CN102746873A - Method for preparing ethylene and propylene through catalytic cracking of light hydrocarbons - Google Patents
Method for preparing ethylene and propylene through catalytic cracking of light hydrocarbons Download PDFInfo
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Abstract
The invention relates to a method for preparing ethylene and propylene through the catalytic cracking of light hydrocarbons to mainly solve problems of difficult realization of the light hydrocarbon high temperature cracking, and low ethylene and propylene yields in the light carbon catalytic cracking process in the prior art. The method which allows the light hydrocarbon catalytic cracking to be carried out through a parallel type or coaxial type internal riser cycle reaction-regeneration device mainly comprises the following steps: 1, allowing a preheated light hydrocarbon raw material to enter an internal riser reactor, and reacting through contacting with a catalyst at 570-720DEG C to generate low carbon olefin-containing products and simultaneously form a carbon deposition catalyst; and 2, regenerating the carbon deposition catalyst through allowing it to enter a regenerator, and returning the regenerated catalyst to the riser reactor, wherein the active component of the catalyst is selected from at least one of a silicon-aluminum molecular sieve, an aluminum-phosphorous molecular sieve, a silicon-phosphorous-aluminum molecular sieve or a composite molecular sieve thereof, and the molecular sieve has a bore diameter of 0.4-0.65nm. The method well solves the problems through above technical scheme, and can be applied to the industrial production of ethylene and propylene.
Description
Technical field
The present invention relates to the method for a kind of lighter hydrocarbons catalytic pyrolysis preparing ethylene, propylene.
Background technology
Ethene, propylene are important basic organic synthesis raw materials, in recent years, receive the driving of downstream verivate demand, the market requirement sustainable growth of global ethene, propylene.At present, the production of ethene, propylene mainly relies on the steam heat cracking.The propylene of the ethene of about 90 weight % and 61 weight % is from the steam heat cracking process; Though this technology is used widely in the world, but still there is unsatisfactory part, especially reaction needed high temperature (800~1000 ℃); Energy consumption is big, and low value-added dry gas yield is high.If the introducing catalyzer adopts catalytic thermal cracking method, then can make temperature of reaction reduce by 50~200 ℃, reduce the generation of energy consumption and dry gas, and improve the propylene selectivity, so at present many investigators are devoted to catalytic pyrolysis preparing ethylene, propylene research.
Because the true boiling point boiling range is lower than 350 ℃ light hydrocarbon feedstocks; Like hybrid C 4, liquefied gas, catalytically cracked gasoline, solar oil, diesel oil, petroleum naphtha, hydrogenation tail oil etc.; Hydrogen richness higher; When carrying out catalytic pyrolysis, ethene, propylene selectivity are high, thereby the research of lighter hydrocarbons catalytic pyrolysis preparing ethylene, propylene causes concern more and more widely.
For the general conventional heavy oils fluidized catalyst cracked technology pattern of using for reference of the lighter hydrocarbons catalytic pyrolysis technology that adopts circulating fluid bed reactor, promptly reaction-regeneration system comprises a riser reactor, revivifier, settling vessel; Revivifier and riser reactor are separate, are side by side and arrange; Raw material gets into riser reactor, with the regenerated catalyst contact reacts, generates all kinds of products, forms reclaimable catalyst simultaneously; Reclaimable catalyst gets into coke-burning regeneration in the revivifier, and the catalyzer that regeneration is accomplished returns riser tube and participates in reaction.
Yet, compare with heavy oil, the hydrogen richness of lighter hydrocarbons is high, even pyroreaction, the green coke amount still seldom, coking yield is less than 1 weight %.The coke that generates when reaction institute heat requirement is by revivifier burning-off catalyst reaction in the ciculation fluidized bed process and providing; For RFCC; 5.1 the heat that the coking yield of weight % when regeneration produces can provide heavy oil 500 ℃ of required heats of reaction, the green coke amount of inferring the lighter hydrocarbons catalytic pyrolysis thus is difficult to the high temperature that guarantees that cracking is required.Therefore, there is more scabrous contradiction aspect the ciculation fluidized bed process of lighter hydrocarbons catalytic pyrolysis preparing ethylene, propylene, the heat undersupply few in needs pyroreaction and green coke amount.
For addressing this problem; Application number is that 200780029774.5 Chinese patent adds a spot of coke precursors in the lighter hydrocarbons charging; Promptly be easy to a kind of in the acetylene of coking, substituted acetylene, diolefine and the combination thereof; Riser temperature can reach 600~720 ℃, and the diene yield reaches 35.84 weight %.Though this method has improved the lighter hydrocarbons cracking temperature, the coke precursors that adds can influence reaction process, and the diene yield is low.
Also some method is coupled lighter hydrocarbons catalytic pyrolysis and RFCC.Application number is that 01808100.2 and 01808224.6 Chinese patent proposes light catalytic naphtha, catalytic cycle oil and water vapour are injected RFCC riser reactor top together; 620~775 ℃ of reactions down, propylene and butylene total recovery are brought up to 10.4 weight %.
Patent ZL200510089849.1 and ZL200510093782.9 adopt two riser reactors; Main riser tube carries out heavy oil catalytic cracking reaction; Isolate liquefied gas cracking propylene enhancing in subsidiary riser of propylene; Subsidiary riser has two reaction zones, carries out the reaction of building-up reactions and catalytic cracking and dehydrating alkanes successively.Temperature of reaction in the main riser tube is 450~650 ℃, and the temperature of subsidiary riser first reaction zone is 150~450 ℃, and the temperature of second reaction zone is 450~650 ℃, and propylene can reach 19.03 weight %.
This method can make the temperature of lighter hydrocarbons catalytic pyrolysis be higher than 600 ℃; And compare with RFCC and can improve propene yield to a certain extent; But because lighter hydrocarbons catalytic pyrolysis and RFCC are coupling in the circulating reaction device; The lighter hydrocarbons catalytic pyrolysis has to be limited by heavy oil catalytic cracking process aspect reaction conditions and the catalyst performance; Lighter hydrocarbons catalytic pyrolysis to greatest extent are ethene, propylene, thereby the yield of ethene, propylene is still lower, can not realize the purpose of lighter hydrocarbons High-efficient Production ethene, propylene.The present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is to exist in the prior art lighter hydrocarbons catalytic pyrolysis process to be difficult to realize the lighter hydrocarbons Pintsch process, and ethene, the problem that propene yield is low provide a kind of new lighter hydrocarbons catalytic pyrolysis preparing ethylene, the method for propylene.This method has the temperature of reaction height, ethene, the advantage that propene yield is high.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is following: the method for a kind of lighter hydrocarbons catalytic pyrolysis preparing ethylene, propylene; Adopt block form or the embedded riser tube circulating reaction-regenerating unit of coaxial-type to carry out the lighter hydrocarbons catalytic pyrolysis, mainly may further comprise the steps: the light hydrocarbon feedstocks after (1) preheating gets in the embedded riser reactor, 570~720 ℃ of following and catalyst I contact reactss; Generation contains the product of low-carbon alkene, forms carbon deposition catalyst II simultaneously; (2) carbon deposition catalyst II gets into revivifier regeneration, and the catalyzer after the regeneration returns riser reactor; Wherein the activity of such catalysts component is selected from sial, aluminium phosphorus, aluminium silicophosphate molecular sieve or its composite molecular screen that at least a aperture is 0.4~0.65 nanometer.
In the technique scheme, the main reaction region of embedded riser reactor is positioned at internal regenerator.The set a plurality of feed nozzles of embedded riser tube can advance different light hydrocarbon feedstocks respectively.
In the technique scheme, the average reaction temperature of each embedded riser reactor is 570~720 ℃, and reaction pressure is counted 0.1~0.35 MPa with gauge pressure, and catalystoil ratio is 6~40: 1, and catalyst in reactor density is 50~400 kilograms/meter
3, oil gas gets under the condition that reactor drum place LV is 1~8 meter per second and carries out lighter hydrocarbons catalytic pyrolysis preparing ethylene, propylene.
In the technique scheme, light hydrocarbon feedstocks is that boiling range is lower than 350 ℃ hydrocarbon mixture, preferred mixed C
4, liquefied gas, petroleum naphtha, catalytically cracked gasoline, catalytic cracking petroleum naphtha, solar oil, diesel oil, hydrogenation tail oil or these lighter hydrocarbons press different ratios blended mixture.The preheating temperature of light hydrocarbon feedstocks is 150~300 ℃.
In the technique scheme, the active ingredient of catalyst system therefor I comprises the composite molecular screen that forms each other between ZSM-5, ZSM-23, ZSM-11, Y/USY, β, SAPO-34, MOR or four, preferred ZSM-5 molecular sieve.The carrier of catalyst I is a porousness body material mixture, and porous matrix material comprises kaolin, aluminum oxide, silicon oxide, Natural manganese dioxide, preferred kaolin, aluminum oxide, silicon oxide.
In the technique scheme, the carbon deposition quantity of carbon deposition catalyst II is 0.3~8 weight %.
Product yield of the present invention is defined as the total raw material amount of the product amount of unit time generation divided by the unit time.Transformation efficiency is defined as (total raw material amount (ton/hour)-unconverted material quantity (ton/hour))/total raw material amount (ton/hour) * 100%.Catalystoil ratio (C/O) is the ratio of catalyst recirculation amount (ton/hour) and total raw material amount (ton/hour).Oil gas refers to the mixture of various hydrocarbon in the riser reactor.Carbon deposition quantity on the carbon deposition catalyst is defined as the quality percentage composition of carbon on the unit mass coked catalyst.
The inventor is through discovering, the ethene of lighter hydrocarbons catalytic pyrolysis and propene yield receive the influence of temperature of reaction obvious, and high temperature is favourable.For the FCC petroleum naphtha, adopt the ZSM-5 catalyzer, when temperature of reaction is elevated to 680 ℃ from 600 ℃, ethene and propylene gross weight yield have increased more than 10 percentage points.
Coke burning on the spent agent in the revivifier; Temperature is between 600 ℃~750 ℃ in the device; If riser reactor is placed internal regenerator, both utilized the hot environment of internal regenerator that reaction institute heat requirement is provided, reduce the calorific loss of riser reactor again; Can realize lighter hydrocarbons catalytic pyrolysis under high temperature more than 600 ℃ easily, thereby solve the problem of the circulating fluidized bed heat undersupply of the independent catalytic pyrolysis of lighter hydrocarbons.
Adopt technical scheme of the present invention can guarantee that average reaction temperature reaches 570~720 ℃ in the riser tube.Be raw material with the FCC petroleum naphtha, adopting the ZSM-5 sieve catalyst, temperature of reaction is 670 ℃, pressure 0.12 MPa, and catalystoil ratio is 30: 1 o'clock, and yield of ethene is 17.68 weight %, and propene yield is 23.03 weight %, has obtained better technical effect.
Description of drawings
Fig. 1 is the structural representation of the embedded riser tube circulating reaction-regenerating unit of block form according to the invention.
Among Fig. 1,1 is embedded riser reactor; 2 is revivifier; 3 is settling vessel; 4 is stripping stage; 5 is regenerator sloped tube; 6 are the regeneration guiding valve; 7 is plug valve to be generated; 8 is the settling vessel internal cyclone separators; 9 is air-distributor; 10 is nozzle; 11 is lighter hydrocarbons, light oil raw material; 12 is splitting gas; 13 for promoting medium; 14 is regeneration air; 15 is the fuel oil gas nozzle; 16 is exhanst gas outlet; 18 is the reclaimable catalyst transfer lime; 19 is the revivifier internal cyclone separators; 20 are the gas-solid quick disconnector.
Fig. 2 is the structural representation of the embedded riser tube circulating reaction-regenerating unit of coaxial-type according to the invention.
Among Fig. 2,21 is embedded riser reactor, and 22 is revivifier, and 23 is settling vessel, and 24 is stripping stage; 25 is regenerator sloped tube, and 26 are the regeneration guiding valve, and 28 is the settling vessel internal cyclone separators, and 29 is air-distributor, and 30 is nozzle; 31 is lighter hydrocarbons, light oil raw material, and 32 is splitting gas, and 33 for promoting medium, and 34 is regeneration air, and 35 is the fuel oil gas nozzle; 36 is exhanst gas outlet, and 37 is guiding valve to be generated, and 38 is inclined tube to be generated, and 39 is the revivifier internal cyclone separators, and 40 are the gas-solid quick disconnector.
Through embodiment the present invention is done further elaboration below, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
On device shown in Figure 1, carried out 4 groups of experiments, reaction raw materials, catalyzer, reaction conditions and result are as shown in table 1.
The content of butylene is 73.8 weight % in the hybrid C 4, and normal butane content is 26.2 weight %; Petroleum naphtha is mainly C
5~C
8Alkane, content are respectively 12.62 weight %, 25.54 weight %, 25.25 weight %, 17.86 weight %; Catalytic cracking petroleum naphtha (FCC petroleum naphtha) is mainly amylene, hexene, and content is respectively 36.4 weight % and 34.1 weight %.
Test used catalyzer and adopt semi-synthesis method to be prepared from,, add suitable quantity of water, HCl and H promptly earlier with molecular sieve, carrier and sticker mechanically mixing
3PO
4(preparation SAPO-34 does not add during catalyzer), the control pH value is not less than 3, and slurries stir the back in 500 ℃ of following spray shapings.In the used ZSM-5 catalyzer, the mass ratio of HZSM-5 molecular sieve and matrix is 3: 6.8, P
2O
5Content is 2 weight %; The silica alumina ratio of HZSM-5 molecular sieve is 38; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 2: 8.In the used ZSM-5+ beta catalyst, the mass ratio of ZSM-5+ beta-molecular sieve and matrix is 3: 7; The silica alumina ratio of ZSM-5 molecular sieve is 25; The silica alumina ratio of beta-molecular sieve is 20; The mass ratio of ZSM-5 and beta-molecular sieve is 7: 3; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 1: 9.In the used SAPO-34 catalyzer, the mass ratio of HSAPO-34 molecular sieve and matrix is 3.5: 6.5; The phosphorus al mole ratio of HSAPO-34 molecular sieve is 0.9, and silica alumina ratio is 1.2; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 1: 9.
Table 1
[comparative example 1]
Do not use the embedded riser tube among Fig. 1, utilize the external riser tube of the conventional flow fluidized catalytic cracking unit of same size to carry out 3 groups of contrast experiments.Reaction raw materials, catalyzer, reaction conditions and result are as shown in table 2.Raw materials used composition and catalyst preparation process are seen embodiment 1.
Table 2
[embodiment 2]
Adopt and embodiment 1 essentially identical embedded riser arrangement; But two feed nozzles are set on the embedded riser tube; Two nozzles advance hybrid C 4 and FCC petroleum naphtha from bottom to top respectively at a distance of 0.3 meter, and reaction raw materials, reaction conditions, catalyzer and reaction result are as shown in table 3.Raw materials used composition and catalyst preparation process are seen embodiment 1.
Table 3
[embodiment 3~7]
On device shown in Figure 2, carried out 5 groups of experiments, reaction raw materials, reaction conditions, catalyzer and reaction result are as shown in table 4.Raw materials used composition and catalyst preparation process are seen embodiment 1.
Propane content is 7.5 weight % in the liquefied gas, and propylene content is 2.5 weight %, and butene content is 33.8 weight %, and butane content is 56.2 weight %.The density of solar oil is 0.72 gram per centimeter
3, H content is 15.2 weight %, and the content of saturated branch is 91.37 weight %, and the content that fragrance divides is 8.63 weight %.The density of diesel oil is 0.78 gram per centimeter
3, H content is 14.7 weight %, and saturated minute content is 89.29 weight %, and it is 10.71 weight % that fragrance divides content.Catalytically cracked gasoline (FCC gasoline) is mainly C
5~C
10Hydro carbons, alkene, alkane, naphthenic hydrocarbon, aromaticity content are 36.4 weight %, 34.1 weight %.
The Preparation of catalysts method is with embodiment 1.Mixture with the MOR molecular sieve is the catalyzer of active ingredient, and the mass ratio of its molecular sieve and matrix is 3: 7; The sial molecular ratio of MOR molecular sieve is 10; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 8: 2.Mixture with beta-molecular sieve is the catalyzer of active ingredient, and the mass ratio of its molecular sieve and matrix is 3.5: 6.5; The sial molecular ratio of beta-molecular sieve is 20; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 7: 3.Mixture with Y molecular sieve is the catalyzer of active ingredient, and the mass ratio of its molecular sieve and matrix is 2.5: 7.5; The sial molecular ratio of Y molecular sieve is 6; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 7: 3.Mixture with the ZSM-23 molecular sieve is the catalyzer of active ingredient, and the mass ratio of its molecular sieve and matrix is 3: 7; The sial molecular ratio of ZSM-23 molecular sieve is 60; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 7: 3.Mixture with the ZSM-11 molecular sieve is the catalyzer of active ingredient, and the mass ratio of its molecular sieve and matrix is 3.2: 68, and the sial molecular ratio of ZSM-11 molecular sieve is 50; Matrix is the mixture of kaolin and aluminium sesquioxide, and both mass ratioes are 7: 3.
Table 4
Claims (9)
1. the method for a lighter hydrocarbons catalytic pyrolysis preparing ethylene, propylene; Adopt block form or the embedded riser tube circulating reaction-regenerating unit of coaxial-type to carry out the lighter hydrocarbons catalytic pyrolysis; Mainly may further comprise the steps: the light hydrocarbon feedstocks after (1) preheating gets in the embedded riser reactor; 570~720 ℃ of following and catalyst I contact reactss, generate the product that contains low-carbon alkene, form carbon deposition catalyst II simultaneously; (2) carbon deposition catalyst II gets into revivifier regeneration, and the catalyzer after the regeneration returns riser reactor; Wherein the active ingredient of catalyst I is selected from sial, aluminium phosphorus, aluminium silicophosphate molecular sieve or its composite molecular screen that at least a aperture is 0.4~0.65 nanometer.
2. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene is characterized in that the main reaction region of embedded riser reactor is positioned at internal regenerator.
3. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene is characterized in that the set a plurality of feed nozzles of embedded riser tube can advance different light hydrocarbon feedstocks respectively.
4. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene; The average reaction temperature that it is characterized in that each embedded riser reactor is 570~720 ℃; Reaction pressure is counted 0.1~0.35 MPa with gauge pressure; Catalystoil ratio is 6~40: 1, and catalyst in reactor density is 50~400 kilograms/meter
3, it is 1~8 meter per second that oil gas gets into reactor drum place LV.
5. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene is characterized in that light hydrocarbon feedstocks is that boiling range is lower than 350 ℃ hydrocarbon mixture.
6. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene, the preheating temperature that it is characterized in that light hydrocarbon feedstocks is 150~300 ℃.
7. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene is characterized in that the used active ingredient of catalyst I comprises ZSM-5, ZSM-23, ZSM-11, Y/USY, β, SAPO-34, MOR or the composite molecular screen that forms each other.
8. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene, the carrier that it is characterized in that catalyst I is a porousness body material mixture, porous matrix material comprises kaolin, aluminum oxide, silicon oxide, Natural manganese dioxide.
9. the method for lighter hydrocarbons catalytic pyrolysis preparing ethylene according to claim 1, propylene, the carbon deposition quantity that it is characterized in that carbon deposition catalyst II are 0.3~8 weight %.
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Cited By (5)
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CN104418685A (en) * | 2013-08-30 | 2015-03-18 | 中国石油化工股份有限公司 | Catalytic conversion method for producing ethylene and propylene |
CN107879876A (en) * | 2016-09-30 | 2018-04-06 | 中国石油化工股份有限公司 | A kind of method and apparatus of light hydrocarbon feedstocks production ethene and propylene |
CN115624987A (en) * | 2022-09-07 | 2023-01-20 | 山东京博石油化工有限公司 | Preparation method and application of catalyst for preparing low-carbon olefin by catalytic cracking of straight-run diesel oil |
CN115888797A (en) * | 2022-11-08 | 2023-04-04 | 洛阳市科创石化科技开发有限公司 | Catalyst for preparing ethylene and propylene by cracking of C, V and C-hexaalkane and preparation method and application thereof |
CN116371454A (en) * | 2023-04-07 | 2023-07-04 | 山东京博石油化工有限公司 | Preparation method and application of light hydrocarbon cracking catalyst |
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Cited By (6)
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CN104418685A (en) * | 2013-08-30 | 2015-03-18 | 中国石油化工股份有限公司 | Catalytic conversion method for producing ethylene and propylene |
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CN107879876B (en) * | 2016-09-30 | 2020-07-24 | 中国石油化工股份有限公司 | Method and device for producing ethylene and propylene from light hydrocarbon raw material |
CN115624987A (en) * | 2022-09-07 | 2023-01-20 | 山东京博石油化工有限公司 | Preparation method and application of catalyst for preparing low-carbon olefin by catalytic cracking of straight-run diesel oil |
CN115888797A (en) * | 2022-11-08 | 2023-04-04 | 洛阳市科创石化科技开发有限公司 | Catalyst for preparing ethylene and propylene by cracking of C, V and C-hexaalkane and preparation method and application thereof |
CN116371454A (en) * | 2023-04-07 | 2023-07-04 | 山东京博石油化工有限公司 | Preparation method and application of light hydrocarbon cracking catalyst |
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