CN102190539B - Method for increasing propylene yield - Google Patents
Method for increasing propylene yield Download PDFInfo
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- CN102190539B CN102190539B CN2010101164640A CN201010116464A CN102190539B CN 102190539 B CN102190539 B CN 102190539B CN 2010101164640 A CN2010101164640 A CN 2010101164640A CN 201010116464 A CN201010116464 A CN 201010116464A CN 102190539 B CN102190539 B CN 102190539B
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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
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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
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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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
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- Y02P30/40—Ethylene production
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Abstract
The invention relates to a method for increasing propylene yield, which mainly solves the problem of low propylene yield in the prior art. The method comprises steps as follows: (a) raw materials, including methanol, are converted into a stream of products, including ethylene, propylene and C4 olefins, under effective conditions, and are passed through a separation system to obtain the ethylene, propylene, mixed C4+ hydrocarbons and other byproducts; (b) the mixed C4+ hydrocarbons enter a catalytic cracking system, and the reaction products are separated to obtain a C4- product stream and a new mixed C4+ hydrocarbon stream; and (c) the C4- product stream returns to the separation system, and the new mixed C4+ hydrocarbon stream and at least part of ethylene enter an olefin disproportionation system to obtain the propylene product. The technical scheme well solves the problem of low propylene yield, and the method can be used for industrial production of low-carbon olefins.
Description
Technical field
The present invention relates to a kind of method that improves propene yield.
Technical background
Low-carbon alkene, namely ethene and propylene are two kinds of important basic chemical industry raw materials, its demand is in continuous increase.Usually, ethene, propylene are to produce by petroleum path, but because limited supply and the higher price of petroleum resources, the cost of being produced ethene, propylene by petroleum resources constantly increases.In recent years, people begin to greatly develop the technology that alternative materials transforms ethene processed, propylene.Wherein, the important alternative materials that is used for light olefin production of one class is oxygenatedchemicals, such as alcohols (methyl alcohol, ethanol), ethers (dme, methyl ethyl ether), ester class (methylcarbonate, methyl-formiate) etc., these oxygenatedchemicalss can be transformed by coal, Sweet natural gas, biomass equal energy source.Some oxygenatedchemicals can reach fairly large production, such as methyl alcohol, can be made by coal or Sweet natural gas, and technique is very ripe, can realize up to a million tonnes industrial scale.Because the popularity in oxygenatedchemicals source, add and transform the economy that generates light olefin technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), particularly the technique by preparing olefin by conversion of methanol (MTO) is subject to increasing attention.
In the US4499327 patent silicoaluminophosphamolecular molecular sieve catalyst is applied to preparing olefin by conversion of methanol technique and studies in great detail, think that SAPO-34 is the first-selected catalyzer of MTO technique.The SAPO-34 catalyzer has very high light olefin selectivity, and activity is also higher, and can make methanol conversion is reaction times of light olefin to be less than 10 seconds degree, more even reach in the reaction time range of riser tube.
Technology and reactor that a kind of oxygenate conversion is low-carbon alkene have been announced among the US6166282, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu reaction of gas speed is finished, after rising to the fast subregion that internal diameter diminishes rapidly, adopt special gas-solid separation equipment initial gross separation to go out most entrained catalyst.Because reaction after product gas and catalyzer sharp separation have effectively prevented the generation of secondary reaction.Through analog calculation, to compare with traditional bubbling fluidization bed bioreactor, this fast fluidized bed reactor internal diameter and the required reserve of catalyzer all greatly reduce.
The multiple riser reaction unit of having announced among the CN1723262 with central catalyst return is low-carbon alkene technique for oxygenate conversion, this covering device comprises a plurality of riser reactors, gas solid separation district, a plurality of offset components etc., each riser reactor has the port of injecting catalyst separately, be pooled to the disengaging zone of setting, catalyzer and gas product are separated.
Olefin metathesis is by under the effect of transition metal compound catalyst, makes the two bond ruptures of C=C and again formation in the alkene, to obtain the process of new olefin product.Utilize the cross disproportionation effect of butylene and ethene, can by adding an amount of ethene, C4 olefin feedstock relative surplus, that added value is lower be converted into the high added value propylene product.US5898091 and US6166279 have reported C4, C5 olefin treated.Wherein in the preparing propylene through olefin disproportionation process, the catalyzer that adopts is Re
2O
7/ Al
2O
3, reactor is moving-bed.US6358482 has proposed a kind of device of producing iso-butylene and propylene with the C 4 fraction hydrocarbon.The C 4 fraction hydrocarbon is isolated iso-butylene and 1-butylene and 2-butylene through selecting after hydrogenation and the rectifying, and the 1-butylene of separating generates 2-butylene by double-bond isomerization, and rich 2-butylene material and ethene disproportionation reaction generate propylene.Used disproportionation reaction catalyzer is Re
2O
7/ Al
2O
3, WO 00014038 has introduced a kind of method of preparing propylene by butene disproportionation.The raw material butylene is 1-butylene, 2-butylene or its mixture, and catalyzer is WO
3/ SiO
2
Disclose a kind of employing among the document CN1490287A take carbon containing four or carbon pentaene hydrocarbon mixture as raw material, in fixed-bed reactor, adopted 350 ℃～500 ℃ temperature, the pressure of 0.6～1.0MPa and 1～10 hour
-1React the method for preparing ethene and propylene under the condition of weight space velocity.The method introduces modification and the reaction result thereof of dissimilar catalyzer, and reaction raw materials is mainly for carbon four and carbon Wuyuan material, and do not comprise the cracking situation of carbon five above alkene, there are the problems such as the life-span yield shorter and the purpose product of catalyzer is lower in the fixed-bed reactor that adopt of the document simultaneously.
LURGI has announced the Propylur technique of its carbon four and above alkene increased low carbon olefine output thereof, this technique is under the reaction conditions of low pressure, high temperature, catalyzer existence and thermal insulation, be C4 propylene to the conversion of olefines of C7, a technique of by-product ethene and pyrolysis gasoline simultaneously.Test in the middle of it at reaction velocity: 1.6 hours
-1, 480 ℃ of reactor inlet temperatures, reactor pressure 0.2MPa, 440 ℃ of reactor outlet temperature, pressure 0.19MPa, water: C4 (mol ratio) reacts under 7.26 conditions.
In methanol-to-olefins reaction process, inevitably can produce the by products such as carbon four above hydrocarbon, reduced to a great extent the carbon back utilization ratio in the methyl alcohol.And the four above hydrocarbon feeds of the carbon in the modern petrochemical industry itself just are in superfluous state, and its further utilization is the focus of discussing always.Because the olefin(e) centent in the carbon four above hydrocarbon by products that methanol to olefins reaction produces is all higher, therefore can consider to be further converted to propylene product.The present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the low problem of propene yield in the prior art, and a kind of method of new raising propene yield is provided.The method is used for the production of low-carbon alkene, has advantages of that propene yield is high.
The technical solution used in the present invention is as follows: a kind of method that improves propene yield, may further comprise the steps: the raw material that (a) comprises methyl alcohol is converted into the product stream that comprises ethene, propylene, C 4 olefin under condition for validity, obtains ethene, propylene, the above hydrocarbon of mixed c 4, other by product after separation system; (b) the above hydrocarbon of described mixed c 4 enters the catalytic pyrolysis system, and reaction product obtains carbon number less than 4 product stream and the new above hydrocarbon stream of mixed c 4 after separating; (c) described carbon number returns described separation system less than 4 product stream, and the above hydrocarbon stream of described new mixed c 4 enters the olefin metathesis system with described at least a portion ethene, obtains comprising the product of propylene.
In the technique scheme, described condition for validity comprises: temperature of reaction is 400～500 ℃, and reaction pressure is counted 0～0.3MPa with gauge pressure, and reactor is fast fluidized bed, and catalyzer is the microsphere particle that comprises the SAPO-34 molecular sieve; Described catalytic pyrolysis system response condition: temperature of reaction is 450～600 ℃, and reactor is fixed bed or fluidized-bed, and catalyzer is SAPO-34 or ZSM-5; Described olefin metathesis system response condition: temperature of reaction is 200～450 ℃, and reaction pressure is counted 0～2Mpa with gauge pressure, and weight hourly space velocity is 0.6～10 hour
-1, catalyzer is at least a metal or its oxide compound of load W, Mo or Re, and charge capacity is 1～25% by weight, and carrier can be aluminum oxide, silicon oxide, MCM-48 or SBA-15 molecular sieve; Other by product comprises hydrogen, methane, ethane, propane; Described carbon number comprises methane, ethane, propane, ethene, propylene less than 4 product stream; Olefin(e) centent is 70～90% by weight in the above hydrocarbon of described mixed c 4; Ethene and butylene mol ratio are 2.0～2.5: 1 in the described olefin metathesis system.
The preparation method of SAPO-34 molecular sieve of the present invention is: at first preparing the molecular sieve presoma, is 0.03～0.6R with the mole proportioning: (Si 0.01～0.98: Al 0.01～0.6: P 0.01～0.6): 2～500H
2O, wherein R represents template, and the constitutive material mixed solution obtains through after the crystallization of certain hour at a certain temperature; Again, molecular sieve presoma, phosphorus source, silicon source, aluminium source, organic formwork agent, water etc. after at least 0.1 hour, are finally obtained the SAPO-34 molecular sieve at 110～260 ℃ of lower hydrothermal crystallizings according to certain ratio mixing is rear.The molecular sieve of preparation is mixed with a certain proportion of binding agent, and through obtaining final SAPO-34 catalyzer after the operation stepss such as spraying drying, roasting, the weight percentage of binding agent in molecular sieve is generally between 10～90%.
In methanol-to-olefins reaction process, inevitably can produce the by products such as carbon four above hydrocarbon.Because the olefin(e) centent in the by products such as described carbon four above hydrocarbon is all higher, by adopting method of the present invention, namely generate ethene, propylene product by carbon four above olefins by catalytic cracking, simultaneously except oxide compounds such as the methyl alcohol of carrying secretly in the carbon elimination four above hydrocarbon, dme, then new carbon four above hydrocarbon mixtures and the part ethene of unreacted or generation carry out disproportionation reaction, the production propylene of highly selective.But the carbon back utilization ratio in the method Effective Raise methanol-to-olefins process of the present invention improves the utility value of carbon four above hydrocarbon, improves the Eco-power purpose of MTO technology thereby reach.
Adopt technical scheme of the present invention: described condition for validity comprises: temperature of reaction is 400～500 ℃, and reaction pressure is counted 0～0.3MPa with gauge pressure, and reactor is fast fluidized bed, and catalyzer is the microsphere particle that comprises the SAPO-34 molecular sieve; Described catalytic pyrolysis system response condition: temperature of reaction is 450～600 ℃, and reactor is fixed bed or fluidized-bed, and catalyzer is SAPO-34 or ZSM-5; Described olefin metathesis system response condition: temperature of reaction is 200～450 ℃, and reaction pressure is counted 0～2Mpa with gauge pressure, and weight hourly space velocity is 0.6～10 hour
-1, catalyzer is at least a metal or its oxide compound of load W, Mo or Re, and charge capacity is 1～25% by weight, and carrier can be aluminum oxide, silicon oxide, MCM-48 or SBA-15 molecular sieve; Other by product comprises hydrogen, methane, ethane, propane; Described carbon number comprises methane, ethane, propane, ethene, propylene less than 4 product stream; Olefin(e) centent is 70～90% by weight in the above hydrocarbon of described mixed c 4; Ethene and butylene mol ratio are 2.0～2.5: 1 in the described olefin metathesis system, and propene yield can bring up to 64.68%, has obtained preferably technique effect.
Description of drawings
Fig. 1 is the schematic flow sheet of scheme of the present invention.
Among Fig. 1,1 is the methanol to olefins reaction system; 2 is the methanol-to-olefins product separation system; 3 is propylene; 4 is ethene; 5 is the above hydrocarbon of mixed c 4; 6 is other by product; 7 is the catalytic cracking reaction system; 8 is the catalytic cracking reaction products centrifugal station; 9 is the new above hydrocarbon of mixed c 4; 10 is the olefin dismutation reaction system.
The raw material that comprises methyl alcohol is converted into the product stream that comprises ethene, propylene, C 4 olefin in methanol to olefins reaction system 1, after separation system 2, obtain ethene 4, propylene 3, the above hydrocarbon 5 of mixed c 4, other by product 6, the above hydrocarbon 5 of mixed c 4 enters catalytic pyrolysis system 7, and reaction product obtains carbon number less than 4 product stream and the new above hydrocarbon stream 9 of mixed c 4 after centrifugal station 8 separates.Described carbon number returns methanol-to-olefins separation system 2 less than 4 product stream, and the above hydrocarbon stream 9 of new mixed c 4 enters olefin metathesis system 10 with described at least a portion ethene 4, obtains propylene product 3.
The invention will be further elaborated below by embodiment, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
In the methanol to olefins reaction system, reactor is fast fluidized bed, revivifier is turbulent fluidized bed, catalyzer is SAPO-34, the methanol feedstock of 99.9% (weight) contacts with catalyzer, generation comprises the product of ethene, propylene, carbon four above hydrocarbon, and the catalyzer of inactivation recycles after entering revivifier regeneration.Temperature of reaction is 460 ℃, and reaction pressure is counted 0.15MPa with gauge pressure, and the ratio of molecular sieve in catalyzer is 35% (weight), and the methyl alcohol weight hourly space velocity is 9.0 hours
-1, products distribution sees Table 1.
[embodiment 2]
According to embodiment 1 described condition, temperature of reaction is 500 ℃, and reaction pressure is counted normal pressure with gauge pressure, and the ratio of molecular sieve in catalyzer is 30% (weight), and the methyl alcohol weight hourly space velocity is 12.0 hours
-1, products distribution sees Table 1.
[embodiment 3]
According to embodiment 1 described condition, temperature of reaction is 400 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and the ratio of molecular sieve in catalyzer is 50% (weight), and the methyl alcohol weight hourly space velocity is 8.0 hours
-1, products distribution sees Table 1.
Table 1
| The product carbon base absorption rate, % (weight) | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Ethene | 41.25 | 48.57 | 35.69 |
| Propylene | 40.67 | 32.47 | 40.32 |
| Carbon four above hydrocarbon | 12.68 | 10.57 | 14.37 |
| Other by product (hydrogen, methane, ethane, propane etc.) | 5.4 | 8.39 | 9.62 |
| Olefin(e) centent in the carbon four above hydrocarbon | 89.18 | 89.97 | 86.32 |
[embodiment 4]
In fixed-bed reactor, carry out the preparing propylene by catalytic cracking experiment of carbon four above hydrocarbon, temperature of reaction is 530 ℃, catalyzer is ZSM-5, raw material is according to the composition of carbon four above hydrocarbon among the embodiment 1, and be that 0.5: 1 ratio is added water vapour according to the weight ratio of water vapour and the above hydrocarbon of mixed c 4 in charging, the above hydrocarbon weight hourly space velocity of mixed c 4 is 1.2 hours
-1, the olefin conversion in the carbon four above hydrocarbon is 59%, and yield of ethene is 5.4% in the product, and propene yield is 39.6%.
[embodiment 5]
According to embodiment 4 described conditions, temperature of reaction changes 450 ℃ into, and the olefin conversion in the carbon four above hydrocarbon is 41%, and yield of ethene is 3.8% in the product, and propene yield is 28.8%.
[embodiment 6]
According to embodiment 4 described conditions, temperature of reaction changes 600 ℃ into, and the olefin conversion in the carbon four above hydrocarbon is 67.5%, and yield of ethene is 12.74% in the product, and propene yield is 40.5%.
[embodiment 7]
According to embodiment 4 described conditions, reactor changes fluidized-bed into, and catalyzer changes SAPO-34 into, is that 0.25: 1 ratio is added water vapour according to the weight ratio of water vapour and the above hydrocarbon of mixed c 4 in charging, and the above hydrocarbon weight hourly space velocity of mixed c 4 is 1.8 hours
-1, the olefin conversion in the carbon four above hydrocarbon is 49.7%, and yield of ethene is 21.36% in the product, and propene yield is 19.49%.
[embodiment 8]
Carry out the olefin metathesis experiment in fixed-bed reactor, catalyzer adopts WO
3/ SBA-15, WO
3Weight content be 12%, lower purge 4 hours with nitrogen at 550 ℃ before the reaction, cooling begins reaction after purging, temperature of reaction is 350 ℃, reaction pressure is counted 0.5Mpa with gauge pressure, weight hourly space velocity is 3.0 hours
-1, raw material adopts the above hydrocarbon of mixed c 4, and olefin(e) centent is 75%, and ethene and butylene mol ratio are 2: 1, and propene yield is 55.25% in the product.
[embodiment 9]
According to embodiment 8 described conditions, changing temperature of reaction is 200 ℃, and reaction pressure is counted 0Mpa with gauge pressure, and weight hourly space velocity is 0.6 hour
-1, propene yield is 25.47% in the product.
[embodiment 10]
According to embodiment 8 described conditions, changing temperature of reaction is 450 ℃, and reaction pressure is counted 2Mpa with gauge pressure, and weight hourly space velocity is 10 hours
-1, propene yield is 22.58% in the product.
[embodiment 10]
According to embodiment 8 described conditions, catalyzer adopts WO
3/ MCM-48, propene yield is 53.58% in the product.
[embodiment 11]
According to embodiment 8 described conditions, catalyzer adopts WO
3/ SiO
2, propene yield is 46.53% in the product.
[embodiment 12]
According to embodiment 8 described conditions, catalyzer adopts WO
3/ Al
2O
3, propene yield is 44.17% in the product.
[embodiment 13]
According to embodiment 8 described conditions, catalyzer adopts MoO
3/ SiO
2, propene yield is 37.53% in the product.
[embodiment 14]
According to embodiment 8 described conditions, catalyzer adopts Re/SiO
2, propene yield is 28.31% in the product.
[embodiment 15]
According to embodiment 8 described conditions, catalyzer adopts WO
3/ SBA-15, WO
3Weight content be 2%, propene yield is 25.09% in the product.
[embodiment 16]
According to embodiment 8 described conditions, catalyzer adopts WO
3/ SBA-15, WO
3Weight content be 24%, propene yield is 58.79% in the product.
[embodiment 17]
According to embodiment 8 described conditions, raw material adopts the above hydrocarbon of mixed c 4, and olefin(e) centent is 83%, and ethene and butylene mol ratio are 2.5: 1, and propene yield is 58.63% in the product.
[embodiment 18]
According to embodiment 1,4,8 described conditions, yield of ethene is 27.43% in the final product, and propene yield is 64.68%.
Obviously, adopt method of the present invention, can reach the purpose that improves propene yield, have larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (1)
1. method that improves propene yield, the raw material that comprises methyl alcohol is converted into the product stream that comprises ethene, propylene, C 4 olefin in methanol to olefins reaction system (1), after separation system (2), obtain ethene (4), propylene (3), the above hydrocarbon of mixed c 4 (5), other by product (6), the above hydrocarbon of mixed c 4 (5) enters catalytic pyrolysis system (7), and reaction product obtains carbon number less than 4 product stream and the new above hydrocarbon stream of mixed c 4 (9) after centrifugal station (8) separates; Described carbon number returns methanol-to-olefins separation system (2) less than 4 product stream, the above hydrocarbon stream of new mixed c 4 (9), enter olefin metathesis system (10) with described at least a portion ethene (4), obtain propylene product (3);
In the aforesaid method, in the methanol to olefins reaction system, reactor is fast fluidized bed, revivifier is turbulent fluidized bed, catalyzer is SAPO-34,99.9 the methanol feedstock of % by weight contacts with catalyzer, generates the product that comprises ethene, propylene, carbon four above hydrocarbon, the catalyzer of inactivation recycles after entering revivifier regeneration; Temperature of reaction is 460 ℃, and reaction pressure is counted 0.15MPa with gauge pressure, and the ratio of molecular sieve in catalyzer is 35 % by weight, and the methyl alcohol weight hourly space velocity is 9.0 hours
-1, products distribution is as follows: ethene 41.25 % by weight; Propylene 40.67 % by weight, carbon four above hydrocarbon 12.68 % by weight, hydrogen, methane, ethane, other by product 5.4 % by weight of propane, olefin(e) centent 89.18 % by weight in the carbon four above hydrocarbon;
In the aforesaid method, in fixed-bed reactor, carry out the preparing propylene by catalytic cracking experiment of carbon four above hydrocarbon, temperature of reaction is 530 ℃, catalyzer is ZSM-5, raw material is according to the composition of above-mentioned carbon four above hydrocarbon, and be that 0.5: 1 ratio is added water vapour according to the weight ratio of water vapour and the above hydrocarbon of mixed c 4 in charging, the above hydrocarbon weight hourly space velocity of mixed c 4 is 1.2 hours
-1, the olefin conversion in the carbon four above hydrocarbon is 59%, and yield of ethene is 5.4% in the product, and propene yield is 39.6%.
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