CN103772089B - For improving the reaction unit of ethene, propene yield - Google Patents

For improving the reaction unit of ethene, propene yield Download PDF

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Publication number
CN103772089B
CN103772089B CN201210393238.6A CN201210393238A CN103772089B CN 103772089 B CN103772089 B CN 103772089B CN 201210393238 A CN201210393238 A CN 201210393238A CN 103772089 B CN103772089 B CN 103772089B
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reaction zone
bed reaction
ethene
zone
tube
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CN103772089A (en
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齐国祯
杨远飞
王洪涛
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/40—Ethylene production

Abstract

The present invention relates to a kind ofly for improving the reaction unit of ethene, propene yield, mainly solve ethene in prior art, problem that propene yield is lower. the present invention mainly comprises fast bed reaction zone 2 by adopting, distribution grid 3, dense bed reaction zone 8, external warmer 14, fast bed reaction zone 2 ports of export are connected with dense bed reaction zone 8 by distribution grid 3, 1/3～3/4 reaction zone At The Height of fast bed reaction zone 2 is connected to regenerator sloped tube 5, dense bed reaction zone 8 tops are that 9 tops, 9 decanting zone, decanting zone are provided with product gas outlet 11, dense bed reaction zone 8 bottoms have catalyst outlet, respectively with inclined tube 4 to be generated, external warmer 14 is connected, the technical scheme that external warmer 14 bottoms are connected with fast bed reaction zone 2 bottoms by external warmer lower oblique tube 15, solve preferably this problem, can be used for ethene, in the industrial production of propylene.

Description

For improving the reaction unit of ethene, propene yield
Technical field
The present invention relates to a kind of for improving the reaction unit of ethene, propene yield.
Background technology
Low-carbon alkene, i.e. ethene and propylene, is two kinds of important basic chemical industry raw materials, its demand is in continuous increase. OneAs, ethene, propylene are to produce by petroleum path, but due to the limited supply of petroleum resources and higher price, byThe cost that petroleum resources are produced ethene, propylene constantly increases. In recent years, people start to greatly develop alternative materials conversion second processedThe technology of alkene, propylene. Wherein, the important alternative materials of producing for low-carbon alkene of a class is oxygenatedchemicals, for example alcohols(methyl alcohol, ethanol), ethers (dimethyl ether, ethyl methyl ether), ester class (dimethyl carbonate, methyl formate) etc., these oxygenatedchemicals canTo be transformed by coal, natural gas, living beings equal energy source. Some oxygenatedchemicals can reach fairly large lifeProduce, as methyl alcohol, can be made by coal or natural gas, technique is very ripe, can realize the production scale of up to a million tonnes. Due toThe popularity in oxygenatedchemicals source, adds and transforms the economy that generates low-carbon alkene technique, so turned by oxygenatedchemicalsChange the technique of alkene processed (OTO), be particularly subject to increasing attention by the technique of preparing olefin by conversion of methanol (MTO).
In US4499327 patent, silicoaluminophosphamolecular molecular sieve catalyst being applied to preparing olefin by conversion of methanol technique has carried outStudy in great detail, think that SAPO-34 is the first-selected catalyst of MTO technique. SAPO-34 catalyst has very high low-carbon alkene and selectsProperty, and activity is also higher, can make methanol conversion is reaction time of low-carbon alkene to be less than the degree of 10 seconds, more even reachesIn the reaction time range of riser.
In US6166282, announce technology and reactor that a kind of methanol conversion is low-carbon alkene, adopted fast fluidizationBed bioreactor, gas phase, after the lower Mi Xiangfanyingqu of gas speed has reacted, rises to after the fast subregion that internal diameter diminishes rapidly, adoptsGo out most entrained catalyst with special gas-solid separation equipment initial gross separation. Owing to reacting, afterproduct gas and catalyst are quickSeparate, effectively prevented the generation of secondary response. Through analog computation, compared with traditional bubbling fluidization bed bioreactor, this is fastSpeed fluidized-bed reactor internal diameter and the required reserve of catalyst all greatly reduce. But in the method, yield of light olefins generally all exists, there is the problem that yield of light olefins is lower in 77% left and right.
In CN1723262, announce with the multiple riser reaction unit of central catalyst return and turned for oxideTurn to low-carbon alkene technique, this covering device comprises multiple riser reactors, gas solid separation district, multiple offset components etc., eachRiser reactor has the port of injecting catalyst separately, is pooled to the Disengagement zone of setting, and catalyst and gas product are separated.In the method, yield of light olefins is general all between 75～80%, has equally the problem that yield of light olefins is lower.
Still there is ethene, shortcoming that propene yield is lower in prior art, the present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the lower problem of ethene, propene yield existing in prior art, carriesFor a kind of new for improving the reaction unit of ethene, propene yield. This device, for the production of ethene, propylene, has productThe higher advantage of yield of light olefins in product.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of for improving the anti-of ethene, propene yieldShould install, mainly comprise fast bed reaction zone 2, distribution grid 3, dense bed reaction zone 8, external warmer 14, fast bed reaction zone 2 goes outMouth end is connected with dense bed reaction zone 8 by distribution grid 3, and 1/3～3/4 reaction zone At The Height of fast bed reaction zone 2 is connected to againRaw inclined tube 5, dense bed reaction zone 8 tops are that 9 tops, 9 decanting zone, decanting zone are provided with product gas outlet 11,8 ends of dense bed reaction zonePortion has catalyst outlet, is connected respectively with inclined tube 4 to be generated, external warmer 14, and external warmer 14 bottoms are by under external warmerInclined tube 15 is connected with fast bed reaction zone 2 bottoms.
In technique scheme, described silicoaluminophosphamolecular molecular sieve is selected from least one in SAPO-18, SAPO-34; InstituteState and in decanting zone 9, be provided with gas-solid cyclone separator 7; Described distribution grid percent opening is 20～70%; 2 ends of described fast bed reaction zonePortion is provided with raw material feed distributing plate 13; On described external warmer lower oblique tube 15, inclined tube to be generated 4, regenerator sloped tube 5, be equipped with guiding valve,Control catalyst flow; 1/3～1/2 reaction zone At The Height of described fast bed reaction zone 2 is connected to regenerator sloped tube 5; Described close phaseBed reaction zone 8 bottoms are provided with dense bed reaction zone feeds pipeline 17; In described external warmer 14, be provided with heat production coil pipe 6; Outside describedHeat collector lower oblique tube 15, inclined tube to be generated 4, regenerator sloped tube 5 export boat type distributor are all set.
In the present invention, described silicoaluminophosphamolecular molecular sieve preferred version is selected from SAPO-34; The reaction of fast bed reaction zone 2Condition is: reaction pressure taking gauge pressure count 0.01～0.3MPa, mean temperature as 400～500 DEG C, the average coke content of catalyst as1.5～3.5% weight; The reaction condition of described dense bed reaction zone 8 is: reaction pressure is counted 0.01～0.3MPa, flat with gauge pressureAll temperature is that 420～550 DEG C, gas phase linear speed are 0.3～1.0 meter per second; Describedly enter external warmer 14 from dense bed reaction zone 8Mass flow of catalyst be 1～25:1 with the ratio of inclined tube 4 inner catalyst mass flows to be generated, preferred version is 4～15:1; CloseIn bed reaction zone 8 bottom feed pipelines 17, can enter the raw material that comprises methyl alcohol or dimethyl ether mutually.
The computational methods of coke content of the present invention are that carbon deposit quality on the catalyst of certain mass is divided by described urgingAgent quality. Carbon deposit measuring method on catalyst is as follows: will mix the catalyst mix with carbon deposit comparatively uniformly,Then the band C catalyst that weighs certain mass, is put in pyrocarbon analyzer and burns, by infrared analysis burn generate twoCarbonoxide quality, thus the carbonaceous amount on catalyst obtained.
The preparation method of silicoaluminophosphamolecular molecular sieve of the present invention is: first prepare molecular sieve presoma, will rubYour proportioning is 0.03～0.6R: (Si0.01～0.98: Al0.01～0.6: P0.01～0.6): 2～500H2O, wherein RRepresent template, constitutive material mixed liquor obtains at a certain temperature after the crystallization of certain hour; Again, by moleculeAfter sieve presoma, phosphorus source, silicon source, aluminium source, organic formwork agent, water etc. mix according to certain ratio at 110～260 DEG C hydro-thermalAfter crystallization at least 0.1 hour, finally obtain SAPO molecular sieve. The molecular sieve of preparation is mixed to warp with a certain proportion of binding agentAfter crossing the operating procedures such as spraying is dry, roasting, obtain final SAPO catalyst, the percetage by weight of binding agent in molecular sieveGenerally between 10～90%.
In the present invention, percent opening refers to the effective area of distribution grid, the area summation that namely refers to hole on distribution grid face withThe ratio of the distribution grid face gross area.
Known in the field, in the course of reaction that is low-carbon alkene in methanol conversion, on catalyst, accumulate a certain amount ofCarbon distribution is conducive to improve the selective of low-carbon alkene. Adopt method of the present invention, methanol feedstock enters after reaction zone, first with treatRaw catalyst contact, production low-carbon alkene that can high selectivity, the product of generation and unconverted methyl alcohol are upwards urged with regenerationAgent contact, transforms unreacted methyl alcohol, simultaneously because regenerated catalyst has high temperature, highly active feature, so turningChange when methyl alcohol the also above high-carbon hydrocarbon of cracking section carbon four. Meanwhile, the conversion zone that regenerated catalyst returns or above regionNeed the methyl alcohol load of conversion less, the respective reaction heat of emitting is just few, and the method can well be controlled the temperature rise of reaction zone,The temperature of reaction zone is controlled under the state that is beneficial to low-carbon alkene generation. In the present invention, dense bed reaction zone is set, from fastThe gaseous stream that bed reaction zone comes and catalyst are in dense bed reaction zone, and because gas-solid contact time increases, carbon is more than four highThe cracking degree of carbon hydrocarbon increases, because the olefin(e) centent in the above high-carbon hydrocarbon of carbon four is generally all more than 80%, so this part heightThe olefin cracking of carbon becomes ethene, propylene, thereby realizes the object that improves yield of light olefins.
Adopt technical scheme of the present invention: described silicoaluminophosphamolecular molecular sieve is selected from SAPO-18, SAPO-34 at leastA kind of; In described decanting zone 9, be provided with gas-solid cyclone separator 7; Described distribution grid percent opening is 20～70%, and described fast bed is anti-Answer 2 bottoms, district to be provided with raw material feed distributing plate 13; On described external warmer lower oblique tube 15, inclined tube to be generated 4, regenerator sloped tube 5, all establishThere is guiding valve, control catalyst flow; 1/3～1/2 reaction zone At The Height of described fast bed reaction zone 2 is connected to regenerator sloped tube 5; InstituteState dense bed reaction zone 8 bottoms and be provided with dense bed reaction zone feeds pipeline 17; In described external warmer 14, be provided with heat production coil pipe 6;Described external warmer lower oblique tube 15, inclined tube to be generated 4, regenerator sloped tube 5 export boat type distributor are all set, low-carbon alkene carbon base absorption rateCan reach 84.19% weight, exceed and can reach 3 percentage points than low-carbon alkene carbon base absorption rate of the prior art, obtain preferablyTechnique effect.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of scheme of the present invention.
In Fig. 1,1 is methanol feedstock charging; 2 is fast bed reaction zone; 3 is distribution grid; 4 is inclined tube to be generated; 5 for regenerating tiltedlyPipe; 6 is heat production coil pipe; 7 is gas-solid cyclone separator; 8 is dense bed reaction zone; 9 is decanting zone; 10 is collection chamber; 11 for producingProduct gas outlet line; 12 is external warmer gaseous phase outlet pipeline; 13 is methanol feeding distributor; 14 is external warmer; 15 be outsideHeat collector lower oblique tube; 16 is external warmer fluidizing agent entrance; 17 is dense bed reaction zone feeds pipeline.
Methanol feedstock enters in fast bed reaction zone 2 through feeding line 1, contacts with molecular sieve catalyst, and reaction generates and containsHave the product of ethene, propylene, carry reclaimable catalyst and enter dense bed reaction zone 8 through distribution grid 3, the gaseous stream of generation andCatalyst is after cyclone separator 7 separates, and catalyst turns back to dense bed reaction zone 8, gas through the dipleg of cyclone separator 7After phase product introduction collection chamber 10, enter follow-up centrifugal station through outlet line 11. Isolated reclaimable catalyst is through strippingAfter be at least divided into two parts, a part turns back to fast bed reaction by external warmer lower oblique tube 15 after heat exchanger 14 heat exchangeDistrict 2, a part enters coke-burning regeneration in regenerator through inclined tube 4 to be generated, and the catalyst of having regenerated returns by regenerator sloped tube 5In fast bed reaction zone 2.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1～2]
In fluidized bed reaction as shown in Figure 1, catalyst type is in table 1, and the methanol feedstock that purity is 99.5% entersEnter fast bed reaction zone, contact with catalyst, the gaseous stream of generation and catalyst enter dense bed reaction zone through distribution grid,Gaseous stream enters centrifugal station after gas solid separation, and isolated catalyst is divided into two parts, Part I catalyst warpAfter external warmer heat-obtaining, return to described fast bed reaction zone bottom, Part II catalyst enters regenerator regeneration, forms regenerationCatalyst, regenerated catalyst enters 1/3 fast bed reaction zone At The Height of fast bed reaction zone after degassed. In decanting zone, be provided withGas-solid cyclone separator. Fast bed reaction zone bottom is provided with raw material feed distributing plate, external warmer lower oblique tube, inclined tube to be generated, againOn raw inclined tube, be equipped with guiding valve, control catalyst flow, dense bed reaction zone bottom is provided with dense bed reaction zone feeds pipeline, outerIn heat collector, be provided with heat production coil pipe, external warmer lower oblique tube 15, inclined tube to be generated 4, regenerator sloped tube 5 export the distribution of ship type are all setDevice. Part I catalyst is 1:1 with the ratio of Part II mass flow of catalyst. The reaction condition of fast bed reaction zone is:Reaction pressure is counted 0.01MPa, mean temperature as 400 DEG C, the average coke content of catalyst are as 1.5% weight taking gauge pressure; Dense bed is anti-Answer the reaction condition in district to be: reaction pressure taking gauge pressure count 0.01MPa, mean temperature as 420 DEG C, gas phase linear speed as 0.3 meter/Second, distribution grid percent opening is 20%. Keep the mobile stability of controlling of catalyst, reactor outlet product adopts online gas phase lookAnalysis of spectrum, reaction result is in table 1.
Table 1
Parameter Catalyst type Low-carbon alkene carbon base absorption rate, % weight
Embodiment 1 SAPO-18 79.28
Embodiment 2 SAPO-34 81.44
[embodiment 3]
According to condition and step described in embodiment 2, regenerated catalyst enters the 3/4 fast of fast bed reaction zone after degassedSpeed bed reaction zone At The Height. Part I catalyst is 25:1 with the ratio of Part II mass flow of catalyst. Fast bed reactionThe reaction condition in district is: reaction pressure taking gauge pressure count 0.01MPa, mean temperature as 500 DEG C, the average coke content of catalyst as3.5% weight; The reaction condition of dense bed reaction zone is: reaction pressure taking gauge pressure count 0.01MPa, mean temperature as 548 DEG C,Gas phase linear speed is 1.0 meter per seconds, and distribution grid percent opening is 70%. Keep the mobile stability of controlling of catalyst, reactor outlet producesThing adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 82.47% weight.
[embodiment 4]
According to condition and step described in embodiment 2, regenerated catalyst enters the 1/2 fast of fast bed reaction zone after degassedSpeed bed reaction zone At The Height. Part I catalyst is 15:1 with the ratio of Part II mass flow of catalyst. Fast bed reactionThe reaction condition in district is: reaction pressure taking gauge pressure count 0.01MPa, mean temperature as 480 DEG C, the average coke content of catalyst as2.5% weight; The reaction condition of dense bed reaction zone is: in feeding line 17, enter the isolated dimethyl ether of centrifugal station and water,The weight ratio of dimethyl ether and water is 1:1. Reaction pressure taking gauge pressure count 0.01MPa, mean temperature as 502 DEG C, gas phase linear speed as0.7 meter per second, distribution grid percent opening is 60%. Keep the mobile stability of controlling of catalyst, reactor outlet product adopts onlineGas chromatographic analysis, low-carbon alkene carbon base absorption rate is 84.19% weight.
[embodiment 5]
According to condition and step described in embodiment 2, regenerated catalyst enters the 1/2 fast of fast bed reaction zone after degassedSpeed bed reaction zone At The Height. Part I catalyst is 4:1 with the ratio of Part II mass flow of catalyst. Fast bed reaction zoneReaction condition be: reaction pressure is counted 0.01MPa, mean temperature as 460 DEG C, the average coke content of catalyst are as 3% weight taking gauge pressureAmount; The reaction condition of dense bed reaction zone is: reaction pressure is counted 0.01MPa, mean temperature as 473 DEG C, gaseous line taking gauge pressureSpeed is 0.5 meter per second, and distribution grid percent opening is 60%. Keep the mobile stability of controlling of catalyst, reactor outlet product adoptsOnline gas chromatographic analysis, low-carbon alkene carbon base absorption rate is 83.14% weight.
[embodiment 6]
According to condition and step described in embodiment 2, regenerated catalyst enters the 1/2 fast of fast bed reaction zone after degassedSpeed bed reaction zone At The Height. Part I catalyst is 8:1 with the ratio of Part II mass flow of catalyst. Fast bed reaction zoneReaction condition be: reaction pressure is counted 0.3MPa, mean temperature as 490 DEG C, the average coke content of catalyst are as 2.4% taking gauge pressureWeight; The reaction condition of dense bed reaction zone is: reaction pressure is counted 0.3MPa, mean temperature as 524 DEG C, gaseous line taking gauge pressureSpeed is 0.5 meter per second, and distribution grid percent opening is 60%. Keep the mobile stability of controlling of catalyst, reactor outlet product adoptsOnline gas chromatographic analysis, low-carbon alkene carbon base absorption rate is 82.75% weight.
[comparative example 1]
According to condition and step described in embodiment 2, just regenerated catalyst directly returns to fast bed by regenerator sloped tubeReaction zone bottom, the low-carbon alkene carbon base absorption rate of reactor outlet is 79.55% (weight).
[comparative example 2]
According to condition and step described in embodiment 4, just regenerated catalyst directly returns to fast bed by regenerator sloped tubeReaction zone bottom, does not arrange distribution grid and dense bed reaction zone, the gaseous stream of fast bed reaction zone outlet and catalyst processAfter gas solid separation, gaseous stream enters centrifugal station. The low-carbon alkene carbon base absorption rate of reactor outlet is 81.23% (weight).
Obviously, adopt device of the present invention, can reach the object that improves ethene, propylene carbon base absorption rate, have largerTechnical advantage, can be used in the industrial production of ethene, propylene.

Claims (6)

1. for improving a reaction unit for ethene, propene yield, mainly comprise fast bed reaction zone (2), distribution grid (3),Dense bed reaction zone (8), external warmer (14), external warmer gaseous phase outlet pipeline (12), external warmer fluidizing agent entrance(16), fast bed reaction zone (2) port of export is connected with dense bed reaction zone (8) by distribution grid (3), fast bed reaction zone (2)1/3～3/4 reaction zone At The Height be connected to regenerator sloped tube (5), dense bed reaction zone (8) top is decanting zone (9), decanting zone(9) top is provided with product gas outlet (11), and dense bed reaction zone (8) bottom has catalyst outlet, respectively with inclined tube to be generated(4), external warmer (14) is connected, external warmer (14) bottom is by external warmer lower oblique tube (15) and fast bed reaction zone (2)Bottom is connected;
Wherein, dense bed reaction zone (8) bottom is provided with dense bed reaction zone feeds pipeline (17); Distribution grid percent opening is 20～70％；
Described fast bed reaction zone (2) bottom is provided with raw material feed distributing plate (13).
2. according to claim 1 for improving the reaction unit of ethene, propene yield, it is characterized in that described decanting zone(9) in, be provided with gas-solid cyclone separator (7).
3. according to claim 1 for improving the reaction unit of ethene, propene yield, it is characterized in that described external warmerLower oblique tube (15), inclined tube to be generated (4), regenerator sloped tube are equipped with guiding valve on (5), control catalyst flow.
4. according to claim 1 for improving the reaction unit of ethene, propene yield, it is characterized in that described fast bed is anti-Answer 1/3～1/2 reaction zone At The Height in district (2) to be connected to regenerator sloped tube (5).
5. according to claim 1 for improving the reaction unit of ethene, propene yield, it is characterized in that described external warmer(14) in, be provided with heat production coil pipe (6).
6. according to claim 1 for improving the reaction unit of ethene, propene yield, it is characterized in that described external warmerLower oblique tube (15), inclined tube to be generated (4), regenerator sloped tube (5) outlet all arrange boat type distributor.
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CN105085130B (en) * 2014-05-14 2017-11-21 中国石油化工股份有限公司 The process units of converting oxygen-containing compound to low-carbon olefins
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CN112569875A (en) * 2019-09-30 2021-03-30 中国石油化工股份有限公司 Reducing fluidized bed reactor

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