CN1962573A - Method and reactor for catalytic cracking for producing propylene using fluid bed - Google Patents

Method and reactor for catalytic cracking for producing propylene using fluid bed Download PDF

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CN1962573A
CN1962573A CN 200610144290 CN200610144290A CN1962573A CN 1962573 A CN1962573 A CN 1962573A CN 200610144290 CN200610144290 CN 200610144290 CN 200610144290 A CN200610144290 A CN 200610144290A CN 1962573 A CN1962573 A CN 1962573A
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reactor
propylene
catalytic cracking
fluid bed
catalyzer
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CN100551883C (en
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王垚
魏飞
钱震
袁学民
周华群
刘家强
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Tsinghua University
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CHINA NATIONAL CHEMICAL ENGINEERING GROUP Corp
Tsinghua University
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Abstract

The invention discloses a manufacturing method of propylene and multi-layer fluid bed reactor structure as main reacting region or olefin transmitting region, which is characterized by the following: separating C2 and component less than C2, C4 and component less than C4 with object product propylene; circulating; returning to fluid bed in the catalytic crack reacting device; transmitting olefin; controlling operating condition to manufacture propylene selectively; avoiding inert component from accumulating.

Description

The method of catalytic cracking for producing propylene using fluid bed and reactor
Technical field
The present invention relates to the method and the device of catalytic cracking for producing propylene using, be particularly useful for the process of alcohol, ether preparing propylene by catalytic cracking, belong to technical field of chemical engineering.
Background technology
Ethene, propylene are two kinds of basic Organic Chemicals that purposes is wide and demand is big.Ethene, production of propylene mainly rely on steam cracking device coproduction and refinery by-product at present.In recent years, along with the demand to acryloyl derivative (as polypropylene, vinyl cyanide, vinylformic acid, propylene oxide etc.) increases sharply, the propylene demand in the world is strong growth trend, and its increasing degree has surpassed ethene.The following whole world may face the problem of propylene shortage of resources.
The steam cracking propylene simultaneously is the main source of present global propylene, almost accounts for 2/3rds of global propylene ultimate production.The height of steam cracking device propylene simultaneously yield mainly is subjected to the influence of cracking stock.The weight ratio of ethene and propylene is about 2: 1 in petroleum naphtha or the solar oil cracking product, and propylene is not then produced in ethane cracking.Refinery's by-product propylene amount 97% from catalytic cracking unit, the main products of this device is gasoline, diesel oil, propene yield generally only is 4%~5%.As seen, though existing production of propylene technology maturity height, because propylene is coproduction or byproduct, so product structure is severely limited, and can't satisfy the requirement that the propylene consumption increases fast.
In addition, existing production of propylene technology relies on serious to petroleum resources.No matter be steam cracking coproduction or refinery's by-product, it is raw materials used all to be petroleum component, and petroleum resources shortage and price rise all can directly influence production of propylene and product price.Producing alkene with the lightweight oil cracking is example, and raw materials cost has accounted for 60%~80% of production cost at present.Therefore, demand developing the production of propylene novel process that does not rely on petroleum resources urgently.
From coal or Sweet natural gas, can produce methyl alcohol or dme via synthetic gas; Utilize biomass, can make ethanol by biological fermentation.Studies show that in a large number alcohol, the further catalytic pyrolysis of ether can obtain low-carbon alkene, this is the new technology route that non-petroleum path is produced low-carbon alkene.Begin to have the research report of pair methanol dehydration producing light olefins aspect abroad as far back as nineteen sixties.Early stage research work mainly concentrates on the catalyzer research and development, occurs reactor and technical process exploitation subsequently.
According to the difference of the catalyst type that is adopted, produce low-carbon alkene by alcohol/ether and can be divided into two big class technology.First kind technology is based on the ZSM-5 catalyst series.U.S.Pat.No.4,387,263rd, such technology patent the earliest applies for nineteen eighty-two, and core is in the process of methanol-to-olefins, and the restriction methanol conversion is lower than 80%, improves product selectivity by the circulation of by product dme.The patent U.S.Pat.No.4 of Mobil company, 587,373 have further improved this technology from operational condition and raw material availability two aspects.The main advantage of ZSM catalyst series is that carbon accumulation resisting ability is strong, and inactivation is slower.But because the ZSM-5 molecular sieve bore diameter is bigger, generate the high-carbon hydrocarbon of more carbon more than four, cause the selectivity of ethene, propylene relatively low.Lurgi company based on improved ZSM-5 catalyst development fixed bed preparing propylene from methanol (MTP) technology (Publication No.U.S.2003/0139635A1).Methyl alcohol generates the mixture of methyl alcohol, dme and water through pre-reactor, enters multi-stage fixed-bed reactor then, and intersegmental heat-obtaining, primary product are propylene, also has other hydro carbons by product in addition.Fixed-bed reactor through operate continuously in 500~700 hours after, need bubbling air carry out the catalyzer coke-burning regeneration.The alkene that the PCT patent of Lurgi company proposes C4~C6 can be converted into ethene, propylene (PCT WO 2004/018089) under the effect of molecular sieve catalyst.EP 1,508,555 open C 4+The by product circulation transforms the yield of light olefins that can improve in methanol-to-olefins (MTO) process.The up-to-date fixed bed MTP technology that Lurgi company announces is with the C of by-product in the process 4~C 6Alkene returns fixed-bed reactor, perhaps with by product ethene, butylene as disproportionation raw material Returning reacting system, to improve purpose product propene yield, it is said that its propene yield can reach 71%.The disclosed fixed bed MTP of MG Technologies AG technology (U.S.Pat.No.7,015,369) adopts a plurality of reactors, and one of them is as the pre-reactor of methyl alcohol generation dme, and all the other are used as the reactor that generates propylene more than two.The identical point of this technology and Lurgi technology is all to adopt fixed-bed reactor, and each reactor adopts the form that is connected in series (discharging that is the previous stage reactor enters the back A reactor), and difference is round-robin C 3+By product can enter different propylene reactors with dme.
It is that the nonzeolite aperture silicoaluminophosphamolecular molecular sieves that the typical case represents is a catalyzer that the second class technology adopts with SAPO-34, has overcome the C that the ZSM-5 catalyzer brings 4+The shortcoming that component concentration is high.The patent U.S.Pat.No.5 of Uop Inc., 095,163, U.S.Pat.No.5,126,308, U.S.Pat.No.5,191,141 have described the content of relevant this class catalyzer in detail.The SAPO-34 catalyzer is used for alcohol/ether-splitting, and to separate the major advantage of preparing low carbon olefin hydrocarbon be the catalytic activity height, the selectivity height of product ethene, propylene.Because the speed of response of alcohol/ether is exceedingly fast under the SAPO-34 catalyst action, cause small catalyst carbon distribution inactivation also very fast, so fluidized-bed successive reaction-regeneration system rapidly becomes the first-selected reactor types of SAPO-34 catalytic pyrolysis alcohol/ether system alkene.PCT patent WO00/41986 and Chinese patent ZL96115333 disclose successive reaction-regeneration techniques that fluidized-bed reactor is used for this process respectively.UOP and Norsk Hydro company once cooperated to have carried out the fluidized-bed MTO pilot scale of 0.75t/d in nineteen ninety-five, use SAPO-34 catalyzer and can successive reaction-regenerated fluidized bed reaction, continuous operation more than 90 day, methanol conversion 100%, the selectivity of ethene and propylene is respectively 20%-55% and 53%-27%.After this, UOP increases olefin cracking unit (OCR) on the basis of original MTO technology, by with the C in the product 4 +The component cracking can bring up to 85~90% with the overall selectivity of ethene+propylene.By changing operational condition, the ratio of product ethene and propylene weight can be regulated between 1.5~0.75.
The fluidized-bed MTO technology (U.S.Pat.No.6,740,790) that ExxonMobil company proposes adopts SAPO catalyst series, by product C 4+Component is further cracking in main reactor or the auxiliary reactor established in addition, and part is converted into low-carbon alkene, to improve the low-carbon alkene total recovery.When adopting auxiliary reactor, the regenerated catalyst auxiliary reactor of flowing through enters main reactor, and flows back to revivifier from main reactor.The gas-phase product of auxiliary reactor no longer enters main reactor.Exxonmobil company has applied for circulating fluidized bed technique patent (U.S.Pat.Pub.No.2005/0124838A1) subsequently again, carries out catalytic cracking reaction, the C in the product in the fluidized-bed reactor of band standpipe 4+Return standpipe behind component and the low-carbon alkene product separation as fluidizing medium, and cracking generates low-carbon alkene in standpipe.
The moving-bed of Uop Inc.'s exploitation contains the thought that oxygen fatty compounds system propylene (OTP) technology (PCT WO2006/012150A2) has been used for reference the fixed bed MTP technology of MG Technologies AG, transform by the circulation of by product alkene, improve purpose product propene yield.Different is to adopt a plurality of polyphone moving-burden bed reactors to replace fixed-bed reactor, can realize catalyzer successive reaction-regeneration.This technology both had been applicable to the ZSM-5 catalyzer, also was applicable to the SAPO-34 catalyzer, also can adopt the mixed catalyst of the two.In order to prolong catalyst life, Uop Inc. has further proposed improved moving-bed OTP technology (U.S.Pat.Pub.No.2006/0063956A1), and the recycled olefins material is carried out selective hydrogenation, thereby reduces the catalyzer coking.
The methyl alcohol that BASF AG proposes/dme system alkene technology (U.S.Pat.No.4,433,188) adopts the borosilicate catalyzer, comprises two-stage reaction and two sections separation.Material benzenemethanol/dme contacts the generation catalytic cracking reaction with catalyzer in first section reaction zone, product is told C through first separation system 2-C 4Alkene and C 1-C 4Alkane, remaining C 5+Component enters second reaction zone and contacts the generation scission reaction with catalyzer, and product removes aromatic component through second separation system, and first separation system is returned in circulation then.The principal feature of the art of this patent is circulation C 5+Component reacts under different conversion zones and condition with raw material.
Because the technology of preparing of most low-carbon alkenes as the purpose product, even if therefore consider the material circulation, also is the C that pays close attention in unconverted raw material and the product with ethene, propylene, butylene 5+Component, the common circulation transition problem that does not relate to ethene and butylene.Part is that the technology of purpose product improves the propylene total recovery by the by product circulation with the propylene, but most simple form that by product is looped back former reactor that adopts.Have only the moving-bed OTP technology (PCT WO2006/012150A2) of UOP clearly to propose with the C in the product 2Olefin component, C 4After telling, olefin component loops back reactive system.Although this technology has adopted a plurality of reactors, each reactors in series connects, and the product of previous stage reactor must pass through the subsequent stages reactor in turn, comes out just can enter gas separation system from the last step reactor.
The conversion of olefines system propylene technology that Tsing-Hua University proposes (Chinese patent application number 2005101167012) employing SAPO-34 catalyzer is converted into propylene by the alkene cyclical operation with ethene and butylene highly selective.This technology with contain oxygen fatty compounds preparing low-carbon olefin by catalytically cracking PROCESS COUPLING, can form new MTP technology, be main contents of the present invention.
Summary of the invention
The present invention aims to provide method and the reactor that contains oxygen fatty compounds catalytic cracking for producing propylene using.
The method of fluid catalytic cracking system propylene provided by the invention is characterized in that, this method contains following steps successively:
Step (1) is sent into main reaction region in the fluidized bed reactor arrangement to the oxygen fatty compounds that contains of producing that propylene uses, and contact with catalyzer catalytic cracking reaction takes place, and generation comprises purpose product propylene at interior lower carbon number hydrocarbons;
Step (2), the gas of this main reaction region outlet is separated into C through a gas separation system 2And C 2Following component, propylene, propane, C 4And C 4Above component, water and unreacting material, unreacting material returns main reaction region;
Step (3), the described C of step (2) 2And C 2Following component, C 4And C 4Above component is returned the olefin reaction district in this fluidized bed reaction, contacts the back with catalyzer and continues reaction, and the reactant gases product enters described gas separation system;
Step (4), the catalyzer in this main reaction region and the olefin reaction district enters revivifier and burns, and the catalyzer after the regeneration returns in described two reaction zones.
Because most low-carbon alkene preparation technologies as the product extraction, therefore do not relate to ethene, butylene it usually and transform.In order to improve the yield of purpose product propylene, the present invention is with the C in the by product 2-(C 2And C 2Following component), C 4+ (C 4And C 4Above component) separate back circulation Returning reacting system with the product propylene and carry out conversion of olefines, by the red-tape operati condition, highly selective obtains propylene.C wherein 2-Logistics contains methane, ethene, ethane, nitrogen, a small amount of CO, CO 2And hydrogen, wherein the effective ingredient as the hydrocarbon conversion is an ethene; C 4+Logistics contains butylene, divinyl, butane, amylene, pentane etc., and wherein the effective ingredient as the hydrocarbon conversion is butylene, divinyl and amylene etc.In order to prevent the inert component accumulation in the recycle stream, C 2-And C 4+Before Returning reacting system, have and speed on a small quantity to put.C 2-And C 4+Can in a reactor (district), transform, also can independently transform in the reactor (district) at two.
In view of having Equilibrium limit between ethene, propylene, the butylene, and can follow secondary side reactions such as hydrogen transference, olefinic polymerization in the reaction system, therefore in order to obtain higher propylene selectivity and yield, need the temperature and the space velocity conditions of independent control conversion of olefines.The present invention adopts independently olefin reactor (district), make olefin reaction carry out in different reactor (district) with the raw material scission reaction, but the catalyst type of respectively reacting used is identical.Material in each reactor (district) does not mix in reactor (district) mutually.For reaction raw materials, each reactor adopts the mode that is connected in parallel, be that the product that certain reactor flows out directly enters separation system and no longer enters other reactor, this is the essential distinction of the present invention and other band by product round-robin multiple reactor MTP technology, its advantage is to control the residence time of material in reaction system, reduce secondary reaction, improve the selectivity of propylene.
Reactor of the present invention is a fluidized-bed reactor, may operate in bubbling, turbulence or fast fluidized regime, and optimum operational stage is the turbulence fluidization.Catalyzer circulates between reactor and revivifier, to realize successive reaction-regeneration.As resurgent gases carbon deposition catalyst is carried out coke burning regeneration with oxygen-containing gas, optimum resurgent gases is an air.For catalyzer, each reactor can adopt the mode of connection of parallel connection or polyphone.Several parallel connections that Fig. 1-3 provides for embodiments of the invention, series connection and series/parallel integrated mode, the actual scheme that can adopt is not limited in the form that the embodiment of the invention provides.Because of catalyst abrasion and deactivation, need suitably to mend live catalyst in the operate continuously process.Live catalyst can any position from the catalyst recirculation chain mend into, suitable mode be from main reactor or olefin reactor mend into, optimum mode be from revivifier mend into.
Raw material of the present invention is the aliphatics oxygenatedchemicals, contains 1~4 carbon atom in the suitable raw molecule, and the suitableeest raw material comprises methyl alcohol, dme, ethanol or its mixture.Raw material injects main reactor with the form of gas phase, liquid phase or gas-liquid mixed.
Catalyzer of the present invention is made of active ingredient and matrix.Active ingredient comprises zeolite molecular sieve, non-zeolite molecular sieve or its mixture, and wherein the suitable basic structure of zeolite molecular sieve is ZSM-5, and the suitable basic structure of non-zeolite molecular sieve is SAPO-34.Matrix comprises packing material and binding agent, requires it not have catalytic activity.The activity of such catalysts component concentration is 10%~95%, and optimum content is 20%~50%.The intensity of catalyzer and granularity should satisfy the service requirements of fluidized-bed reactor.
Gas separation system has the function of separating the low-carbon (LC) hydro carbons, the reactant gases product can be separated into C 2And C 2Following component, propylene, propane, C 4And C 4Above component, water and unreacting material can be used for reference the gas separation system in thermo-cracking system ethylene unit or the oil catalytic cracking unit.
System propylene multicompartment fluidized bed reactor provided by the invention is characterized in that described reactor body comprises:
A) at least one is arranged on the feed(raw material)inlet of this reactor lower part;
B) at least one is arranged on the decaying catalyst outlet of reactor lower part;
C) at least one is arranged on the regeneration and the live catalyst inlet on reactor top;
D) reaction product gas outlet that is arranged on this reactor head;
E) one or more this inside reactor or outside catalyzer upflow tubes of being arranged on make catalyzer form counter current contact with bottom-up raw material by reactor by described upflow tube from up to down by this reactor;
F) be arranged at least 2 layers of gas distributor at different axial heights place in the described reactor;
G) at least one is arranged on described inside reactor or outside gas-solid quick disconnector and/or cyclonic separator.
Different axial heights place is provided with layer 2-3 or gas distributor more than 3 layers in fluidized-bed reactor, and the orlop gas distributor adopts pipe distributor or board-like sparger, and all the other each layers are board-like sparger.When the orlop gas distributor adopted pipe distributor, the decaying catalyst outlet can place reactor bottom, so that install when stopping catalyst in reactor is drawn off fully.
Catalyzer forms the dense fluidized bed at each gas distributor place, and each layer dense bed material height is identical or different.The upflow tube place is provided with the granules of catalyst flowrate control valve outside, by the valve opening control upper strata fluidized-bed height of bed; Also can not establish the granules of catalyst flowrate control valve, the overflow port height control upper strata fluidized-bed height of bed by interior (outward) upflow tube, interior (outward) upflow tube lower end is provided with back taper or flutter valve structure, and be embedded in lower floor's dense-phase bed, guarantee to have in the upflow tube one section packed particle, pass through the upflow tube short circuit to avoid gas.
Catalyzer flows through reactor from top to bottom, and raw material flows through reactor from bottom to top, and catalyzer and raw material form the gas-solid counter current contact in reactor.Multicompartment fluidized bed effectively reduces the back-mixing in the fluidized-bed reactor.Fresh feed contacts with the low activity catalyst of bottom, helps suppressing carbon distribution and hydrogen transfer reactions, and is useful to improving the propylene selectivity; Residual raw material contacts with the high reactivity regenerated catalyst of top layer, helps raw material and fully transforms.
Influence the yield and the selectivity of purpose product propylene in view of side reaction meetings such as hydrogen transference, olefinic polymerizations, therefore the reactor head particles settling space of not expanding, adopt fast branch or cyclonic separator that gaseous product is separated rapidly with catalyzer, isolated gas phase enters gas separation system, solid catalyst particle by fast branch or revolve the branch dipleg return the fluidized-bed reactor the superiors close mutually in.Detailed fast separation structure design is referring to Chinese invention patent CN1111077C.
Above-mentioned multicompartment fluidized bed reactor can be used as main reactor, also can be used as olefin reactor.Main reactor and olefin reactor can have separately independently quick disconnector or cyclonic separator, also can a shared cover quick disconnector or the cyclonic separator of a plurality of reactors.
The present invention compared with prior art has the following advantages and the high-lighting effect:
(1) adopts independently olefin reactor (district), can the independent regulation main reactor and the operational condition of each olefin reactor, comprise temperature of reaction, reaction pressure, air speed etc., make each reactor all work in optimum regime, help improving the total recovery of purpose product propylene;
(2) product of each reactor no longer entered other reactor tell purpose product propylene through separation system before, can reduce side reactions such as hydrogen transference, olefinic polymerization, helped improving the selectivity of purpose product propylene;
(3) operation of multicompartment fluidized bed gas-solid counter current contact reduces the back-mixing in the fluidized-bed reactor, can suppress side reactions such as hydrogen transference, olefinic polymerization, helps improving the selectivity of feed stock conversion and purpose product propylene;
(4) dilute phase space that do not expand of fluidized-bed reactor top, directly enter fast branch or revolve branch behind product and the catalyzer disengaging fluidized-bed bed and carry out gas solid separation, can reduce side reactions such as hydrogen transference, olefinic polymerization, help improving the selectivity of purpose product propylene;
(5) transform by the by product circulation, can improve the total recovery of purpose product propylene.
Description of drawings
Fig. 1 is the process flow sheet of embodiment one.
Fig. 2 is the process flow sheet of embodiment two.
Fig. 3 is the process flow sheet of embodiment three.
Fig. 4 is a kind of multicompartment fluidized bed structure of reactor synoptic diagram.
Fig. 5 is another kind of multicompartment fluidized bed structure of reactor synoptic diagram.
Among the figure: the 100-revivifier; The 101-olefin reactor; 102-C 2Olefin reactor;
The 104-main reactor; 106-C 4+Olefin reactor; The 110-gas separation system;
The 20-regenerated flue gas; The 22-resurgent gases; The 24-raw material; 25-C 2-With C 4+Reaction product; 26-C 2-Reaction product;
28-C 2-Returning reactor; 30-raw material split product; 32-advances the main reactor material; 34-C 4+Reaction product;
36-C 4+Returning reactor; The unconverted raw material of 38-goes out separation system; 40-C 2-Go out separation system;
42-C 4+Go out separation system; The charging of 44-separation system; 46-C 4+Discharge; The 48-propylene; 50-propane;
52-water; 54-C 2-discharge;
80,81,84,88,89,91, the 92-reclaimable catalyst;
82,86,87, the fresh or regenerated catalyst of 90-;
83, catalyzer in the middle of the 85-
201-gas-solid quick disconnector; The 202-cyclonic separator; The 203-catalyst inlet; Heat removing tube in the 205-;
The board-like gas distributor of 207-; 209-outside heat removing pipe; The 211-external warmer; 213-tubular gas sparger;
The 215-material inlet; The 217-catalyst outlet; 219-catalyst stream control valve; 221-catalyzer upflow tube;
The 223-reacting product outlet
Bottom gas distributor among Fig. 4 and Fig. 5, catalyzer upflow tube form can exchange, and gas-solid quick disconnector and cyclonic separator can exchange.The interior outside heat removing mode of bed can exchange about among Fig. 4 and Fig. 5, but also each bed all adopts interior heat-obtaining or outside heat removing mode.Gas-solid quick disconnector and cyclonic separator among Fig. 4 and Fig. 5 can be used in combination, to improve gas-solid separating effect.
Embodiment
Embodiment one
With methyl alcohol is raw material, and the SAPO-34/ silica gel particle is a catalyzer, and the content of active ingredient SAPO-34 in catalyzer is 30%.Adopt technical process as shown in Figure 1.Reactive system comprises two reactors: 104 are main reactor, are used for the raw material cracking; 101 is olefin reactor, is used for C 2-With C 4+Transform.The product of two reactors converges and enters gas separation system, is separated into C 2-, propylene, propane, C 4+, unconverted raw material and water, wherein C 2-With C 4+Each returns 101 olefin reactor after discharging 1% (weight percent), and unconverted raw material returns 104 main reactors.400 ℃ of main reactor interior reaction temperatures, pressure 0.1MPa, charging (comprising recycle feed) weight space velocity 10hr -1600 ℃ of olefin reactor interior reaction temperatures, pressure 0.1MPa, feed weight air speed 100hr -1, one way olefin conversion 10%.The catalyzer of part inactivation enters revivifier in each reactor, carries out coke burning regeneration with air, returns each reactor after the regeneration continuously.650 ℃ of regeneration temperatures, regeneration pressure 0.1MPa.
Embodiment two
With methyl alcohol and alcoholic acid mixture is raw material, and the SAPO-34/ silica gel particle is a catalyzer, and the content of active ingredient SAPO-34 in catalyzer is 80%.Adopt technical process as shown in Figure 2.Reactive system comprises three reactors: 102 are C 2Olefin reactor is used for C 2-Transform; 104 is main reactor, is used for the dme cracking; 106 is C 4+Olefin reactor is used for C 4+Transform.The product of three reactors converges and enters gas separation system, is separated into C 2-, propylene, propane, C 4+, dme and water, wherein C 2-With C 4+Return 102 and 106 olefin reactor after each discharges 2% respectively, unconverted raw material returns 104 main reactors.350 ℃ of main reactor 104 interior reaction temperatures, pressure 1MPa, charging (comprising recycle feed) weight space velocity 0.5hr -1C 2400 ℃ of olefin reactor 102 interior reaction temperatures, pressure 1MPa, feed weight air speed 0.1hr -1C 4+400 ℃ of olefin reactor 106 interior reaction temperatures, pressure 1MPa, feed weight air speed 1hr -1The regenerated catalyst agent enters reactor 102,104,106 respectively from revivifier 100, and reclaimable catalyst returns revivifier 100 from reactor 102,104,106.Revivifier carries out coke burning regeneration with air, 600 ℃ of regeneration temperatures, regeneration pressure 1MPa.
Embodiment three
With the dme is raw material, and the ZSM-5/ silica gel particle is a catalyzer, and the content of active ingredient ZSM-5 in catalyzer is 10%.Adopt technical process as shown in Figure 3.Reactive system comprises three reactors: 102 are C 2Olefin reactor is used for C 2-Transform; 104 is main reactor, is used for the dme cracking; 106 is C 4+Olefin reactor is used for C 4+Transform.The product of three reactors converges and enters gas separation system, is separated into C 2-, propylene, propane, C 4+, dme and water, wherein C 2-With C 4+Return 102 and 106 olefin reactor after each discharges 2% respectively, unconverted dme returns 104 main reactors.400 ℃ of main reactor 104 interior reaction temperatures, pressure 1MPa, charging (comprising the circulation dme) weight space velocity 10hr -1C 2500 ℃ of olefin reactor 102 interior reaction temperatures, pressure 1MPa, feed weight air speed 0.1hr -1, C 2Alkene per pass conversion 50%; C 4+400 ℃ of olefin reactor 106 interior reaction temperatures, pressure 1MPa, feed weight air speed 20hr -1, C 4+Alkene per pass conversion 10%.The regenerator that comes out from revivifier 100 at first enters C 2Olefin reactor 102 flows into C again behind main reactor 104 4+Olefin reactor 106, reclaimable catalyst is from C 4+Olefin reactor 106 is returned revivifier 100.Revivifier carries out coke burning regeneration with air, 600 ℃ of regeneration temperatures, regeneration pressure 1MPa.
Embodiment four
Mixture with methyl alcohol and dme is a raw material, SAPO-34/Al 2O 3Particle is a catalyzer, and the content of active ingredient SAPO-34 in catalyzer is 30%.Adopt technical process as shown in Figure 1.Reactive system comprises two reactors: 104 are main reactor, are used for the raw material cracking; 101 is olefin reactor, is used for C 2With C 4+Transform.The product of two reactors converges and enters gas separation system, is separated into C 2-, propylene, propane, C 4+, unconverted raw material and water, wherein C 2-With C 4+Each returns 101 olefin reactor after discharging 1% (weight percent), and unconverted raw material returns 104 main reactors.500 ℃ of main reactor interior reaction temperatures, pressure 0.1MPa, charging (comprising recycle feed) weight space velocity 10hr -1600 ℃ of olefin reactor interior reaction temperatures, pressure 0.1MPa, feed weight air speed 100hr -1, one way olefin conversion 40%.The catalyzer of part inactivation enters revivifier in each reactor, carries out coke burning regeneration with air, returns each reactor after the regeneration continuously.650 ℃ of regeneration temperatures, regeneration pressure 0.1MPa.
Embodiment five
With ethanol is raw material, SAPO-34/Al 2O 3Particle is a catalyzer, and the content of active ingredient SAPO-34 in catalyzer is 50%.Adopt technical process as shown in Figure 3.Reactive system comprises three reactors: 102 are C 2Olefin reactor is used for C 2Transform; 104 is main reactor, is used for the dme cracking; 106 is C 4+Olefin reactor is used for C 4+Transform.The product of three reactors converges and enters gas separation system, is separated into C 2-, propylene, propane, C 4+, dme and water, wherein C 2-With C 4+Return 102 and 106 olefin reactor after each discharges 2% respectively, unconverted dme returns 104 main reactors.450 ℃ of main reactor 104 interior reaction temperatures, pressure 0.1MPa, charging (comprising the circulation dme) weight space velocity 10hr -1C 2500 ℃ of olefin reactor 102 interior reaction temperatures, pressure 0.1MPa, feed weight air speed 0.1hr -1, C 2Alkene per pass conversion 50%; C 4+450 ℃ of olefin reactor 106 interior reaction temperatures, pressure 0.1MPa, feed weight air speed 5hr -1, C 4+Alkene per pass conversion 70%.The regenerator that comes out from revivifier 100 at first enters C 2Olefin reactor 102 flows into C again behind main reactor 104 4+Olefin reactor 106, reclaimable catalyst is from C 4+Olefin reactor 106 is returned revivifier 100.Revivifier carries out coke burning regeneration with air, 650 ℃ of regeneration temperatures, regeneration pressure 0.1MPa.
Embodiment six
Mixture with ethanol and dme is a raw material, SAPO-34/Al 2O 3Particle is a catalyzer, and the content of active ingredient SAPO-34 in catalyzer is 50%.Adopt technical process as shown in Figure 3.Reactive system comprises three reactors: 102 are C 2Olefin reactor is used for C 2-Transform; 104 is main reactor, is used for the dme cracking; 106 is C 4+Olefin reactor is used for C 4+Transform.The product of three reactors converges and enters gas separation system, is separated into C 2-, propylene, propane, C 4+, dme and water, wherein C 2-With C 4+Return 102 and 106 olefin reactor after each discharges 4% respectively, unconverted dme returns 104 main reactors.350 ℃ of main reactor 104 interior reaction temperatures, pressure 0.1MPa, charging (comprising the circulation dme) weight space velocity 10hr -1C 2350 ℃ of olefin reactor 102 interior reaction temperatures, pressure 0.1MPa, feed weight air speed 0.1hr -1, C 2Alkene per pass conversion 10%; C 4+350 ℃ of olefin reactor 106 interior reaction temperatures, pressure 0.1MPa, feed weight air speed 5hr -1, C 4+Alkene per pass conversion 60%.The regenerator that comes out from revivifier 100 at first enters C 2Olefin reactor 102 flows into C again behind main reactor 104 4+Olefin reactor 106, reclaimable catalyst is from C 4+Olefin reactor 106 is returned revivifier 100.Revivifier carries out coke burning regeneration with air, 650 ℃ of regeneration temperatures, regeneration pressure 0.1MPa.
Embodiment seven
With SAPO-34/Al 2O 3Being catalyzer, is raw material with methyl alcohol, adopts technical process shown in 3 and two-section flowing bed reactor made propylene as shown in Figure 4.Two-layer gas distributor is set in the reactor, and wherein lower floor adopts pipe distributor, and board-like sparger is adopted on the upper strata.The sparger percentage of open area is 1%.The upper strata is by the inner coil pipe heat-obtaining, and lower floor is by the external warmer heat-obtaining.Regenerated catalyst and live catalyst inlet are positioned on the second layer dense fluidized bed, and the reclaimable catalyst outlet is positioned at the bed bottom.Regulate the height of two-layer fluidized-bed layer up and down by the control valve that is positioned on the outer upflow tube.The particles settling space that does not expand at the fluidized-bed top makes gaseous product separate rapidly with granules of catalyst by the gas-solid quick disconnector.The following dipleg of quick disconnector is imbedded in the dense-phase bed of upper strata, and its end is provided with the back taper structure.Isolated gaseous product is drawn from reactor top.
Embodiment eight
With SAPO-34/Al 2O 3Being catalyzer, is raw material with methyl alcohol, adopts technical process shown in 3 and two-section flowing bed reactor made propylene as shown in Figure 5.Two-layer board-like gas distributor is set in the reactor, and percentage of open area is 1%.The upper strata is by the inner coil pipe heat-obtaining, and lower floor is by the external warmer heat-obtaining.Regenerated catalyst and live catalyst inlet are positioned on the second layer dense fluidized bed, and the reclaimable catalyst outlet is positioned at the bed bottom, and raw material gas inlet is positioned at the reactor lower curtate.The height of the overflow port position control upper strata fluidized-bed bed by interior upflow tube, interior upflow tube bottom is embedded in lower floor's dense-phase bed, and its end is provided with the back taper structure.The particles settling space that does not expand at the fluidized-bed top adopts built-in two stage cyclone separator that gaseous product is separated rapidly with granules of catalyst.The following dipleg of cyclonic separator is imbedded in the dense-phase bed of upper strata, and its end is provided with the flutter valve structure.Isolated gaseous product is drawn from reactor top.

Claims (34)

1. the method for catalytic cracking for producing propylene using fluid bed is characterized in that, this method contains following steps successively:
Step (1) is sent into main reaction region in the fluidized bed reactor arrangement to the oxygen fatty compounds that contains of producing that propylene uses, and contact with catalyzer catalytic cracking reaction takes place, and generation comprises purpose product propylene at interior lower carbon number hydrocarbons;
Step (2), the gas of this main reaction region outlet is separated into C through a gas separation system 2And C 2Following component, propylene, propane, C 4And C 4Above component, water and unreacting material, unreacting material returns main reaction region;
Step (3), the described C of step (2) 2And C 2Following component, C 4And C 4Above component is returned the olefin reaction district in this fluidized bed reaction, contacts the back with catalyzer and continues reaction, and the reactant gases product enters described gas separation system;
Step (4), the catalyzer in this main reaction region and the olefin reaction district enters revivifier and burns, and the catalyzer after the regeneration returns in described two reaction zones.
2. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the C described in the step (2) 2And C 2Following component contains methane, ethene, ethane, nitrogen, a small amount of CO, CO 2And hydrogen, wherein the effective constituent as the hydrocarbon conversion is ethene.
3. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the C described in the step (2) 4And C 4Above component contains butylene, divinyl, butane, pentane, amylene, and wherein the effective constituent as the hydrocarbon conversion is butylene, divinyl and amylene.
4. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the C described in the step (2) 2And C 2Following component, C 4And C 4Above component had on a small quantity before returning described olefin reaction district and discharges, to prevent the inert component accumulation.
5. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the C described in the step (2) 2And C 2Following component, C 4And C 4Above component is carried out olefin reaction in same olefin reaction district.
6. the method for catalytic cracking for producing propylene using fluid bed is characterized in that, the C described in the step (2) 2And C 2Following component, C 4And C 4Above component is independently carried out olefin reaction in the olefin reaction district at two respectively.
7. according to the method for claim 1,5,6 described catalytic cracking for producing propylene using fluid bed, it is characterized in that the exit gas in described olefin reaction district and the exit gas of main reaction region are respectively or enter described gas separation system after converging.
8. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the used catalyst type in main reaction region and olefin reaction district is identical.
9. according to the method for claim 1,5,6 described catalytic cracking for producing propylene using fluid bed, it is characterized in that the decaying catalyst in main reaction region and the olefin reaction district independently enters revivifier and burns, corresponding reaction zone is independently returned in the regeneration back.
10. according to the method for claim 1,5,6 described catalytic cracking for producing propylene using fluid bed, it is characterized in that, live catalyst from described revivifier mend into or add.
11. the method for catalytic cracking for producing propylene using fluid bed according to claim 9 is characterized in that, in described revivifier, used resurgent gases was an air when catalyzer burnt.
12. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, described main reaction region and olefin reaction district are fluidized-bed reactors independently.
13. the method according to claim 1,5,6 described catalytic cracking for producing propylene using fluid bed is characterized in that, for catalyzer, between described main reaction region and the olefin reaction district, all be connected in series between each olefin reaction district.
14. the method according to claim 1,5,6 described catalytic cracking for producing propylene using fluid bed is characterized in that, for catalyzer, between described main reaction region and the olefin reaction district, all be connected in parallel between each olefin reaction district.
15. method according to claim 1,6 described catalytic cracking for producing propylene using fluid bed, it is characterized in that, for catalyzer, not only connected between described main reaction region and the olefin reaction district, between each olefin reaction district, but also be connected in parallel.
16. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, contain 1-4 carbon atom described containing in the oxygen fatty compounds molecule.
17. the method for catalytic cracking for producing propylene using fluid bed according to claim 16 is characterized in that, the optimum raw material comprises methyl alcohol or dme or ethanol or two mixture among them at least.
18. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, described catalyzer is made of active ingredient and inert base, and the content of active ingredient is 10%-95%.
19. the method for catalytic cracking for producing propylene using fluid bed according to claim 18 is characterized in that, the optimum content of described active ingredient is 20%-50%.
20. the method for catalytic cracking for producing propylene using fluid bed according to claim 18, it is characterized in that, described activity of such catalysts component comprises: zeolite molecular sieve, non-zeolite molecular sieve or its mixture, and wherein zeolite molecular sieve is suitable for ZSM-5, and non-zeolite molecular sieve is suitable for SAPO-34.
21. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, described raw material enters main reaction region with gas phase, liquid phase or gas-liquid mixed form.
22. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the temperature of described main reaction region is 350 ℃-500 ℃, and pressure is 0.1MPa-1MPa, and the weight space velocity that comprises the charging of recycle feed is 0.5hr -1-10hr -1
23. the method for catalytic cracking for producing propylene using fluid bed according to claim 1 is characterized in that, the temperature in described olefin reaction district is 350 ℃-600 ℃, and pressure is 0.1MPa-1MPa, and the weight space velocity of charging is 1hr -1-100hr -1
24. the method for catalytic cracking for producing propylene using fluid bed according to claim 1, it is characterized in that, described gas separation system has the function of separating the low-carbon (LC) hydro carbons, adopts the gas separation system in thermo-cracking ethylene unit gas separation system or the oil catalytic cracking unit.
25. the method according to claim 1,5,6 described catalytic cracking for producing propylene using fluid bed is characterized in that, described C 2And C 4The olefin reaction district in decaying catalyst enter corresponding revivifier respectively and burn, corresponding reaction zone is independently returned in the regeneration back.
26. make the multicompartment fluidized bed reactor that propylene is used for one kind, it is characterized in that this reactor can be used as main reactor or olefin reactor, described reactor body comprises:
A) at least one is arranged on the feed(raw material)inlet of this reactor lower part;
B) at least one is arranged on the decaying catalyst outlet of reactor lower part;
C) at least one is arranged on the regeneration and the live catalyst inlet on reactor top;
D) reaction product gas outlet that is arranged on this reactor head;
E) one or more this inside reactor or outside catalyzer upflow tubes of being arranged on make catalyzer form counter current contact with bottom-up raw material by reactor by described upflow tube from up to down by this reactor;
F) be arranged at least 2 layers of gas distributor at different axial heights place in the described reactor;
G) at least one is arranged on described inside reactor or outside gas-solid quick disconnector and/or cyclonic separator.
27. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26 is characterized in that, undermost gas distributor adopts pipe distributor or board-like sparger in the described gas distributor.
28. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 27 is characterized in that, when orlop adopted the tubular gas sparger, the decaying catalyst outlet was positioned at reactor bottom.
29. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26 is characterized in that, the upflow tube place is provided with the catalyst stream control valve with the control upper strata fluidized-bed height of bed outside described.
30. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26, it is characterized in that, in the described catalyzer or outer upflow tube lower end is provided with back taper or flutter valve structure, and is embedded in lower floor's dense fluidized bed, avoids reactant gases by described upflow tube short circuit.
31. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26, it is characterized in that, described gas-solid quick disconnector or cyclonic separator are arranged in the particle dilute phase space of described reactor head, reduce the volume of particle dilute phase space simultaneously as far as possible.
32. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26 is characterized in that, constitutes a cover reaction unit with a plurality of described reactors, described a plurality of reactors all have separately independently gas-solid quick disconnector and/or cyclonic separator.
33. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26 is characterized in that, in the cover reaction unit with a plurality of reactors formations, and a shared cover gas-solid quick disconnector and/or the cyclonic separator of described a plurality of reactors.
34. a kind of multicompartment fluidized bed reactor that propylene is used of making according to claim 26, it is characterized in that, described reactor has at least one group of inner and/or outside heat removing tube, described outside heat removing tube is arranged in outside heat collector, and described inside heat removing pipe is arranged in the dense fluidized bed that catalyzer forms on each gas distributor.
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