The silicoaluminophosphate molecular ratio of beta-molecular sieve is 20；Substrate is the mixture of Kaolin, silicon dioxide and aluminium sesquioxide, and the mass ratio of three is 7:1:2.It is the solution of 2% by Ga mass of ion percentage composition, impregnates than for 0.4:1 with solution and catalyst weight, be dried 5 hours at 120 DEG C, place into Muffle furnace roasting at 550 DEG C and within 6 hours, be prepared as the Ga-beta catalyst that Ga constituent content is 0.8 weight %.
Reaction result is shown in Table 1.
[embodiment 4]
Use device as shown in Figure 1.
A diameter of 3 meters of reactor the first conversion zone, highly account for the 31% of total reactor height；The diameter ratio of the second conversion zone diameter and the first conversion zone is 1.5:1, and it highly accounts for the 60% of total reactor height；The diameter ratio of the 3rd conversion zone diameter and the second conversion zone is 0.5:1, and it highly accounts for the 4% of total reactor height.The height of First Transition section accounts for the 3% of total reactor height, and the height of the second changeover portion accounts for the 2% of total reactor height.Arranging heat collector outside reactor, heat collector height accounts for the 60% of height for reactor.Arranging heat collector outside regenerator, heat collector height accounts for the 70% of regenerator height.
The reaction condition of reactor is: temperature is 500 DEG C, in terms of gauge pressure, reaction pressure is 0.5 MPa, the weight space velocity of methanol is 4 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 30: 1, average gas superficial velocity 1.3 meter per second.The temperature of regenerator is 700 DEG C.
Stripping fluid is water vapour and N2Mixture, volume ratio is 5: 5.Regenerating medium is air and N2Mixture, volume ratio is 9: 1.
With dimethyl ether as raw material.Mass ratio non-aromatic for ethane C4 and C5 and C6 in recycle stock is 3:7.Methanol and recycle stock charge-mass ratio are 14:1.
Use Mn-ZSM-11 catalyst.
The preparation process of Mn-ZSM-11 catalyst: by ZSM-11 molecular sieve, carrier and binding agent mechanical mixture, add suitable quantity of water, HCl, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the ZSM-11 catalyst intermediate of 60 ~ 300 mesh.The mass ratio of ZSM-11 molecular sieve and substrate is 3:7；The silicoaluminophosphate molecular ratio of ZSM-11 molecular sieve is 50；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 7:3.It is the solution of 10% by Mn mass of ion percentage composition, impregnate with the weight ratio of solution and catalyst for 1:1, it is dried 5 hours at 120 DEG C, places into Muffle furnace roasting at 550 DEG C and within 6 hours, be prepared as the Mn-ZSM-11 catalyst that Mn constituent content is 9.09 weight %.
Reaction result is shown in Table 1.
[embodiment 5]
Use the device of embodiment 4.
The reaction condition of reactor is: temperature is 475 DEG C, in terms of gauge pressure, reaction pressure is 0.25 MPa, the weight space velocity of methanol is 2 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 20: 1, average gas superficial velocity 0.7 meter per second.The temperature of regenerator is 630 DEG C.
Stripping fluid is water vapour.Regenerating medium is air and O2Mixture, volume ratio is 9: 1.
With methanol as raw material, water content is 15 weight %.In recycle stock, the mass ratio of ethane propane is 5:5.Methanol and recycle stock charge-mass ratio are 16:1.
Use Zn-P-ZSM-5 catalyst.
The preparation process of Zn-P-ZSM-5 catalyst: by ZSM-5 molecular sieve, carrier and binding agent mechanical mixture, adds suitable quantity of water, H3PO4, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the P-ZSM-5 catalyst intermediate of 60 ~ 300 mesh.H3PO4The concentration of solution be the weight ratio of 1 weight %, solution and molecular sieve be 1.53:1.The mass ratio of ZSM-5 molecular sieve and substrate is 3.5:6.5；The silicoaluminophosphate molecular ratio of ZSM-5 molecular sieve is 25；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 7:3.It is the solution of 5% by Zn mass of ion percentage composition, impregnate with solution and P-ZSM-5 catalyst weight than for 0.6:1, it is dried 5 hours at 120 DEG C, place into Muffle furnace roasting 6 hours at 550 DEG C, being prepared as Zn constituent content is 2.87 weight %, and P element content is the Zn-P-ZSM-5 catalyst of 1.48 weight %.
Reaction result is shown in Table 1.
[embodiment 6]
Use device as shown in Figure 1.
A diameter of 4 meters of reactor the first conversion zone, highly account for the 40% of total reactor height；The diameter ratio of the second conversion zone diameter and the first conversion zone is 0.8:1, and it highly accounts for the 52% of total reactor height；The diameter ratio of the 3rd conversion zone diameter and the second conversion zone is 0.5:1, and it highly accounts for the 3% of total reactor height.The height of First Transition section accounts for the 2% of total reactor height, and the height of the second changeover portion accounts for the 3% of total reactor height.Arranging heat collector in reactor, heat collector height accounts for the 90% of height for reactor.Arranging heat collector outside regenerator, heat collector height accounts for the 50% of regenerator height.
The reaction condition of reactor is: temperature is 520 DEG C, in terms of gauge pressure, reaction pressure is 0.4 MPa, the weight space velocity of methanol is 7 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 35: 1, average gas superficial velocity 2.3 meter per second.The temperature of regenerator is 600 DEG C.
Stripping fluid is water vapour and N2Mixture, volume ratio is 2: 8.Regenerating medium is air and O2Mixture, volume ratio is 5: 5.
With methanol as raw material, water content is 3 weight %.Mass ratio non-aromatic for ethane propane C4 and C5 and C6 in recycle stock is 3:3:4.Methanol and recycle stock charge-mass ratio are 12.5:1.
Use ZSM-5-beta catalyst.
The preparation process of ZSM-5-beta catalyst: by ZSM-5 molecular sieve, beta-molecular sieve, carrier and binding agent mechanical mixture, add suitable quantity of water, HCl, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the ZSM-5-beta catalyst of 60 ~ 300 mesh.The mass ratio of ZSM-5 and beta-molecular sieve and substrate is 3.5: 6.5.The silicoaluminophosphate molecular ratio of ZSM-5 molecular sieve is 38；The silicoaluminophosphate molecular ratio of beta-molecular sieve is 20；The mass ratio of ZSM-5 and beta-molecular sieve is 9:1.Substrate is the mixture of Kaolin, silicon dioxide and aluminium sesquioxide, and the mass ratio of three is 5:2:3.
Reaction result is shown in Table 1.
[embodiment 7]
Use the device of embodiment 6.
The reaction condition of reactor is: temperature is 440 DEG C, in terms of gauge pressure, reaction pressure is 0.1 MPa, the weight space velocity of methanol is 2 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 5: 1, average gas superficial velocity 0.9 meter per second.The temperature of regenerator is 720 DEG C.
Stripping fluid is water vapour.Regenerating medium is air and N2Mixture, volume ratio is 7: 3.
With methanol as raw material, water content is 7 weight %.Mass ratio non-aromatic for ethane propane C4 and C5 and C6 in recycle stock is 0.5:0.5:9.Methanol and recycle stock charge-mass ratio are 20:1.
Use Zn-Ag-P-ZSM-5 catalyst.
The preparation process of Zn-Ag-P-ZSM-5 catalyst: by ZSM-5 molecular sieve, carrier and binding agent mechanical mixture, adds suitable quantity of water, H3PO4, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the P-ZSM-5 catalyst intermediate of 60 ~ 300 mesh.H3PO4The concentration of solution be the weight ratio of 2.5 weight %, solution and molecular sieve be 2:1.The mass ratio of ZSM-5 molecular sieve and substrate is 3.5:6.5；The silicoaluminophosphate molecular ratio of ZSM-5 molecular sieve is 28；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 8:2.By Ag mass of ion percentage composition be 1%, Zn mass of ion percentage composition be the solution of 3%, impregnate with solution and P-ZSM-5 catalyst weight than for 0.8:1, it is dried 5 hours at 120 DEG C, place into Muffle furnace roasting 6 hours at 550 DEG C, being prepared as Zn constituent content is 2.32 weight %, Ag constituent content is 0.78 weight %, and P element content is the Zn-Ag-P-ZSM-5 catalyst of 1.51 weight %.
Reaction result is shown in Table 1.
[embodiment 8]
Use device as shown in Figure 1.
A diameter of 4 meters of reactor the first conversion zone, highly account for the 50% of total reactor height；The diameter ratio of the second conversion zone diameter and the first conversion zone is 0.7:1, and it highly accounts for the 42% of total reactor height；The diameter ratio of the 3rd conversion zone diameter and the second conversion zone is 0.4:1, and it highly accounts for the 3% of total reactor height.The height of First Transition section accounts for the 2.5% of total reactor height, and the height of the second changeover portion accounts for the 2.5% of total reactor height.Arranging heat collector outside reactor, heat collector height accounts for the 90% of height for reactor.Arranging heat collector in regenerator, heat collector height accounts for the 80% of regenerator height.
The reaction condition of reactor is: temperature is 490 DEG C, in terms of gauge pressure, reaction pressure is 0.2 MPa, the weight space velocity of methanol is 2 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and methanol inlet amount is 35: 1, average gas superficial velocity 0.8 meter per second.The temperature of regenerator is 630 DEG C.
Stripping fluid is water vapour and N2Mixture, volume ratio is 8: 2.Regenerating medium is air and O2Mixture, volume ratio is 7: 3.
With methanol as raw material.Mass ratio non-aromatic for ethane propane C4 and C5 and C6 in recycle stock is 1:1:8.Methanol and recycle stock charge-mass ratio are 30:1.
Use Zn-Mg-P-ZSM-5 catalyst.
The preparation process of Zn-Mg-P-ZSM-5 catalyst: by ZSM-5 molecular sieve, carrier and binding agent mechanical mixture, adds suitable quantity of water, H3PO4, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make the P-ZSM-5 catalyst intermediate of 60 ~ 300 mesh.H3PO4The concentration of solution be the weight ratio of 4 weight %, solution and molecular sieve be 2:1.The mass ratio of ZSM-5 molecular sieve and substrate is 3:7；The silicoaluminophosphate molecular ratio of ZSM-5 molecular sieve is 32；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 7:3.By Mg mass of ion percentage composition be 2%, Zn mass of ion percentage composition be the solution of 3%, impregnate with solution and P-ZSM-5 catalyst weight than for 1:1, it is dried 5 hours at 120 DEG C, place into Muffle furnace roasting 6 hours at 550 DEG C, being prepared as Zn constituent content is 2.86 weight %, Mg constituent content is 1.9 weight %, and P element content is the Zn-Mg-P-ZSM-5 catalyst of 2.35 weight %.
Reaction result is shown in Table 1.
Table 1
Yield of ethene, weight % Propene yield, weight % Aromatics yield, weight %
Embodiment 1 26.7 19.1 42.8
Embodiment 2 12.3 9.8 61.9
Embodiment 3 29.2 18.5 39.7
Embodiment 4 13.8 9.2 63.7
Embodiment 5 11.7 8.4 69.1
Embodiment 6 17.9 15.2 51.7
Embodiment 7 15.8 14.7 55
Embodiment 8 18.1 13.4 57.3

Claims (9)

1. methanol and/or a reaction method for dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, the reaction unit of employing includes reactor (1), regenerator (2), stripper (3)；Reactor (1) is the first conversion zone (12), First Transition section (13), the second conversion zone (14), the second changeover portion (15), the 3rd conversion zone (16) the most according to this；It is internal that 3rd conversion zone (16) is positioned at stripper (3)；The height of reactor the first conversion zone (12) accounts for the 17～70% of reactor (1) total height；The diameter ratio of the second conversion zone (14) diameter and the first conversion zone (12) is 0.3～2:1, and it highly accounts for the 20～75% of reactor (1) total height；The diameter ratio of the 3rd conversion zone (16) diameter and the first conversion zone (12) is 0.3～1:1, and it highly accounts for the 3～5% of reactor (1) total height；Raw material (6) at reactor (1) first conversion zone (12), recycle stock (7) in reactor (1) second conversion zone (14) and catalyst haptoreaction；
Reaction method includes following step:
A) raw material (6) enters first conversion zone (12) of reactor (1), recycle stock (7) is at second conversion zone (14) of reactor (1), with catalyst haptoreaction, reaction of formation product and carbon deposited catalyst；
B) product and carbon deposited catalyst enter stripper (3), carbon deposited catalyst contacts stripping with stripping fluid (9), carbon deposited catalyst after the stripped product (8) obtained and stripping, stripped product (8) enters subsequent separation system after gas-solid cyclone separator separation carbon deposited catalyst；
C) carbon deposited catalyst after stripping enters regenerator (2) through inclined tube to be generated (4) and contacts with regenerating medium (10) and to burn, the catalyst after being regenerated and flue gas (11)；
D) catalyst after regeneration enters reactor (1) through regenerator sloped tube (5)；
E) part ethane and/or propane and/or C4 and/or C5 and/or C6 is non-aromatic proceeds reaction as recycle stock (7) in the product that separated system separates, remaining using ethylene, propylene, BTX aromatics product as output of products system.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterised in that the total height of reactor First Transition section (13) and the second changeover portion (15) accounts for the 5% of reactor (1) total height.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterized in that product that reactor (1) generates and carbon deposited catalyst enter stripper (3), carbon deposited catalyst after stripping enters regenerator (2) regeneration through inclined tube to be generated (4), and the catalyst after regeneration enters reactor the first conversion zone (12) through regenerator sloped tube (5).
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterised in that reactor (1) interiorly or exteriorly arranges heat collector, heat collector height accounts for the 30%～95% of height for reactor；Regenerator (2) interiorly or exteriorly arranges heat collector, and heat collector height accounts for the 30%～80% of regenerator height.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterised in that regenerator (2) and stripper (3) inside are equipped with 1～3 grade of gas-solid cyclone separator.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, the temperature that it is characterized in that reactor (1) is 400～550 DEG C, the weight space velocity of raw material (6) is 2～10 (Grams Per Hours)/gram catalyst, in terms of gauge pressure, reaction pressure is 0～0.5 MPa, the mass ratio of catalyst circulating load and raw material (6) inlet amount is 3～40: 1, average gas superficial velocity 0.7～5.0 meter per second；The temperature of regenerator (2) is 580～720 DEG C, the charcoal on catalyst after regeneration, and with the mass percent of catalyst, content is less than 0.1 weight %.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterised in that the active component of catalyst is ZSM-5, ZSM-23, ZSM-11, beta-molecular sieve, Y molecular sieve or the composite molecular screen formed each other；Carrier is Kaolin, aluminium oxide, silicon dioxide；The mass ratio of active component and carrier is (10～50): (50～90)；Catalyst is loaded with in Zn, Ag, P, Ga, Cu, Mn, Mg one or more elements or oxide, and with the mass percent of catalyst, its content is 0.01～15 weight %.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterised in that raw material (6) is methanol or dimethyl ether or both mixture, and the weight/mass percentage composition of water is 0.01～30 weight %.
Methanol the most according to claim 1 and/or the reaction method of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, it is characterised in that stripping fluid (9) is water vapour or N2Or water vapour and N2Mixture, regenerating medium (10) is air or air and O2Mixture or air and N2Mixture.
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