CN103509595B - A kind of Light hydrocarbon oil catalytic conversion method - Google Patents
A kind of Light hydrocarbon oil catalytic conversion method Download PDFInfo
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- CN103509595B CN103509595B CN201210216139.0A CN201210216139A CN103509595B CN 103509595 B CN103509595 B CN 103509595B CN 201210216139 A CN201210216139 A CN 201210216139A CN 103509595 B CN103509595 B CN 103509595B
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Abstract
A kind of Light hydrocarbon oil catalytic conversion method, light hydrocarbon oil raw material enters in the riser reactor of cat-cracker and reacts with catalyst exposure, react rear reaction oil gas to be separated with reclaimable catalyst, be separated further and obtain ethene, propylene, C2 ~ C3 alkane, C4 hydrocarbon-fraction and other products; Reclaimable catalyst coke burning regeneration Posterior circle uses; Described cat-cracker comprise revivifier (2), riser reactor (1), riser reactor (1) outlet outside seal bootr (3) and cyclonic separator (5); The outlet of described riser reactor outlet through seal bootr (3) top is communicated with the entrance of cyclonic separator (5), and the bottom dipleg of cyclonic separator (5) is communicated with seal bootr (3); Described seal bootr (3) bottom is communicated with revivifier (2) through inclined tube to be generated (9).Method provided by the invention reduces the heat radiation total surface area of reaction-regeneration system, decreases the radiation energy consumption of reactor, solves the shortage of heat problem that light hydrocarbon oil cracking green coke deficiency is brought.
Description
Technical field
The present invention relates to a kind of catalysis conversion method not depositing hydrocarbon ils in the context of hydrogen, more particularly, relate to a kind of method of light hydrocarbon oil producing light olefins through catalytic conversion.
Background technology
Ethene is one of most important basic material of petrochemical industry, by vinyl polymerization, with the alkylation of benzene and the addition reaction with water, oxygen, halogen, a series of extremely valuable derivative can be obtained.World Ethylene Industry continues the situation that remain stable development.At present, the ethene of about 98% comes from tube furnace steam cracking technology in the world, and in ethylene production raw material, petroleum naphtha accounts for 46%, and ethane accounts for 34%.
Propylene is one of most important alkene, and consumption is only second to ethene.The derivative of propylene research on maximum utilized quantity is polypropylene, accounts for 61% of global propylene consumption.2005, about 62% propylene in the whole world was from the coproduction of preparing ethylene by steam cracking, and 34% propylene, from refinery catalytic cracking device by-product, also has 4% propylene from dehydrogenating propane and Ethylene/Butylene metathesis reaction.
At present, steam cracking technology becomes better and approaching perfection day by day, and is the process consuming the energy in a large number, is used again and the limitation of high temperature material, and the potentiality improved further are very little.The output of the ethene that hydrocarbon vapours cracking is produced and propylene is very large, and the raising of small yield and the saving of small raw material and the energy all will bring considerable economic benefit.In order to improve the selectivity of cracking process alkene, reduce scission reaction temperature, the yield of further increase ethene and propylene, by improving the diversity of raw material, develop multiple new ethylene, as preparing low-carbon olefin by catalytically cracking technology, methane oxidation coupling technology, oxidative dehydrogenation of ethane technology, natural gas via methyl alcohol or dimethyl ether alkene technology etc., wherein producing olefin hydrocarbon by catalytic pyrolysis technology is compared with steam cracking technology, have and can reduce cracking temperature, improve ethene and propene yield and scission reaction selectivity, save the advantage of energy, thus become the technology of very attractive.
CN1566272A discloses a kind of method utilizing light petroleum fraction catalyzed conversion to produce ethene and propylene, is that the light petroleum fraction being rich in alkene is contacted with the five-ring high silica zeolite catalyst of heat and reacted under catalyticing conversioning condition in main reaction region; Reaction product isolated and reclaimable catalyst; Reaction product is separated into further after being drawn by main reaction region and is rich in ethene, below the C4 cut of propylene and C4 and more than C4 cut; Reclaimable catalyst enters revivifier after stripping, coke burning regeneration under oxygen-containing gas exists; The regenerated catalyst of heat is introduced in pre-reaction zone, and contact with above-mentioned C4 and more than the C4 cut from main reaction region, react, the oil agent mixture generated returns to main reaction region and recycles.
CN1958731A discloses a kind of catalytic thermal cracking process to prepare lower olefine method.This invention will comprise the cracking petroleum hydrocarbon raw material of petroleum naphtha, solar oil and hydrogenation tail oil, by the beds of connect up and down two filling different catalysts a and b, carry out catalytic cracking reaction, will obtain olefine in low carbon number.Preferred employing double-reactor, dual catalyst bed technique, by two sections of fixed-bed reactor series connection; Or adopt single reactor, dual catalyst bed technique, in same fixed-bed reactor, load two beds.The method of this invention can improve the transformation efficiency of raw material, and improves the selectivity of reaction, increases the yield of object product (ethene and propylene).
CN101228104A proposes a kind of method improving the productive rate of light olefin in hydrocarbon feed catalytic cracking reaction.In the method, employ a kind of separating technology structure and circulation means of effective light olefin, the ethene low by circulation added value and propylene vapor cracking unit, to circulate C in most economical mode
4~ C
5cut, and control C neatly
6+cut is circulated to the feed entrance point of catalytic cracking unit, can effectively improve ethene and productivity of propylene.Take petroleum naphtha as raw material, the massfraction 85.5% of its paraffin, temperature of reaction 675 DEG C, HXSM-5 catalyzer, one way ethene and productivity of propylene are respectively 20.71% and 22.06%, if by C2 ~ C3 alkane and C4 ~ C 5 fraction circulation, by adding and calculating, ethene can be obtained and productivity of propylene is respectively 34.7% and 24.6%.
CN101279881A discloses a kind of method that catalytic pyrolysis petroleum naphtha produces ethene and propylene, this invention is by adopting with the petroleum naphtha of C4 ~ C10 hydrocarbon composition as raw material, after raw material hydrocarbon vaporization, first mix with rare gas element, wherein the mol ratio of rare gas element and petroleum naphtha is greater than 0 ~ 5.0: 1, be 580 ~ 750 DEG C in temperature of reaction, reaction pressure (in gauge pressure) is greater than 0 ~ 0.5MPa, weight space velocity 0.5 ~ 3h
-1under the condition of water/petroleum naphtha weight ratio 0 ~ 5: 1, material mixed gas and catalyst exposure react and generate ethene and propylene, wherein used catalyst is selected from the technical scheme of at least one in ZSM-5/ mercerization zeolite symbiosis molecular screen, ZSM-5/ beta zeolite coexisting molecular sieve or ZSM-5/Y zeolite coexisting molecular sieve, mainly solves the problem that life-span is shorter, palpus consumes a large amount of water vapour that naphtha catalytic pyrolysis preparing ethylene propylene reacting middle catalyst causes because of coking.
CN102040438A discloses a kind of riser tube reaction-regenerative device, is intended to solve in existing lighter hydrocarbons, naphtha catalytic cracking process, when adopting riser reactor to carry out circulating reaction regeneration, is difficult to the problem realizing pyroreaction.The main reaction region that this invention have employed riser reactor is positioned at internal regenerator and settling vessel, stripping stage and riser reactor are positioned at the technical scheme on same axis, with hybrid C 4 and FCC petroleum naphtha for raw material, temperature of reaction 630 DEG C, ZSM-5 catalyzer, 3.7 seconds residence time, agent oil quality is than under 22 conditions, and ethene and productivity of propylene are respectively 11.34% and 33.40%.
CN102295510A proposes a kind of method that Naphtha is converted into low-carbon alkene, this invention is in Conventional catalytic cracking technical foundation, have employed the structural shape of riser reactor beds connected in series reactor, a carbon deposited catalyst part after stripping is returned convert naphtha reactor epimere, a part enters revivifier regeneration, and the catalyzer after regeneration enters convert naphtha reactor hypomere; The bed reactor of employing series connection ensure that the gas-solid contact time needed for Naphtha Pyrolysis Reaction, and carbon deposited catalyst returns more than the C4 hydrocarbon mixture of riser tube epimere catalyzed conversion freshening, further increases yield of light olefins.The massfraction 93.5% of stable hydrocarbon in petroleum naphtha, adopt ZSM-5 catalyzer, temperature of reaction 675 DEG C, water oil quality is than 10:1, and low-carbon alkene total recovery is about 43.52%.
Because the cracking reaction transformation efficiency of Deep Catalytic Cracking process is high, temperature of reaction is high, cracking reaction heat is large, and the heat needed in reaction is more Conventional catalytic cracking or other catalysis conversion method is many, and the coke that self cracking generates often can not meet the thermally equilibrated demand of reaction-regeneration system self.Above-mentioned prior art proposes the method and the catalyzer that by catalytic cracking reaction process, petroleum hydrocarbon are converted into low-carbon alkene, but fails to solve the problem of reaction heat deficiency in light hydrocarbon oil cracking process.In addition, prior art is all being conventional catalyst cracking process-technology-evolutions, and the main device of typical catalytic cracking reaction-regeneration system comprises riser reactor, settling vessel and revivifier.The oil agent mixture leaving riser reactor enters settling vessel after initial gross separation, the existence of settling vessel large space is difficult to realize the sharp separation of oil gas and catalyzer and the quick extraction of oil gas, cause the low-carbon alkene generation secondary reaction generated, decrease productivity of low carbon olefin hydrocarbon, therefore, reduce the unnecessary space in catalytic cracking unit settling vessel, and even cancel settling vessel, develop most important to catalytic cracking increased low carbon olefine output without the catalytic cracking process technology of settling vessel.
Summary of the invention
The object of this invention is to provide and a kind ofly save energy consumption, light hydrocarbon oil producing low-carbon alkene by catalytically cracking that selectivity is good, i.e. the method for ethene and propylene.
A kind of Light hydrocarbon oil catalytic conversion method, comprise: light hydrocarbon oil raw material enters bottom the riser reactor of cat-cracker, contact with regenerated catalyst while of carrying out catalytic cracking reaction and upwards flow, the reaction oil gas of riser reactor outlet and reclaimable catalyst gas solid separation, isolated reaction oil gas caterpillar, is separated further and obtains ethene, propylene, C2 ~ C3 alkane, C4 hydrocarbon-fraction and other products; Isolated reclaimable catalyst enters coke burning regeneration in revivifier, recycles in the regenerated catalyst Returning reactor of activity recovery; Described cat-cracker comprises revivifier 2, runs through the riser reactor 1 of revivifier 2, riser reactor 1 export outside seal bootr 3 and cyclonic separator 5; The outlet of described riser reactor outlet through seal bootr 3 top is communicated with the entrance of cyclonic separator 5, and the bottom dipleg of cyclonic separator 5 is communicated with seal bootr; The catalyst outlet of described seal bootr 3 bottom is communicated with revivifier 2 through inclined tube 9 to be generated.
In method provided by the invention, the gaseous phase outlet of described cyclonic separator is communicated with large oil gas collection pipeline 24 through effuser 7; The bottom of described riser reactor 1 is stretched out outside revivifier 2, and the hydrocarbon oil crude material entrance bottom riser reactor and catalyst inlet are positioned at outside revivifier 2.
Preferably, described riser reactor 1 exports and connects gas-solid quick disconnector 4.Described gas-solid quick disconnector 4 has tangential opening, and gas-solid quick disconnector 4 is positioned at seal bootr 3.The oil agent mixture of riser reactor outlet is after the tangential opening ejection of gas-solid quick disconnector 4, stronger rotational flow field is formed in seal bootr space, realize the sharp separation of gas-solid, catalyzer falls into rapidly in seal bootr 3, and the outlet pipe of reaction oil gas through seal bootr top, airway 6 directly enter in cyclonic separator 5.
Described cyclonic separator 5 is the cyclonic separator of single-stage or plural serial stage, and preferably, described cyclonic separator 5 is the cyclonic separator of more than two-stage, and every grade is the cyclonic separator of one or more parallel connection.
Preferably, the bottom dipleg 8 of described cyclonic separator 5 is multiple, and part or all of dipleg wherein stretches in described seal bootr 3, and the catalyst outlet of described cyclonic separator 5 is in described seal bootr 3.
Preferably, bottom described seal bootr 3 and reclaimable catalyst inclined tube 9 is set between revivifier.Described reclaimable catalyst inclined tube entrance is communicated with bottom seal bootr, the outlet revivifier of reclaimable catalyst inclined tube.
Preferably, described reclaimable catalyst inclined tube 9 pipeline also arranges guiding valve 10 to be generated.Described guiding valve to be generated 10 is arranged in the pipeline of inclined tube 9 to be generated, for controlling the material level of catalyzer in described seal bootr.
Preferably, in the pipeline of described inclined tube 9 to be generated, fuel inlet is set, such as fuel oil gas nozzle, oil fuel and/or fuel gas is sprayed in reclaimable catalyst inclined tube 9, enter after fully mixing with reclaimable catalyst in revivifier 2.
Preferably, the regenerated catalyst outlet of described revivifier 2 is connected with bottom riser reactor 1 by regenerator sloped tube 16.
Preferably, described revivifier 2 also comprises regenerated catalyst degassing vessel 15, described regenerated catalyst degassing vessel 15 comprises regenerated catalyst inlet, regenerated catalyst outlet and pneumatic outlet, the regenerated catalyst inlet of described degassing vessel 15 is connected by the regenerated catalyst outlet of inclined tube 14 with revivifier 2, the regenerated catalyst outlet of described degassing vessel 15 is connected with riser reactor 1 by reclaimable catalyst inclined tube 16, and the pneumatic outlet of described degassing vessel 4 is connected with revivifier 2 by pipeline 13.
Preferably, described device also comprises the cyclonic separator 11 for separating of flue gas be arranged in revivifier 2.
Preferably, described riser reactor 1, revivifier 2 and seal bootr 3 are coaxial.
In method provided by the invention, the operational condition of described riser reactor is: temperature of reaction is 500 ~ 750 DEG C, preferably 540 ~ 720 DEG C, more preferably 560 ~ 700 DEG C, reaction times is 1 ~ 10 second, preferably 2 ~ 6 seconds, more preferably 2 ~ 4 seconds, apparent pressure is 0.05 ~ 1.0MPa, and agent-oil ratio is 1 ~ 100, preferably 10 ~ 50, more preferably 20 ~ 40.
The operational condition of described revivifier is: regeneration temperature is 550 ~ 750 DEG C, and fluidized bed gas apparent linear velocity is 0.8 ~ 3.0 meter per second, and catalyzer mean residence time is 0.6 ~ 2.0 minute.
Preferably, the C4 hydrocarbon-fraction described in reaction product is returned in riser reactor and continue reaction.
Preferably, the described C4 hydrocarbon-fraction returning riser reactor introduces reactor after described light hydrocarbon oil feedstock position.
In method provided by the invention, with the total weight of catalyzer, described catalyzer contains: the heavy % of the heavy % of zeolite 1 ~ 60, the heavy % of inorganic oxide 5 ~ 99 and clay 0 ~ 70, its mesolite is selected from mesopore zeolite and optional large pore zeolite, mesopore zeolite accounts for 50 ~ 100 heavy % of zeolite gross weight, and large pore zeolite accounts for 0 ~ 50 heavy % of zeolite gross weight.
Preferably, described mesopore zeolite accounts for 70 ~ 100 heavy % of zeolite gross weight, and large pore zeolite accounts for 0 ~ 30 heavy % of zeolite gross weight.
In method provided by the invention, described light hydrocarbon oil raw material to be boiling range the be hydrocarbon-fraction of 25-204 DEG C.
The beneficial effect of light hydrocarbon oil catalyzed conversion production method provided by the invention is:
Method provided by the invention have employed riser reactor and to be placed in catalyst regenerator and the structure running through revivifier, and meanwhile, riser reactor outlet does not arrange settling vessel and stripper.Reduce device radiation total surface area, decrease the radiation energy consumption of catalytic cracking unit; Built-in riser reactor also can obtain heat from revivifier, solve the not enough and thermal balance question that brings of low-density oil hydrocarbon cracking green coke, reaction oil gas directly carries out gas solid separation through cyclonic separator, quick derivation oil gas, avoid due to catalyzer and the long and non-selective reaction caused reaction product duration of contact, improve productivity of low carbon olefin hydrocarbon, wherein ethylene yield can reach 27.64 heavy %, and productivity of propylene reaches 27.97 heavy %.
In a preferred approach fuel inlet is set on inclined tube pipeline to be generated, in use, reclaimable catalyst fully mixes with oil fuel before entering revivifier, be not only the more heat of reaction zone, it also avoid oil fuel simultaneously and directly spray into catalyzer dense-phase bed and the hot localised points problem brought, alleviate the infringement of high temperature to catalyzer.
In sum, adopt the refinery of catalytic cracker for petroleum hydrocarbon provided by the invention can produce ethene, propylene to greatest extent from light petroleum hydrocarbon, thus realize the technological breakthrough of refinery's concept, change from traditional fuel type and fuel-Lube Type refinery production model to chemical industry type, make refinery from single oil refining to industrial chemicals production development and extension, both solve the problem of petrochemical material shortage, turn improve the economic benefit of refinery.
Accompanying drawing explanation
Accompanying drawing is the schematic flow sheet of a kind of preferred implementation of the method for light hydrocarbon oil producing light olefins through catalytic conversion provided by the invention.
Description of reference numerals:
1-riser reactor; 2-revivifier; 3-seal bootr;
4-(riser reactor 1 exit end) gas-solid quick disconnector;
5-cyclonic separator; 6-airway;
7-(is communicated with the pneumatic outlet of cyclonic separator 5 and main oil gas piping) effuser;
The bottom dipleg of 8-cyclonic separator; 9-reclaimable catalyst inclined tube
10-guiding valve to be generated; 11-revivifier cyclonic separator;
12-(is communicated with cyclonic separator 11 pneumatic outlet) flue;
13-(is communicated with degassing vessel 15 pneumatic outlet and revivifier 2) pipeline;
14-(is communicated with catalyst outlet and the degassing vessel 4 of described revivifier 2) pipeline;
15-degassing vessel;
16-(is communicated with regenerated catalyst outlet and the riser reactor 1 of degassing vessel 15) pipeline;
17-regenerates guiding valve; 18-(revivifier 2) main air source line;
19-air distributor;
20-is the pipeline of riser reactor 1 transferring raw material;
21-is the pipeline of riser reactor 1 delivery of mist steam transferring raw material;
22-is the pipeline that pre-lift medium carried by riser reactor 1;
23-is that the pipeline loosening wind carried by seal bootr 3;
24-main oil gas piping
The pipeline of 25-transfer the fuel oil dispersion medium
26-(is connected with inclined tube to be generated) oil fuel (or gas) pipeline.
Embodiment
Below illustrate the embodiment of method provided by the invention, but the present invention is not therefore subject to any restriction: below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The regenerated catalyst being rich in mesopore zeolite enters the pre lift zone of riser reactor, upwards flow under the effect of pre-lift medium, light hydrocarbon oil raw material is after preheating, injecting lift pipe reactor bottom together with atomizing steam, contacts with regenerated catalyst while of carrying out catalytic cracking reaction and upwards flows; After reaction, logistics enters in seal bootr 3 through riser reactor outlet, airway 6 through seal bootr 3 top enters cyclonic separator 5 and carries out gas solid separation, isolated reaction oil gas caterpillar, is separated further obtains ethene, propylene, C2 ~ C3 alkane, C4 hydrocarbon-fraction, gasoline fraction and diesel oil distillate with after the heat exchange of lightweight material oil; The reclaimable catalyst of isolated band charcoal directly enters in seal bootr 3, reclaimable catalyst bottom described seal bootr 3 enters in revivifier through inclined tube 9 to be generated, contact coke burning regeneration with oxygen, the regenerated catalyst of activity recovery returns in riser reactor and recycles.
In method provided by the invention, described cat-cracker comprises revivifier 2, runs through the riser reactor 1 of revivifier, riser reactor exports outside seal bootr 3 and cyclonic separator 5; Described riser reactor 1 stretches in revivifier 2 from the bottom of revivifier 2, until in seal bootr 3 above revivifier 2, and the reacting material outlet of described riser reactor 1 is connected with the material inlet of cyclonic separator 5 through seal bootr top exit, airway 6, reclaimable catalyst outlet bottom described seal bootr 3 is communicated with regenerator bottoms through inclined tube 9 to be generated, and described inclined tube 9 to be generated is positioned at revivifier outside.
The gaseous phase outlet of described cyclonic separator can be communicated with subsequent separation system through effuser 7, and cyclonic separator solid-phase outlet, without stripping stage, is directly communicated with catalyst regenerator inside through seal bootr, inclined tube to be generated.
In method provided by the invention, the bottom dipleg 8 of described cyclonic separator 5 stretches at least partially in described seal bootr 3 and (catalyst outlet of described bottom dipleg 8 is in described seal bootr 3), and the catalyzer separated from cyclonic separator is returned seal bootr 3.The catalyst inlet of the bottom dipleg 8 of preferred described cyclonic separator 5 is positioned at seal bootr 3 top.
The regenerated catalyst outlet of described revivifier 2 is connected with bottom riser reactor 1 by regenerator sloped tube 16, preferred regenerator sloped tube 16 is arranged regeneration guiding valve 17, the catalyzer after regeneration is returned to the bottom of riser reactor 1 through regeneration guiding valve 17.
In method provided by the invention, on preferred described inclined tube 9 to be generated, guiding valve 10 to be generated is also set, regulates the aperture of guiding valve to be generated to can be used for controlling the material level of catalyzer in seal bootr 3.
In method provided by the invention, preferably, setting-fuel oil gas nozzle in the pipeline of described inclined tube to be generated 9, sprays in reclaimable catalyst inclined tube 9 using the oil fuel introduced through oil fuel line of pipes 26 with as the high-temperature flue gas introduced through line of pipes 25 of dispersion medium.
In method provided by the invention, described riser reactor 1 runs through revivifier 2, is preferably all in revivifier 2, to reduce heat radiation as far as possible from the part that the catalyst inlet of riser tube is later.The catalytic cracking riser reactor of the routine that described riser reactor can be known to the skilled person, such as, described riser tube can be selected from equal diameter riser reactor, etc. one or more in linear speed riser reactor and various variable diameters riser reactor, preferred equal diameter riser tube.Under preferable case, described riser reactor 1 comprises pre lift zone and at least one reaction zone from bottom to top successively, fully react to enable stock oil, and according to different needs (such as reducing the requirement of benzene content in stock oil), described reaction zone can be 2-8, is preferably 2-3.
In method provided by the invention, described riser reactor 1 runs through revivifier 2, the top of riser reactor 1 is positioned at seal bootr, and the material outlet of described riser reactor 1 communicates with cyclonic separator through the outlet pipe of seal bootr 3 topmost, cyclonic separator airway; The catalyzer of riser reactor 1 reaction zone and the mixture of reaction oil gas are exported by riser reactor and enter in described cyclonic separator 5 be separated through seal bootr outlet, airway 6.The exit end of preferred described riser reactor 1 connects gas-solid quick disconnector 4, catalyzer and reaction oil gas mixture spray through gas-solid quick disconnector 4, enter in seal bootr, reclaimable catalyst and reaction oil gas gas solid separation faster, thus reduce the reaction of hydro carbons secondary cracking, improve productivity of low carbon olefin hydrocarbon.
In method provided by the invention, described cyclonic separator 5 can be the Cyclonic separating apparatus for gas solid separation of routine known in those skilled in the art.Wherein said cyclonic separator 5 can be that single-stage also can for multistage, it is series connection between every grade of cyclonic separator in usual multi-cyclone, in addition, every grade of cyclonic separator all can arrange one or more cyclonic separator being preferably parallel connection as required.When described cyclonic separator 5 is single-stage time, the top material outlet of riser reactor 1 is connected with the material inlet of single stage cyclone through seal bootr outlet pipe, airway 6, the pneumatic outlet on single stage cyclone top is connected with effuser 7, and the catalyst outlet (dipleg 8) of single stage cyclone is communicated with seal bootr 3.
In method provided by the invention, described revivifier 2 is the conventional revivifier for cracking hydrocarbon oil device.The described reclaimable catalyst needing revivifier 2 to regenerate, from inclined tube 9 to be generated, controls to enter in revivifier 2 through guiding valve 10 to be generated.The catalyst outlet of described revivifier 2 is connected with riser reactor 1 by regenerator sloped tube 16, recycles to be returned in riser reactor 1 through regeneration guiding valve 17 by the catalyzer after being regenerated by revivifier 2.
In order to prevent from regenerated catalyst being returned after in riser reactor 1, flue gas be brought in riser reactor, and affect absorbing-stabilizing system, pneumatic press, increase unnecessary energy expenditure.Under preferable case, remove the flue gas carried secretly in the catalyzer after regeneration, degassing vessel 15 is set between revivifier and riser reactor, described degassing vessel 15 comprises pneumatic outlet, regenerated catalyst inlet and regenerated catalyst outlet, the regenerated catalyst inlet of described degassing vessel 15 is connected by the regenerated catalyst outlet of inclined tube 14 with revivifier 2, the regenerated catalyst outlet of described degassing vessel 15 is communicated with bottom riser reactor 1 by regenerator sloped tube 16, and the pneumatic outlet of described degassing vessel 15 is connected with revivifier 2 by pipeline 13.More preferably, in situation, introduce degassing vessel 15 in order to more be convenient to the catalyzer after by regeneration from the outlet of revivifier 2, the catalyst outlet of described revivifier 2 is positioned at the bottom of revivifier.In method provided by the invention, in described catalyst regenerator, the regenerated catalyst of coke burning regeneration is introduced in degassing vessel, introduce riser reactor bottom cycle after removing oxygen-containing gas to use, in the oxygen-containing gas return catalizer revivifier that degassing vessel top removes, riser reactor is entered to avoid a large amount of regenerated flue gas, finally arrive absorbing-stabilizing system, pneumatic press, increase unnecessary energy expenditure.
In addition, in described revivifier 2, main air source line 18 is from the oxygen-containing gas (as air) bottom revivifier 2 required for enter catalyst regeneration, more preferably, as shown in Figure 1, required oxygen-containing gas enters in air distributor 19 by main air source line 18, enters equably in revivifier 2 after distribution.
In method provided by the invention, described hydrocarbon ils cracker can also comprise effuser 7, described effuser 7 is for collecting the oil gas be separated by described cyclonic separator 5, described effuser 7 can also be communicated with main oil gas piping 24, for carrying the oil gas of collection, described effuser 7 is connected with the subsequent condensation cooling separation of oil gas by main oil gas piping 24.
Preferably, the flue gas in cyclonic separator 11 separation regeneration device and regenerated catalyst are set in described revivifier 2.Flue gas is discharged from the flue 12 at device top by whirlwind.For the ease of discharging flue gas, described cyclonic separator 11 is preferably arranged on the top of revivifier 2.
In method provided by the invention, the operational condition of described riser reactor is: temperature of reaction is 500 ~ 750 DEG C, preferably 540 ~ 720 DEG C, more preferably 560 ~ 700 DEG C, reaction times is 1 ~ 10 second, preferably 2 ~ 6 seconds, more preferably 2 ~ 4 seconds, apparent pressure is 0.05 ~ 1.0MPa, agent-oil ratio is 1 ~ 100, preferably 10 ~ 50, more preferably 20 ~ 40, and the weight ratio of water vapor and stock oil is 0.05 ~ 1.0.
In method provided by the invention, described light hydrocarbon oil raw material to be boiling range the be hydrocarbon-fraction of 25-204 DEG C.One or more in catalytic cracking gasoline, catalytically cracked gasoline, virgin naphtha, coker gasoline, pyrolysis gasoline, pressure gasoline and hydrogenated gasoline can be selected from.
In method provided by the invention, light hydrocarbon oil raw material preheating is introduced in riser reactor after 200-550 DEG C, preferably 250-500 DEG C, more preferably 300-480 DEG C, at a feed entrance point, whole described light hydrocarbon oil stock oil can be introduced in reactor, or at least two different feed entrance points, described light hydrocarbon oil raw material be introduced in reactor according to identical or different ratio.
In method provided by the invention, the described reaction oil gas be separated through cyclonic separator enters subsequent separation system, is separated further and obtains ethene, propylene, C2 ~ C3 alkane, C4 hydrocarbon-fraction, gasoline fraction and diesel oil distillate.Dry gas and liquefied gas be separated further through gas separation equipment and obtain ethene, propylene, C2 ~ C3 alkane, C4 hydrocarbon-fraction, from reaction product, separating ethene is similar to this area convenient technical process with methods such as propylene, and the present invention is not limited in this respect.
Preferably isolated C4 hydrocarbon-fraction is introduced in riser reactor and carry out freshening.Wherein, light hydrocarbon oil raw material can be introduced in reactor in identical position or different feed entrance points from C4 hydrocarbon-fraction.In a more preferred embodiment, the described C4 hydrocarbon-fraction returning riser reactor introduces reactor after described light hydrocarbon oil feedstock position.
In method provided by the invention, oxygen-containing gas is introduced in the bottom of revivifier, described oxygen-containing gas (such as air) introduces revivifier, reclaimable catalyst contacts coke burning regeneration with oxygen, the flue gas generated after catalyzer coke burning regeneration is in revivifier top gas solid separation, such as after cyclonic separator gas solid separation, isolated regenerated flue gas discharges revivifier.
In method provided by the invention, preferred scheme introduces stripping fluid bottom degassing vessel, removes the flue gas that the regenerated catalyst in degassing vessel adsorbs further.Described stripping fluid can be lighter hydrocarbons, water vapour or nitrogen, preferred refinery dry gas or water vapour.In preferred scheme, the stripping fluid introduced bottom degassing vessel is lighter hydrocarbons, such as, adopt the dry gas of refinery.Consumption is the heavy % of 3-10 of light hydrocarbon oil total amount.
In method provided by the invention, preferably in catalyst regenerator, spray into fuel with supplementing energy, described fuel is geseous fuel and/liquid fuel, is preferably the stock oil of fluid catalytic cracking or fluidized catalytic cracking solution preocess or diesel oil distillate or other liquid fuel.
In method provided by the invention, the described pre-lift medium entered bottom riser reactor is various pre-lift medium well known to those skilled in the art, as one or more in water vapour, refinery dry gas, light paraffins, light olefin.The effect of pre-lift medium makes catalyzer accelerate to rise, and forms the catalyst activity plug flow of even density bottom riser reactor.The consumption of pre-lift medium is well known for the person skilled in the art, and in general, the consumption of pre-lift medium accounts for 1 ~ 30 heavy % of hydrocarbon ils total amount, preferably 2 ~ 15 heavy %.
In method provided by the invention, with the total weight of catalyzer, described catalyzer contains: the heavy % of the heavy % of zeolite 1 ~ 60, the heavy % of inorganic oxide 5 ~ 99 and clay 0 ~ 70, its mesolite is as active ingredient, be selected from mesopore zeolite and optional large pore zeolite, mesopore zeolite accounts for 50 ~ 100 heavy % of zeolite gross weight, preferably 70 ~ 100 heavy %, large pore zeolite accounts for 0 ~ 50 heavy % of zeolite gross weight, preferably 0 ~ 30 heavy %.
Described mesopore zeolite is selected from the zeolite with MFI structure, such as ZSM-5 zeolite and/or ZRP zeolite, also modification can be carried out to transition metals such as the non-metallic elements such as above-mentioned mesopore zeolite phosphorus and/or iron, cobalt, nickel, about the more detailed description of ZRP is see US5232675, about the more detailed description of ZSM-5 is see US3702886.Described large pore zeolite is selected from Rare Earth Y (REY), rare earth hydrogen Y(REHY), one or more in the overstable gamma zeolite that obtains of different methods.Described inorganic oxide, as caking agent, is selected from silicon-dioxide (SiO
2) and/or aluminium sesquioxide (Al
2o
3).Described clay, as matrix (i.e. carrier), is selected from kaolin and/or halloysite.
The method that light hydrocarbon oil raw material catalytic cracking provided by the invention produces low-carbon alkene also has the following advantages:
In preferred scheme, postcombustion in a regenerator, can the temperature of flexible revivifier, is whole reactive system additional heat.Inject replacement media bottom regenerated catalyst degassing vessel, both can replace the flue gas of catalyst entrainment further, again can fuel heatable catalyst as a supplement, for device provides more heat.
Adopt method provided by the invention, refinery can produce ethene and propylene to greatest extent from petroleum hydrocarbon, thus realize the technological breakthrough of refinery's concept, change from traditional fuel type and fuel-Lube Type refinery production model to chemical industry type, make refinery from single oil refining to industrial chemicals and the production development of high added value derived product and extension, both solve the problem of petrochemical material shortage, turn improve the economic benefit of refinery.
Further illustrate method provided by the present invention below in conjunction with accompanying drawing, but the present invention is not therefore subject to any restriction.
Accompanying drawing is the schematic flow sheet of the catalysis conversion method of light hydrocarbon oil raw material production low-carbon alkene provided by the invention.As shown in drawings: pre-lift medium enters by bottom riser reactor 1 through pipeline 22, from the regenerated catalyst of regenerator sloped tube 16 under the castering action of pre-lift medium along the upwards accelerated motion of the pre lift zone of riser reactor 1, wherein, described pre-lift medium can be dry gas, water vapour or their mixture.Stock oil through pipeline 20 with the atomizing steam from pipeline 21 in nozzle injecting lift pipe reactor 1, with the catalyst mix in riser reactor 1, there is cracking reaction in stock oil on the catalyzer of heat, and upwards accelerated motion.
The reaction product oil gas generated and the reclaimable catalyst mixture of carbon deposit spray from the gas-solid quick disconnector 4 of riser reactor 1 exit end with cyclonic form, under different centrifugal action, reclaimable catalyst falls into rapidly seal bootr 3, and reaction oil gas enters cyclonic separator 5 through seal bootr upper outlet, airway 6 realizes being separated of reclaimable catalyst and reaction product oil gas, cyclonic separator can be two-stage, to improve gas-solid disngaging efficiency.The pneumatic outlet of reaction product oil gas through cyclonic separator 5 top enters effuser 7, the dipleg 8 of reclaimable catalyst through cyclonic separator 5 bottom after being separated enters seal bootr 3, the to be generated inclined tube 9 of reclaimable catalyst in seal bootr 3 through seal bootr 3 bottom enters in revivifier 2, can be regulated the catalyzer material level in seal bootr by regeneration guiding valve 10; Oil fuel (or gas) injects inclined tube 9 bottom to be generated through pipeline 26 and the dispersion medium (high-temperature flue gas) from pipeline 25 through nozzle, enter in revivifier 2 through inclined tube 9 to be generated after mixing with reclaimable catalyst, main air enters revivifier 2 through pipeline 18 through air distributor 19, burning-off is arranged in the coke on the dense-phase bed reclaimable catalyst bottom revivifier 2, the reclaimable catalyst of inactivation is regenerated, and flue gas enters subsequent power recovery system through the upper gas pipeline 12 of cyclonic separator 11.
The pipeline 14 of catalyzer after regeneration through being communicated with revivifier 2 catalyst outlet enters degassing vessel 15, regenerated catalyst after degassed is recycled to the bottom of riser reactor 1 through inclined tube 16, catalyst recirculation amount can be controlled by regeneration guiding valve 17, gas returns in revivifier 2 through pipeline 13, and the reaction product oil gas in effuser 7 enters subsequent separation system through main oil gas piping 24.
Reaction oil gas in effuser 7 enters the catalytic pyrolysis hydrogen, methane and the ethene that are separated further in follow-up separation system and obtain through main oil gas piping 24, obtain object product ethylene through being separated further; Ethane, propane, propylene and C4 hydrocarbon-fraction, gasoline fraction and diesel oil distillate; C4 hydrocarbon-fraction partly or entirely returns in riser reactor and continues reaction, and C4 hydrocarbon-fraction can mix with light hydrocarbon oil raw material in pipeline 20 injecting lift pipe reactor 1, also can distinguish in injecting lift pipe reactor 1.
The following examples will be further described present method, but not thereby limiting the invention.
Raw material used in embodiment is virgin naphtha, and its character is as shown in table 1.
Catalytic cracking catalyst preparation method used in embodiment is summarized as follows:
1) by 20gNH
4cl is dissolved in 1000g water, in this solution, add 100g(butt) crystallization product ZRP-1 zeolite (produce, SiO by Qilu Petrochemical Company's catalyst plant
2/ Al
2o
3=30, content of rare earth RE
2o
3=2.0 heavy %), after exchanging 0.5h at 90 DEG C, filter to obtain filter cake; Add 4.0gH
3pO
4(concentration 85%) and 4.5gFe (NO
3)
3be dissolved in 90g water, dry with filter cake hybrid infusion; Then within 2 hours, obtain phosphorous and MFI structure mesopore zeolite that is iron 550 DEG C of roasting temperature process, its elementary analytical chemistry consists of
0.1Na
2O·5.1Al
2O
3·2.4P
2O
5·1.5Fe
2O
3·3.8RE
2O
3·88.1SiO
2。
2) use 250kg decationized Y sieve water by 75.4kg halloysite (Suzhou china clay company Industrial products, the heavy % of solid content 71.6) making beating, add 54.8kg pseudo-boehmite (Shandong Aluminum Plant's Industrial products, the heavy % of solid content 63) again, with hydrochloric acid, its PH is adjusted to 2 ~ 4, stir, at 60 ~ 70 DEG C, leave standstill aging 1 hour, keep PH to be 2 ~ 4, cool the temperature to less than 60 DEG C, add 41.5kg Alumina gel (Qilu Petrochemical Company's catalyst plant product, Al
2o
3content is 21.7 heavy %), stir 40 minutes, obtain mixed serum.
3) the MFI structure mesopore zeolite (butt is 22.5kg) of the phosphorous and iron prepared by step 1) and DASY zeolite (Qilu Petrochemical Company's catalyst plant Industrial products, lattice constant is 2.445 ~ 2.448nm, butt is 2.0kg) join step 2) in the mixed serum that obtains, stir, spray drying forming, with ammonium dihydrogen phosphate (phosphorus content is 1 heavy %) washing, wash away free Na+, be drying to obtain catalytic cracking catalyst sample, the MFI structure mesopore zeolite consisting of the phosphorous and iron of 18 heavy % of this catalyzer, 2 heavy %DASY zeolites, 28 heavy % pseudo-boehmites, 7 heavy % Alumina gel and balance kaolin.
Embodiment 1
Embodiment 1 is tested according to the flow process of accompanying drawing, take virgin naphtha as raw material, the middle-scale device of riser reactor is tested, the stock oil being preheated to 250 DEG C enters bottom riser tube, temperature of reaction 675 DEG C, 2 seconds reaction times, the weight ratio 25 of catalytic cracking catalyst and stock oil, the weight ratio of water vapor and stock oil is carry out cracking reaction under 0.5 condition, reaction product and water vapour and reclaimable catalyst enter seal bootr from riser reactor outlet through gas-solid quick disconnector, after initial gross separation, reaction oil gas enters in cyclonic separator with catalyzer and is separated further, react and cut by boiling range through effuser introducing subsequent separation system, thus obtain dry gas, propylene, the cuts such as C4 hydrocarbon-fraction and gasoline, wherein C4 hydrocarbon-fraction Returning reactor reacts further.Reclaimable catalyst enters into revivifier by seal bootr bottom through inclined tube 9 to be generated under gravity, contacts coke burning regeneration with air.Catalyzer after regeneration enters degassing vessel, with the non-hydrocarbon gas impurity removing regenerated catalyst absorption and carry.Regenerated catalyst after stripping turns back in riser tube reaction again and recycles.Operational condition and product slates list in table 2.
As can be seen from Table 2, ethylene yield can reach 21.56 heavy %, and productivity of propylene can reach 23.95 heavy %, and propylene/ethylene ratio is about 1.11.
Embodiment 2
Embodiment 2 is tested according to the flow process of accompanying drawing, take virgin naphtha as raw material, and the middle-scale device of riser reactor is tested, and reaction process is with embodiment 1.Difference is, reaction oil gas is introduced separation system cutting through effuser and obtained dry gas, propylene, carbon four and gasoline fraction, and wherein carbon four returns the further cracking of riser reactor is ethene and propylene.Operational condition and product slates list in table 2.
As can be seen from Table 2, ethylene yield can reach 23.51 heavy %, and productivity of propylene can reach 24.83 heavy %, and propylene/ethylene ratio is about 1.06.
Embodiment 3
This embodiment 2 is tested according to the flow process of accompanying drawing, take virgin naphtha as raw material, reaction process is with embodiment 1, reaction oil gas is introduced separation system cutting through collection chamber and is obtained dry gas, propylene, carbon four and gasoline fraction, and difference is: it is ethene and propylene that (1) C-4-fraction returns the further cracking of riser reactor.(2) C2 ~ C3 alkane enters steam cracking device, under 830 DEG C of conditions, with water vapor contact reacts, is separated and obtains object product ethylene and propylene.Operational condition and product slates list in table 2.
As can be seen from Table 2, ethylene yield can reach 27.64 heavy %, and productivity of propylene can reach 27.97 heavy %, and propylene/ethylene ratio is about 1.01.
Table 1
| Stock oil character | |
| Density (20 DEG C), g/cm 3 | 0.7358 |
| Vapour pressure/kPa | 50.0 |
| Group composition/weight % | |
| Paraffinic hydrocarbons | 51.01 |
| Naphthenic hydrocarbon | 38.24 |
| Alkene | 0.12 |
| Aromatic hydrocarbons | 10.52 |
| Boiling range, DEG C | |
| IBP | 46 |
| 10％ | 87 |
| 30％ | 107 |
| 50% | 120 |
| 70％ | 133 |
| 90％ | 149 |
| 95% | 155 |
Table 2
| Catalyst cracking unit | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Outlet temperature of riser, DEG C | 675 | 675 | 675 |
| Reaction times, second | 2.0 | 1.8 | 1.8 |
| The weight ratio of water vapor/raw material | 0.5 | 0.5 | 0.5 |
| Agent-oil ratio | 25 | 25 | 25 |
| Steam cracking unit | |||
| Cracking temperature | / | / | 830 |
| The weight ratio of water vapor/raw material | / | / | 0.5 |
| The residence time, second | / | / | 0.1 |
| Product slates, heavy % | |||
| Hydrogen+methane | 14.04 | 15.22 | 16.35 |
| Ethene | 21.56 | 23.51 | 27.64 |
| Propylene | 23.95 | 24.83 | 27.97 |
| Ethane+propane | 8.20 | 8.97 | / |
| C4 | 6.27 | / | / |
| Gasoline | 22.02 | 23.08 | 23.77 |
| Diesel oil | 2.36 | 2.43 | 2.35 |
| Coke | 1.60 | 1.96 | 1.92 |
| Add up to | 100.00 | 100.00 | 100.00 |
Claims (18)
1. a Light hydrocarbon oil catalytic conversion method, comprise: light hydrocarbon oil raw material enters bottom the riser reactor of cat-cracker, contact with regenerated catalyst while of carrying out catalytic cracking reaction and upwards flow, the reaction oil gas of riser reactor outlet and reclaimable catalyst gas solid separation, isolated reaction oil gas caterpillar, is separated further and obtains ethene, propylene, C2 ~ C3 alkane, C4 hydrocarbon-fraction and other products; Isolated reclaimable catalyst enters coke burning regeneration in revivifier, recycles in the regenerated catalyst Returning reactor of activity recovery; It is characterized in that, described cat-cracker comprises revivifier (2), runs through the riser reactor (1) of revivifier (2), seal bootr (3) outside riser reactor (1) outlet and cyclonic separator (5); Described riser reactor outlet is communicated with through the entrance of seal bootr (3) top exit with cyclonic separator (5), and the catalyst outlet of cyclonic separator (5) is communicated with seal bootr (3); Described seal bootr (3) bottom is communicated with revivifier (2) through being arranged at revivifier (2) inclined tube to be generated (9) outward.
2. according to the method for claim 1, it is characterized in that, described riser reactor (1) outlet connects gas-solid quick disconnector (4), and described gas-solid quick disconnector (4) has tangential opening, and gas-solid quick disconnector (4) is positioned at seal bootr (3).
3. according to the method for claim 1, it is characterized in that, described riser reactor (1), revivifier (2) and seal bootr (3) are coaxially arranged.
4. according to the method for claim 1, it is characterized in that, the regenerated catalyst outlet of described revivifier (2) is communicated with riser reactor (1) bottom by regenerator sloped tube (16).
5. according to the method for claim 1, it is characterized in that, described cat-cracker also comprises regenerated catalyst degassing vessel (15), regenerated catalyst from revivifier (2) enters regenerated catalyst degassing vessel, regenerated catalyst after degassed returns riser reactor (1) bottom cycle and uses, and the oxygen-containing gas on degassing vessel top returns in revivifier (2).
6. according to the method for claim 5, it is characterized in that, bottom described degassing vessel, introduce stripping fluid, remove the flue gas that the regenerated catalyst in degassing vessel adsorbs further.
7. according to the method for claim 6, it is characterized in that, described stripping fluid is lighter hydrocarbons and/or water vapour, and the amount introducing stripping fluid in degassing vessel is the heavy % of 3-10 of light hydrocarbon oil total amount.
8. according to the method for claim 1, it is characterized in that, in described revivifier, spray into fuel.
9. according to the method for claim 1, it is characterized in that, described inclined tube to be generated (9) arranges fuel inlet, sprays into fuel and dispersion medium through fuel inlet, contain or do not contain oxygen-containing gas.
10. according to any one method of claim 1-9, it is characterized in that, the operational condition of described riser reactor is: temperature of reaction is 500 ~ 750 DEG C, reaction times is 1 ~ 10 second, apparent pressure is 0.05 ~ 1.0MPa, the weight ratio of catalyzer and stock oil is 1 ~ 100, and the weight ratio of water vapor and stock oil is 0.05 ~ 1.0.
11. according to the method for claim 10, and it is characterized in that, the operational condition of described riser reactor is: temperature of reaction is 540 ~ 720 DEG C, and the reaction times is 2 ~ 6 seconds, and agent-oil ratio is 10 ~ 50.
12. according to the method for claim 11, and it is characterized in that, the operational condition of described riser reactor is: temperature of reaction is 560 ~ 700 DEG C, and the reaction times is 2 ~ 4 seconds, and agent-oil ratio is 20 ~ 40.
13. according to any one method of claim 1-9, and it is characterized in that, the operational condition of described revivifier is: regeneration temperature is 550 ~ 750 DEG C, and fluidized bed gas apparent linear velocity is 0.8 ~ 3.0 meter per second, and catalyzer mean residence time is 0.6 ~ 2.0 minute.
14., according to any one method in claim 1-9, is characterized in that, are returned by the C4 hydrocarbon-fraction described in reaction product in riser reactor and continue reaction.
15. according to the method for claim 14, and it is characterized in that, the described C4 hydrocarbon-fraction returning riser reactor introduces reactor after described light hydrocarbon oil feedstock position.
16. according to any one method in claim 1-9, it is characterized in that, with the total weight of catalyzer, described catalyzer contains: the heavy % of the heavy % of zeolite 1 ~ 60, the heavy % of inorganic oxide 5 ~ 99 and clay 0 ~ 70, its mesolite is selected from mesopore zeolite and optional large pore zeolite, mesopore zeolite accounts for 50 ~ 100 heavy % of zeolite gross weight, and large pore zeolite accounts for 0 ~ 50 heavy % of zeolite gross weight.
17., according to the method for claim 16, is characterized in that, described mesopore zeolite accounts for 70 ~ 100 heavy % of zeolite gross weight, and large pore zeolite accounts for 0 ~ 30 heavy % of zeolite gross weight.
18., according to any one method in claim 1-9, is characterized in that, described light hydrocarbon oil raw material to be boiling range the be hydrocarbon-fraction of 25-204 DEG C.
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| CN1319643A (en) * | 2001-02-14 | 2001-10-31 | 中国石化集团洛阳石油化工工程公司 | apparatus for producing low carbon olefines by high-tmep. catalyzing contact cracking from heavy petroleum hydrocarbon |
| CN1974727A (en) * | 2006-12-12 | 2007-06-06 | 中国石油大学(北京) | Catalytic cracker without settler |
| CN102010438A (en) * | 2010-11-11 | 2011-04-13 | 陕西科技大学 | Amino-containing cage type silsesquioxane and preparation method thereof |
| CN102039107A (en) * | 2009-10-13 | 2011-05-04 | 中国石油化工股份有限公司 | Parallel cyclic reaction-regeneration device with embedded riser |
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| CN1319643A (en) * | 2001-02-14 | 2001-10-31 | 中国石化集团洛阳石油化工工程公司 | apparatus for producing low carbon olefines by high-tmep. catalyzing contact cracking from heavy petroleum hydrocarbon |
| CN1974727A (en) * | 2006-12-12 | 2007-06-06 | 中国石油大学(北京) | Catalytic cracker without settler |
| CN102039107A (en) * | 2009-10-13 | 2011-05-04 | 中国石油化工股份有限公司 | Parallel cyclic reaction-regeneration device with embedded riser |
| CN102010438A (en) * | 2010-11-11 | 2011-04-13 | 陕西科技大学 | Amino-containing cage type silsesquioxane and preparation method thereof |
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