CN104549072B - Fluidized bed reaction system and method for preparing ethylene, propylene and aromatic hydrocarbon by converting methanol and/or dimethyl ether - Google Patents

Fluidized bed reaction system and method for preparing ethylene, propylene and aromatic hydrocarbon by converting methanol and/or dimethyl ether Download PDF

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CN104549072B
CN104549072B CN201310512281.4A CN201310512281A CN104549072B CN 104549072 B CN104549072 B CN 104549072B CN 201310512281 A CN201310512281 A CN 201310512281A CN 104549072 B CN104549072 B CN 104549072B
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catalyst
reactor
regenerator
propylene
reaction
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CN104549072A (en
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李晓红
钟思青
金永明
王莉
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • 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
    • 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
    • B01J8/005—Separating solid material from the gas/liquid stream
    • B01J8/0055—Separating solid material from the gas/liquid stream using cyclones
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
    • 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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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a fluidized bed reaction system and a fluidized bed reaction method for preparing ethylene, propylene and aromatic hydrocarbon by converting methanol and/or dimethyl ether. According to the fluidized bed reaction system and the fluidized bed reaction method, the problem that ethylene, propylene and aromatic hydrocarbon are low yield in the prior art are mainly solved. The fluidized bed reaction system comprises a reactor (1), a regenerator (2) and a stripper (3); raw materials (8) are fed to the bottom of a reactor reaction section (15) to be subjected to contact reaction with a catalyst, after the reaction, a carbon deposit catalyst is downwards conveyed into the stripper (3) through a to-be-generated inclined tube (4) which is connected with the bottom of the reactor (1), the stripped catalyst is upwards conveyed to the regenerator (2) through a stripping inclined tube (5) and a stripping vertical tube (6) and is regenerated, the regenerated catalyst is downwards conveyed to the reactor reaction section (15) through a catalyst regenerating inclined tube (7). According to the technical scheme, the problems are well solved. The fluidized bed reaction system and the fluidized bed reaction method can be well applied to the industrial production of ethylene, propylene and aromatic hydrocarbon.

Description

Methanol and/or the fluid bed of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Response system and reaction method thereof
Technical field
The present invention relates to a kind of methanol and/or the fluidized bed reaction system of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons and reaction thereof Method.
Background technology
Ethylene, propylene and aromatic hydrocarbons (especially triphen, benzene Benzene, toluene Toluene, dimethylbenzene Xylene, i.e. BTX) It it is important basic organic synthesis raw material.Being driven by downstream derivative thing demand, the market demand of ethylene, propylene and aromatic hydrocarbons is held Continuous growth.
It is ethylene, propylene and virtue with the liquid hydrocarbon (such as Petroleum, diesel oil, the secondary operations oil) steam cracking process as raw material The main production of hydrocarbon.This technique belongs to petroleum path production technology, in recent years, due to the supply that petroleum resources are limited 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 Pay close attention to more and more widely.Wherein, for coal-based methanol, dimethyl ether raw material, due to rich coal resources in China, the most gradually Become a kind of important Chemical Manufacture raw material, become the important supplement of petroleum.Accordingly, it is considered to methanol and/or dimethyl ether Ethylene, propylene and aromatic hydrocarbons is prepared for raw material.
In various existing methanol, dimethyl ether catalysis transformation technology, the product of methanol/dimethyl ether conversion aromatic hydrocarbons includes simultaneously Ethylene, propylene and aromatic hydrocarbons.This technology initially see Chang of Mobil company in 1977 et al. (Journal of Catalysis, 1977,47,249) report methanol and oxygenatedchemicals conversion thereof on ZSM-5 molecular sieve catalyst and prepare the carbon such as aromatic hydrocarbons The method of hydrogen compound.1985, Mobil company, in its United States Patent (USP) US1590321 applied for, disclosed first first Alcohol, the result of study of dimethyl ether conversion aromatic hydrocarbons, it is that the ZSM-5 molecular sieve of 2.7 weight % is for being catalyzed that this research uses phosphorous Agent, 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, yield is low.Such as, the patent in terms of methanol arenes catalytic agent: Chinese patent CN102372535, CN102371176、CN102371177、CN102372550、CN102372536、CN102371178、CN102416342、 CN101550051, United States Patent (USP) US4615995, US2002/0099249A1 etc..Such as, about methanol aromatic hydrocarbons work Patent in terms of skill: 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, Multi-function methanol processing method and device disclosed in patent CN102775261 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 under special-purpose catalyst 1 acts on Carbon olefin, second step by the reaction gas containing low-carbon alkene after heat exchange, chilling, carrying out washing treatment, at the work of special-purpose catalyst 2 With lower synthesis aromatic hydrocarbons and or gasoline.The reactor of two courses of reaction can be fixed bed or fluid bed.The method uses two-step method, 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 aromatic hydrocarbons also through methanol alkylation reaction and aromatization Coproduction gasoline.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, 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, adopts With load 2.2～6.0 weight %La and the ZSM-5 catalyst of 1.0～2.8 weight %P, fixed bed reactors or fluidisation can be used 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 relatively Height, 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 specially Profit is 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 technology to the property of the present invention is directed to Scheme, solves 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, A kind of methanol and/or the fluidized bed reaction system of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons are provided.This system have ethylene, Propylene and the high advantage of aromatics yield.
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 dimethyl ether conversion ethylene, Propylene and the fluidized bed reaction system of aromatic hydrocarbons, including reactor 1, regenerator 2, stripper 3；Reactor 1 is from bottom to top Conversion zone 15, changeover portion 16, dilute phase section 17；Raw material 8 enters bottom reactor reaction section 15 and catalyst haptoreaction, Reacted carbon deposited catalyst is descending, and warp enters stripper 3, after stripping with the inclined tube to be generated 4 being connected bottom reactor 1 Catalyst goes upward to regenerator 2 regenerate through stripping inclined tube 5, stripping standpipe 6, and the catalyst after regeneration is through regenerator sloped tube 7 times Walk to reactor reaction section 15.
In technique scheme, reactor 1 is conversion zone 15, changeover portion 16, dilute phase section 17 from bottom to top.
In technique scheme, the height of reactor 1 conversion zone 15 accounts for the 60～85% of total reactor height；Dilute phase section 17 The diameter ratio of diameter and conversion zone 15 is 1.1～2:1, and it highly accounts for the 10～35% of total reactor height.
In technique scheme, changeover portion 16 highly accounts for the 5% of total reactor height.
In technique scheme, bottom reactor reaction section 15 to inclined tube 4 to be generated and reactor reaction section 15 junction away from From less than the 50% of reactor reaction section 15 overall length.
In technique scheme, reactor 1 interiorly or exteriorly arranges heat collector, and heat collector height accounts for height for reactor 30%～95%；Regenerator 2 interiorly or exteriorly arranges heat collector, and heat collector height accounts for the 30%～80% of regenerator height.
In technique scheme, reactor (1), regenerator (2) and stripper (3) are internal is equipped with one group of gas-solid rotation Wind separator, is 1～3 grade.
In technique scheme, reactor 1, for raw material 8 and catalyst haptoreaction being converted into ethylene, propylene and Aromatic hydrocarbons is main product；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.
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 dimethyl ether conversion ethylene, Propylene and the fluidized bed reaction method of aromatic hydrocarbons, use above-mentioned response system, described reaction method to include following step:
A) raw material 8 enters reactor reaction section 15 and catalyst haptoreaction, reaction of formation product 9 and carbon deposited catalyst, Product 9 enters subsequent separation system after gas-solid cyclone separator separation carbon deposited catalyst；
B) carbon deposited catalyst warp enters stripper 3 and bottom stripper 3 with the inclined tube to be generated 4 being connected bottom reactor 1 The stripping fluid 12 contact stripping entered, the carbon deposited catalyst after the stripped product 13 obtained and stripping, stripped product 13 Subsequent separation system is entered after gas-solid cyclone separator separation carbon deposited catalyst；
C) carbon deposited catalyst after stripping enters stripping standpipe 6 through stripping inclined tube 5, and boosted medium 14 is promoted to regenerator 2；
D) regenerating medium 10 contact that the carbon deposited catalyst after stripping neutralizes entrance bottom regenerator 2 at regenerator 2 is burnt, Catalyst after being regenerated and flue gas 11；
E) catalyst after regeneration is advanced into reactor reaction section 15 7 times through regenerator sloped tube.
In technique scheme, the temperature of reactor 1 is 400～550 DEG C, and in terms of gauge pressure, reaction pressure is 0～0.5 MPa, Weight space velocity is 0.1～10 (Grams Per Hours)/gram catalyst, the mass ratio of catalyst circulating load and raw material 8 inlet amount be 3～ 40: 1, the density of catalyst of conversion zone 15 is 50～200 kgs/m3, average gas superficial velocity 0.01～1 meter per second.Maximum Under amount ethylene, propylene operator scheme, temperature is 480～550 DEG C, and in terms of gauge pressure, reaction pressure is 0～0.3 MPa, and weight is empty Speed is 2～10 (Grams Per Hours)/gram catalyst, and the mass ratio of catalyst circulating load and raw material 8 inlet amount is 10～40: 1, reaction The density of catalyst of section 15 is 50～140 kgs/m3, average gas superficial velocity 0.06～1 meter per second；Maximum aromatic hydrocarbons operation mould Under formula, temperature is 400～500 DEG C, and in terms of gauge pressure, reaction pressure is 0.1～0.5 MPa, weight space velocity be 0.1～2 (Grams Per Hours)/ Gram catalyst, the mass ratio of catalyst circulating load and raw material 8 inlet amount is 3～30: 1, the density of catalyst of conversion zone 15 It it is 100～200 kgs/m3, average gas superficial velocity 0.01～0.3 meter per second；Under coproduction ethylene, propylene and aromatic hydrocarbons pattern, temperature Degree is 440～520 DEG C, and in terms of gauge pressure, reaction pressure is 0.1～0.4 MPa, and weight space velocity is 0.3～4 (Grams Per Hours)/gram catalyst, The mass ratio of catalyst circulating load and raw material 8 inlet amount is 5～30: 1, and the density of catalyst of conversion zone 15 is 80～180,000 Grams m3, average gas superficial velocity 0.01～0.5 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 ℃。
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 molecule Sieve or the composite molecular screen formed each other, preferably ZSM-5；Carrier is Kaolin, aluminium oxide, silicon dioxide；Activity group Divide and the mass ratio of 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, Zn element or oxide, the P element of 0.1～8 weight % or the oxide of 0.01～5 weight % is loaded on catalyst.
In technique scheme, raw material 8 is methanol or dimethyl ether or both mixture, preferably methanol.
In technique scheme, in raw material 8, the weight/mass percentage composition of water is 0.01～30 weight %, preferably shorter than 10 weight %.
In technique scheme, stripping fluid 12 is water vapour or N2Or water vapour and N2Mixture, promote medium 14 For water vapour or N2Or water vapour and N2Mixture, regenerating medium 10 is air or air and O2Mixture or air and N2Mixture.
The technical scheme that the present invention provides, uses catalyst and the fluidized-bed reactor of reaction mass countercurrent movement, on the one hand has Promoting to effect the contact of reaction mass and catalyst active center, minimizing extends influence, and improves mass-transfer efficiency；On the other hand Air speed range of accommodation can be expanded, thus conveniently realize maximum ethylene, propylene, maximum aromatic hydrocarbons and coproduction ethylene, third The alkene operator scheme that produce purpose different with three kinds of aromatic hydrocarbons.
Use technical scheme, operate under maximum ethylene, propylene pattern, with methanol as raw material, reactor Reaction temperature is 480 DEG C, and in terms of gauge pressure, reaction pressure is 0.2 MPa, and weight space velocity is 2 (Grams Per Hours)/gram catalyst, urges The mass ratio of agent circulating load and feedstock amount is 12: 1, and in reactor, the density of catalyst of reaction zone is 80 kgs/m3, Average gas superficial velocity 0.08 meter per second；Use Cu-ZSM-5 catalyst；Methanol feeds；Ethylene carbon base absorption rate be 21.7 weight %, Propylene carbon base absorption rate be 18.3 weight %, aromatic hydrocarbons carbon base absorption rate be 41.0 weight %, BTX carbon base absorption rate is 32.8 weight %.
Use technical scheme, operate under maximum aromatic hydrocarbons pattern, with methanol as raw material, the reaction temperature of reactor Degree is 465 DEG C, and in terms of gauge pressure, reaction pressure is 0.25 MPa, and weight space velocity is 0.3 (Grams Per Hour)/gram catalyst, catalyst The mass ratio of circulating load and feedstock amount is 10: 1, and in reactor, the density of catalyst of reaction zone is 130 kgs/m3, Average gas superficial velocity 0.01 meter per second；Use Zn-P-ZSM-5 catalyst；Methanol feeds；Ethylene carbon base absorption rate is 11.1 weights Measure %, propylene carbon base absorption rate is 7.8 weight %, aromatic hydrocarbons carbon base absorption rate is 62.2 weight %, and BTX carbon base absorption rate is 49.4 weights Amount %.
Use technical scheme, operate under coproduction ethylene, propylene and aromatic hydrocarbons pattern, with methanol as raw material, reaction The reaction temperature of device is 460 DEG C, and in terms of gauge pressure, reaction pressure is 0.2 MPa, and weight space velocity is 0.5 (Grams Per Hour)/gram catalysis Agent, the mass ratio of catalyst circulating load and feedstock amount is 30: 1, and in reactor, the density of catalyst of reaction zone is 120 Kg/m3, average gas superficial velocity 0.02 meter per second；Use Zn-Mg-P-ZSM-5 catalyst；Methanol feeds；Ethylene carbon back Yield be 16.5 weight %, propylene carbon base absorption rate be 12.0 weight %, aromatic hydrocarbons carbon base absorption rate be 53.5 weight %, BTX carbon back Yield is 41.7 weight %.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram of technical scheme of the present invention.
In Fig. 1,1 is reactor；2 is regenerator；3 is stripper；4 is inclined tube to be generated；5 is stripping inclined tube；6 are Stripping standpipe；7 is regenerator sloped tube；8 is methanol and/or dimethyl ether；9 is the product of reactor；10 is regenerating medium；11 For flue gas；12 is stripping fluid；13 is stripped product；14 for promoting medium；15 is the conversion zone of reactor；16 is anti- Answer the changeover portion of device；17 is the dilute phase section of reactor.
In Fig. 1, raw material 8 enters reactor reaction section 15 and catalyst haptoreaction, and reaction of formation product 9 and carbon deposit are urged Agent, product 9 enters subsequent separation system after gas-solid cyclone separator separation carbon deposited catalyst；Carbon deposited catalyst warp The inclined tube to be generated 4 being connected with bottom reactor 1 enters stripper 3 and the stripping fluid 12 entered bottom stripper 3 connects Touching stripping, the carbon deposited catalyst after the stripped product 13 obtained and stripping, stripped product 13 separates through gas-solid cyclone separator Subsequent separation system is entered after carbon deposited catalyst；Carbon deposited catalyst after stripping enters stripping standpipe 6, warp through stripping inclined tube 5 Promote medium 14 and be promoted to regenerator 2；Carbon deposited catalyst after stripping neutralizes entrance bottom regenerator 2 at regenerator 2 Regenerating medium 10 contact is burnt, the catalyst after being regenerated and flue gas 11；Catalyst after regeneration is through regenerator sloped tube 7 times It is advanced into reactor reaction section 15；Product 9 and stripped product 13 enter subsequent separation 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 1.5 meters of the conversion zone of reactor, it highly accounts for the 80% of total reactor height, The diameter ratio of dilute phase section diameter and conversion zone is 2:1, and it highly accounts for the 15% of total reactor height.Arrange outside reactor and take Hot device, heat collector height accounts for the 85% of height for reactor.Arranging heat collector outside regenerator, heat collector height accounts for regenerator height 80%.
The reaction condition of reactor is: temperature is 480 DEG C, and in terms of gauge pressure, reaction pressure is 0.2 MPa, weight space velocity be 2 (gram / hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 12: 1, the catalysis of reaction zone in reactor Agent density is 80 kgs/m3, average gas superficial velocity 0.08 meter per second.Regenerator temperature is 650 DEG C.With methanol as raw material, Water content is 5 weight %.
Stripping fluid is water vapour.Lifting medium is steam.Regenerating medium is air.
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 appropriate Water, HCl, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make 60～300 purposes ZSM-5 catalyst intermediate.The mass ratio of ZSM-5 molecular sieve and substrate is 4:6；The silicoaluminophosphate molecular ratio of ZSM-5 molecular sieve It is 25；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 7:3.By Cu mass of ion percentage Content is the solution of 5%, impregnates with the weight ratio of solution and catalyst for 1.74:1, is 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 5 meters of the conversion zone of reactor, it highly accounts for the 60% of total reactor height, The diameter ratio of dilute phase section diameter and conversion zone is 1.1:1, and it highly accounts for the 35% of total reactor height.Arrange outside reactor Heat collector, heat collector height accounts for the 95% of height for reactor.Arranging heat collector outside regenerator, it is high that heat collector height accounts for regenerator The 30% of degree.
The reaction condition of reactor is: temperature is 400 DEG C, and in terms of gauge pressure, reaction pressure is 0.5 MPa, weight space velocity be 10 (gram / hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 3: 1, the catalyst of reaction zone in reactor Density is 50 kgs/m3, average gas superficial velocity 0.17 meter per second.The temperature of regenerator is 680 DEG C.With methanol as raw material, Water content is 30 weight %.
Stripping fluid is N2.Lifting medium is N2.Regenerating medium is air.
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 machinery Mixing, adds suitable quantity of water, HCl, controls pH value not less than 3, serosity stir after at 500 DEG C spray shaping, system Become 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 sieve mass ratio is 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.By Ag mass of ion percentage composition it is The solution of 1%, impregnates with solution and catalyst weight than for 0.1:1, is dried 5 hours, places into horse at 120 DEG C Not stove roasting at 550 DEG C is prepared as the Ag-Y-ZSM-23 catalyst that Ag constituent content is 0.1 weight % for 6 hours.
Reaction result is shown in Table 1.
[embodiment 3]
Use the device of embodiment 1.
The reaction condition of reactor is: temperature is 550 DEG C, and in terms of gauge pressure, reaction pressure is 0 MPa, weight space velocity be 10 (gram / hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 30: 1, the catalysis of reaction zone in reactor Agent density is 200 kgs/m3, average gas superficial velocity 1.2 meter per second.The temperature of regenerator is 580 DEG C.With methanol as raw material, Water content is 0.01 weight %.Arranging heat collector in reactor, heat collector height accounts for the 30% of height for reactor.In regenerator Arranging heat collector, heat collector height accounts for the 30% of regenerator height.
Stripping fluid is water vapour.Lifting medium is N2.Regenerating medium is air and O2Mixture, volume ratio is 8: 2.
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, Control pH value not less than 4, serosity stir after at 500 DEG C spray shaping, make in the beta catalyst of 60～300 mesh Mesosome.The mass ratio of beta-molecular sieve and substrate is 5:5；The silicoaluminophosphate molecular ratio of beta-molecular sieve is 20；Substrate is Kaolin, dioxy SiClx and the mixture of aluminium sesquioxide, the mass ratio of three is 7:1:2.By Ga mass of ion percentage composition be 2% molten Liquid, impregnates with solution and catalyst weight than for 0.4:1, at 120 DEG C be dried 5 hours, place into Muffle furnace in At 550 DEG C, roasting is prepared as the Ga-beta catalyst that Ga constituent content is 0.8 weight % for 6 hours.
Reaction result is shown in Table 1.
[embodiment 4]
Use device as shown in Figure 1.A diameter of 3 meters of the conversion zone of reactor, it highly accounts for the 70% of total reactor height, The diameter ratio of dilute phase section diameter and conversion zone is 1.4:1, and it highly accounts for the 25% of total reactor height.Arrange outside reactor Heat collector, heat collector height accounts for the 60% of height for reactor.Arranging heat collector outside regenerator, it is high that heat collector height accounts for regenerator The 70% of degree.
The reaction condition of reactor is: temperature is 470 DEG C, and in terms of gauge pressure, reaction pressure is 0.3 MPa, weight space velocity be 1 (gram / hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 25: 1, the catalysis of reaction zone in reactor Agent density is 80 kgs/m3, average gas superficial velocity 0.03 meter per second.The temperature of regenerator is 700 DEG C.It is former with dimethyl ether Material.
Stripping fluid is water vapour and N2Mixture, volume ratio is 5: 5.Lifting medium is N2.Regenerating medium is air And N2Mixture, volume ratio is 9: 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, adds suitable Amount water, HCl, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make 60～300 mesh ZSM-11 catalyst intermediate.The mass ratio of ZSM-11 molecular sieve and substrate is 3:7；The sial of ZSM-11 molecular sieve Molecular proportion is 50；Substrate is the mixture of Kaolin and aluminium sesquioxide, and both mass ratioes are 7:3.By Mn ion matter Amount percentage composition is the solution of 10%, impregnates with the weight ratio of solution and catalyst for 1:1, is dried 5 at 120 DEG C Hour, place into Muffle furnace roasting at 550 DEG C and within 6 hours, be prepared as the Mn-ZSM-11 that Mn constituent content is 9.09 weight % Catalyst.
Reaction result is shown in Table 1.
[embodiment 5]
Use the device of embodiment 4.
The reaction condition of reactor is: temperature is 465 DEG C, and in terms of gauge pressure, reaction pressure is 0.25 MPa, and weight space velocity is 0.3 (Grams Per Hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 10: 1, and in reactor, reaction zone urges Agent density is 130 kgs/m3, average gas superficial velocity 0.01 meter per second.The temperature of regenerator is 630 DEG C.It is former with methanol Material, water content is 10 weight %.
Stripping fluid is water vapour.Promoting medium is water vapour and N2Mixture, volume ratio is 1: 9.Regenerating medium is Air and O2Mixture, volume ratio is 9: 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 Amount water, H3PO4, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make 60～300 mesh P-ZSM-5 catalyst intermediate.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 kaolinite Soil and the mixture of aluminium sesquioxide, both mass ratioes are 7:3.It is the solution of 5% by Zn mass of ion percentage composition, with Solution and P-ZSM-5 catalyst weight impregnate than for 0.6:1, at 120 DEG C be dried 5 hours, place into Muffle furnace in Roasting 6 hours at 550 DEG C, being prepared as Zn constituent content is 2.87 weight %, and P element content is 1.48 weight % Zn-P-ZSM-5 catalyst.
Reaction result is shown in Table 1.
[embodiment 6]
Use device as shown in Figure 1.A diameter of 0.3 meter of the conversion zone of reactor, it highly accounts for the 85% of total reactor height, The diameter ratio of dilute phase section diameter and conversion zone is 2:1, and it highly accounts for the 10% of total reactor height.Arrange in reactor and take Hot device, heat collector height accounts for the 90% of height for reactor.Arranging heat collector outside regenerator, heat collector height accounts for regenerator height 50%.
The reaction condition of reactor is: temperature is 480 DEG C, and in terms of gauge pressure, reaction pressure is 0.1 MPa, weight space velocity be 2 (gram / hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 20: 1, the catalysis of reaction zone in reactor Agent density is double centner/rice3, average gas superficial velocity 0.12 meter per second.The temperature of regenerator is 600 DEG C.It is former with dimethyl ether Material.
Stripping fluid is water vapour and N2Mixture, volume ratio is 2: 8.Promoting medium is water vapour and N2Mixture, Volume ratio is 2: 8.Regenerating medium is air and O2Mixture, volume ratio is 5: 5.
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 60～300 Purpose ZSM-5-beta catalyst.The mass ratio of ZSM-5 and beta-molecular sieve and substrate is 3.5: 6.5.The silicon of ZSM-5 molecular sieve Aluminum molecular proportion 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, the mass ratio of three is 5:2:3.
Reaction result is shown in Table 1.
[embodiment 7]
Use device as shown in Figure 1.A diameter of 6 meters of the conversion zone of reactor, it highly accounts for the 65% of total reactor height, The diameter ratio of dilute phase section diameter and conversion zone is 1.1:1, and it highly accounts for the 30% of total reactor height.Arrange outside reactor Heat collector, heat collector height accounts for the 80% of height for reactor.Arranging heat collector outside regenerator, it is high that heat collector height accounts for regenerator The 40% of degree.
The reaction condition of reactor is: temperature is 450 DEG C, and in terms of gauge pressure, reaction pressure is 0.15 MPa, and weight space velocity is 0.8 (Grams Per Hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 6: 1, and in reactor, reaction zone urges Agent density is 70 kgs/m3, average gas superficial velocity 0.04 meter per second.With methanol, dimethyl ether mixture as raw material, two Person's mass ratio is 8:2.The temperature of regenerator is 720 DEG C.
Stripping fluid is water vapour.Promoting medium is water vapour and N2Mixture, volume ratio is 8: 2.Regenerating medium is Air and N2Mixture, volume ratio is 7: 3.
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 60～300 Purpose P-ZSM-5 catalyst intermediate.H3PO4The concentration of solution is that the weight ratio of 2.5 weight %, solution and molecular sieve is 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 Kaolin and the mixture of aluminium sesquioxide, both mass ratioes are 8:2.By Ag mass of ion percentage composition be 1%, Zn Mass of ion percentage composition is the solution of 3%, impregnates with solution and P-ZSM-5 catalyst weight than for 0.8:1, Being 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 weights Amount %, 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 2 meters of the conversion zone of reactor, it highly accounts for the 70% of total reactor height, The diameter ratio of dilute phase section diameter and conversion zone is 1.3:1, and it highly accounts for the 25% of total reactor height.Arrange outside reactor Heat collector, heat collector height accounts for the 90% of height for reactor.Arranging heat collector in regenerator, it is high that heat collector height accounts for regenerator The 80% of degree.
The reaction condition of reactor is: temperature is 460 DEG C, and in terms of gauge pressure, reaction pressure is 0.2 MPa, and weight space velocity is 0.5 (Grams Per Hour)/gram catalyst, the mass ratio of catalyst circulating load and feedstock amount is 30: 1, and in reactor, reaction zone urges Agent density is 120 kgs/m3, average gas superficial velocity 0.02 meter per second.The temperature of regenerator is 630 DEG C.It is former with methanol Material, water content is 0.01 weight %.
Stripping fluid is water vapour and N2Mixture, volume ratio is 8: 2.Promoting medium is water vapour and N2Mixture, Volume ratio is 5: 5.Regenerating medium is air and O2Mixture, volume ratio is 7: 3.
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, add Enter suitable quantity of water, H3PO4, control pH value not less than 3, serosity stir after at 500 DEG C spray shaping, make 60～300 Purpose P-ZSM-5 catalyst intermediate.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 be Kaolin and The mixture of aluminium sesquioxide, both mass ratioes are 7:3.By Mg mass of ion percentage composition be 2%, Zn mass of ion Percentage composition is the solution of 3%, impregnates with solution and P-ZSM-5 catalyst weight than for 1:1, is dried at 120 DEG C 5 hours, placing into Muffle furnace roasting 6 hours at 550 DEG C, being prepared as Zn constituent content is 2.86 weight %, Mg element 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 21.7 18.3 41.0
Embodiment 2 12.3 10.4 57.2
Embodiment 3 20.2 17.9 43.1
Embodiment 4 13.8 10.2 58.3
Embodiment 5 11.1 7.8 62.2
Embodiment 6 15.9 14.2 52.4
Embodiment 7 12.6 8.8 60.2
Embodiment 8 16.5 12.0 53.5

Claims (8)

1. methanol and/or a fluidized bed reaction system for dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, including Reactor (1), regenerator (2), stripper (3)；Reactor (1) be from bottom to top conversion zone (15), Changeover portion (16), dilute phase section (17)；Raw material (8) enters reactor reaction section (15) bottom and catalysis Agent haptoreaction, reacted carbon deposited catalyst is descending, the inclined tube to be generated that warp is connected with reactor (1) bottom (4) entering stripper (3), the catalyst after stripping is up through stripping inclined tube (5), stripping standpipe (6) Regenerating to regenerator (2), the catalyst after regeneration comes downwards to reactor reaction section (15) through regenerator sloped tube (7)；
Wherein, the height of reactor reaction section (15) accounts for the 60～85% of total reactor height；Dilute phase section (17) The diameter ratio of diameter and conversion zone (15) is 1.1～2:1, and it highly accounts for the 10～35% of total reactor height； Changeover portion (16) highly accounts for the 5% of total reactor height.
Methanol the most according to claim 1 and/or the fluidisation of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Bed response system, it is characterised in that reactor reaction section (15) bottom is anti-to inclined tube to be generated (4) and reactor The distance of the section of answering (15) junction is less than the 50% of reactor reaction section (15) overall length.
Methanol the most according to claim 1 and/or the fluidisation of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Bed response system, it is characterised in that reactor (1) interiorly or exteriorly arranges heat collector, and heat collector height accounts for instead Answer the 30%～95% of device height；Regenerator (2) interiorly or exteriorly arranges heat collector, and heat collector height accounts for regeneration The 30%～80% of device height.
Methanol the most according to claim 1 and/or the fluidisation of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Bed response system, it is characterised in that reactor (1), regenerator (2) and stripper (3) are internal to be equipped with 1～3 grade of gas-solid cyclone separator.
5. methanol and/or a fluidized bed reaction method for dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons, uses Any one response system described in Claims 1 to 4, described reaction method includes following step:
A) raw material (8) enters reactor reaction section (15) and catalyst haptoreaction, reaction of formation product (9) And carbon deposited catalyst, product (9) enters follow-up point after gas-solid cyclone separator separation carbon deposited catalyst From system；
B) inclined tube to be generated (4) that carbon deposited catalyst warp is connected with reactor (1) bottom enters stripper (3) Stripping is contacted, the stripped product (13) obtained with the stripping fluid (12) entered from stripper (3) bottom With the carbon deposited catalyst after stripping, stripped product (13) is laggard through gas-solid cyclone separator separation carbon deposited catalyst Enter subsequent separation system；
C) carbon deposited catalyst after stripping enters stripping standpipe (6), boosted medium through stripping inclined tube (5) (14) regenerator (2) it is promoted to；
D) carbon deposited catalyst after stripping neutralizes the regeneration entered from regenerator (2) bottom at regenerator (2) Medium (10) contact is burnt, the catalyst after being regenerated and flue gas (11)；
E) catalyst after regeneration is advanced into reactor reaction section (15) under regenerator sloped tube (7)；
The reaction temperature of reactor (1) is 400～550 DEG C, the weight space velocity of raw material (8) be 0.1～10 (gram/ Hour)/gram catalyst, in terms of gauge pressure, reaction pressure is 0～0.5 MPa, and catalyst circulating load and raw material (8) enter The mass ratio of doses is 3～40: 1, and density of catalyst is 50～200 kgs/m3, average gas superficial velocity 0.01～1 meter per second；The temperature of regenerator (2) is 580～720 DEG C, and the charcoal on catalyst after regeneration, to urge The mass percent of agent, content is less than 0.1 weight %.
Methanol the most according to claim 5 and/or the fluidisation of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Bed reaction method, it is characterised in that the active component of catalyst is that ZSM-5, ZSM-23, ZSM-11, β divide Son 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 be loaded with Zn, Ag, P, One or more elements or oxide in Ga, Cu, Mn, Mg, with the mass percent of catalyst, its Content is 0.01～15 weight %.
Methanol the most according to claim 5 and/or the fluidisation of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Bed reaction method, it is characterised in that raw material (8) is methanol or dimethyl ether or both mixture, the quality of water Percentage composition is 0.01～30 weight %.
Methanol the most according to claim 5 and/or the fluidisation of dimethyl ether conversion ethylene, propylene and aromatic hydrocarbons Bed reaction method, it is characterised in that stripping fluid (12) is water vapour or N2Or water vapour and N2Mixture, Promoting medium (14) 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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