CN103772088A - Method for improving yield of ethylene and propylene - Google Patents
Method for improving yield of ethylene and propylene Download PDFInfo
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- CN103772088A CN103772088A CN201210393205.1A CN201210393205A CN103772088A CN 103772088 A CN103772088 A CN 103772088A CN 201210393205 A CN201210393205 A CN 201210393205A CN 103772088 A CN103772088 A CN 103772088A
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of 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
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/40—Ethylene production
Abstract
The invention relates to a method for improving the yield of ethylene and propylene, and mainly solves the problem of lower yield of ethylene and propylene in the prior art. The method comprises the following steps: (1) a raw material mainly containing methanol goes into a fast-bed reaction zone and is contacted with a catalyst comprising a silicoaluminophosphate molecular sieve; the generated gas phase material flow and the catalyst go into a dense phase bed reaction zone through a distribution plate, and the gas phase material flow goes into a separation working section after being subjected to gas-solid separation; and the separated-out catalyst is at least divided into two parts, the first part of the catalyst returns to the bottom of the fast-bed reaction zone after heat is removed by an external heat remover, and the second part of the catalyst goes into a regenerator for regeneration to form a regenerated catalyst; and (2) the regenerated catalyst is degassed and then goes into a fast-bed reaction zone position with the height of 1/3 to 3/4 that of the fast-bed reaction zone, wherein the mass flow quantity ratio of the first part of the catalyst to the second part of the catalyst is 1-25:1. Through adopting the above technical scheme, the problem is relatively well solved, and the method can be used in industrial production of ethylene and propylene.
Description
Technical field
The present invention relates to a kind of method that improves 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.Usually, ethene, propylene are to produce by petroleum path, but due to the limited supply of petroleum resources and higher price, the cost of being produced ethene, propylene by petroleum resources constantly increases.In recent years, people start to greatly develop the technology of alternative materials conversion ethene processed, propylene.Wherein, the important alternative materials of producing for low-carbon alkene 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, as methyl alcohol, can be made by coal or Sweet natural gas, and technique is very ripe, can realize the industrial scale of up to a million tonnes.Due to the popularity in oxygenatedchemicals source, add and transform the economy that generates low-carbon alkene technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), be particularly subject to increasing attention by the technique of preparing olefin by conversion of methanol (MTO).
In US 4499327 patents, silicoaluminophosphamolecular molecular sieve catalyst is applied to preparing olefin by conversion of methanol technique and studies in detail, think that SAPO-34 is the first-selected catalyzer of MTO technique.SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, and can make methanol conversion is reaction times of low-carbon alkene to be less than the degree of 10 seconds, more even reaches in the reaction time range of riser tube.
Technology and reactor that a kind of methanol conversion is low-carbon alkene in US 6166282, are announced, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu of gas speed has reacted, rise to after the fast subregion that internal diameter diminishes rapidly, adopt special gas-solid separation equipment initial gross separation to go out most entrained catalyst.Due to reaction after product gas and catalyzer sharp separation, effectively prevent the generation of secondary reaction.Through analog calculation, compared with traditional bubbling fluidization bed bioreactor, this fast fluidized bed reactor internal diameter and the required reserve of catalyzer all greatly reduce.But in the method, yield of light olefins is general all in 77% left and right, has the problem that yield of light olefins is lower.
In CN 1723262, having announced with the multiple riser reaction unit of central catalyst return is low-carbon alkene technique for oxygenate conversion, this covering device comprises multiple riser reactors, gas solid separation district, multiple 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.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, and a kind of new raising ethene, the method for propene yield are provided.The method, for the production of ethene, propylene, has advantages of that in product, yield of light olefins is higher.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of ethene that improves, the method of propene yield, comprise the following steps: the raw material that (1) is mainly methyl alcohol enters fast bed reaction zone, contact with the catalyzer that comprises silicoaluminophosphamolecular molecular sieve, the gaseous stream generating and catalyzer enter dense bed reaction zone through grid distributor, gaseous stream enters centrifugal station after gas solid separation, isolated catalyzer is at least divided into two portions, first part's catalyzer returns to bottom, described fast bed reaction zone after external warmer heat-obtaining, second section catalyzer enters revivifier regeneration, form regenerated catalyst, (2) described regenerated catalyst enters 1/3～3/4 fast bed reaction zone At The Height of fast bed reaction zone after degassed, wherein, described first part catalyzer is 1～25:1 with the ratio of second section mass flow of catalyst.
In technique scheme, described silicoaluminophosphamolecular molecular sieve is selected from least one in SAPO-18, SAPO-34, and preferred version is selected from SAPO-34.The reaction conditions of fast bed reaction zone is: reaction pressure is counted 0.01～0.3MPa, medial temperature as 400～500 ℃, the average coke content of catalyzer are as 1.5～3.5% weight take gauge pressure.The reaction conditions of described dense bed reaction zone is: reaction pressure is counted 0.01～0.3MPa, medial temperature as 420～550 ℃, gas phase linear speed are as 0.3～1.0 meter per second take gauge pressure.Described first part catalyzer is 4～15 with the ratio of second section mass flow of catalyst, and preferable range is 6 ~ 12.Described grid distributor percentage of open area is 20～70%, and preferable range is 30 ~ 60%.
The method of calculation of coke content of the present invention are that carbon deposit quality on the catalyzer of certain mass is divided by described catalyst quality.Carbon deposit measuring method on catalyzer is as follows: will mix the catalyst mix with carbon deposit comparatively uniformly, then weigh the band C catalyst of certain mass, be put in pyrocarbon analyser and burn, by infrared analysis burn generate carbonic acid gas quality, thereby obtain the carbonaceous amount on catalyzer.
The preparation method of silicoaluminophosphamolecular molecular sieve of the present invention is: first preparing molecular sieve presoma, is 0.03～0.6R by mole proportioning: (Si 0.01～0.98: Al 0.01～0.6: P 0.01～0.6): 2～500 H
2o, wherein R represents template, constitutive material mixed solution obtains at a certain temperature after the crystallization of certain hour; Again, molecular sieve presoma, phosphorus source, silicon source, aluminium source, organic formwork agent, water etc. are mixed according to certain ratio after at 110～260 ℃ hydrothermal crystallizing after at least 0.1 hour, finally obtain SAPO molecular sieve.The molecular sieve of preparation is mixed with a certain proportion of binding agent, after the operation stepss such as, roasting dry through spraying, obtain final SAPO catalyzer, the weight percentage of binding agent in molecular sieve is generally between 10～90%.
In the present invention, percentage of open area refers to the useful area of grid distributor, namely refers to the area summation in hole on grid distributor face and the ratio of the grid distributor face total area.
Known in the field, in the reaction process that is low-carbon alkene in methanol conversion, on catalyzer, accumulate the selectivity that a certain amount of carbon distribution is conducive to improve low-carbon alkene.Adopt method of the present invention, methanol feedstock enters behind reaction zone, first contact with reclaimable catalyst, production low-carbon alkene that can highly selective, the product generating upwards contacts with regenerated catalyst with unconverted methyl alcohol, transform unreacted methyl alcohol, simultaneously because regenerated catalyst has high temperature, highly active feature, so in transforming methyl alcohol the also above high-carbon hydrocarbon of cracking section carbon four.Simultaneously, the methyl alcohol load that the conversion zone that regenerated catalyst returns or above region need to be changed is less, the respective reaction heat of emitting is just few, and the method can well be controlled the temperature rise of reaction zone, and 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, the gaseous stream coming from fast bed reaction zone and catalyzer are dense bed reaction zone, because gas-solid contact time increases, the cracking degree of carbon four above high-carbon hydrocarbons increases, because the olefin(e) centent in the above high-carbon hydrocarbon of carbon four is generally all more than 80%, so the olefin cracking of this part high-carbon becomes ethene, propylene, thereby realize the object that improves yield of light olefins.
Adopt technical scheme of the present invention: described silicoaluminophosphamolecular molecular sieve is selected from least one in SAPO-18, SAPO-34; The reaction conditions of described reaction zone is: reaction pressure is counted 0.01～0.3MPa, medial temperature as 400～500 ℃, the average coke content of catalyzer are as 1.5～3.5% weight take gauge pressure; Described reclaimable catalyst is at least divided into three parts, and 30～50% return to bottom, described reaction zone, and 20～30% return to described reaction zone 1/5～3/5 reaction zone At The Height, and 20～50% enter revivifier regeneration; Described second section reclaimable catalyst returns to reaction zone through after being provided with the external warmer heat-obtaining of heat production coil pipe, low-carbon alkene carbon base absorption rate can reach 84.19% weight, exceed and can reach 3 percentage points than low-carbon alkene carbon base absorption rate of the prior art, obtained good technique effect.
Accompanying drawing explanation
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 grid distributor; 4 is inclined tube to be generated; 5 is regenerator sloped tube; 6 is heat production coil pipe; 7 is gas-solid cyclone separator; 8 is dense bed reaction zone; 9 is negative area; 10 is collection chamber; 11 is product gas outlet pipeline; 12 is external warmer gaseous phase outlet pipeline; 13 is methanol feeding sparger; 14 is external warmer; 15 is external warmer lower oblique tube.
Methanol feedstock enters in fast bed reaction zone 2 through feeding line 1, contact with molecular sieve catalyst, reaction generates the product that contains ethene, propylene, carry reclaimable catalyst and enter dense bed reaction zone 8 through grid distributor 3, generate gaseous stream with catalyzer after cyclonic separator 7 separates, catalyzer turns back to dense bed reaction zone 8 through the dipleg of cyclonic separator 7, and gaseous products enters follow-up centrifugal station through outlet line 11 after entering collection chamber 10.Isolated reclaimable catalyst is at least divided into two portions after stripping, a part turns back to fast bed reaction zone 2 by external warmer lower oblique tube 15 after interchanger 14 heat exchange, a part enters coke-burning regeneration in revivifier through inclined tube 4 to be generated, and the catalyzer of having regenerated returns in fast bed reaction zone 2 by regenerator sloped tube 5.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1～2]
In fluidized bed reaction as shown in Figure 1, catalyst type is in table 1, purity is that 99.5% methanol feedstock enters fast bed reaction zone, contact with catalyzer, the gaseous stream generating and catalyzer enter dense bed reaction zone through grid distributor, gaseous stream enters centrifugal station after gas solid separation, isolated catalyzer is divided into two portions, first part's catalyzer returns to bottom, described fast bed reaction zone after external warmer heat-obtaining, second section catalyzer enters revivifier regeneration, form regenerated catalyst, regenerated catalyst enters 1/3 fast bed reaction zone At The Height of fast bed reaction zone after degassed.First part's catalyzer is 1:1 with the ratio of second section mass flow of catalyst.The reaction conditions of fast bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 400 ℃, the average coke content of catalyzer are as 1.5% weight take gauge pressure; The reaction conditions of dense bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 420 ℃, gas phase linear speed are as 0.3 meter per second take gauge pressure, and grid distributor percentage of open area is 20%.The stability that keeps catalyst flow control, reactor outlet product adopts online gas chromatographic analysis, and 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 |
| |
SAPO-34 | 81.44 |
[embodiment 3]
According to condition and step described in embodiment 2, regenerated catalyst enters 3/4 fast bed reaction zone At The Height of fast bed reaction zone after degassed.First part's catalyzer is 25:1 with the ratio of second section mass flow of catalyst.The reaction conditions of fast bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 500 ℃, the average coke content of catalyzer are as 3.5% weight take gauge pressure; The reaction conditions of dense bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 548 ℃, gas phase linear speed are as 1.0 meter per seconds take gauge pressure, and grid distributor percentage of open area is 70%.The stability that keeps catalyst flow control, reactor outlet product 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 1/2 fast bed reaction zone At The Height of fast bed reaction zone after degassed.First part's catalyzer is 15:1 with the ratio of second section mass flow of catalyst.The reaction conditions of fast bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 480 ℃, the average coke content of catalyzer are as 2.5% weight take gauge pressure; The reaction conditions of dense bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 502 ℃, gas phase linear speed are as 0.7 meter per second take gauge pressure, and grid distributor percentage of open area is 60%.The stability that keeps catalyst flow control, reactor outlet product adopts online gas chromatographic analysis, and 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 1/2 fast bed reaction zone At The Height of fast bed reaction zone after degassed.First part's catalyzer is 4:1 with the ratio of second section mass flow of catalyst.The reaction conditions of fast bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 460 ℃, the average coke content of catalyzer are as 3% weight take gauge pressure; The reaction conditions of dense bed reaction zone is: reaction pressure is counted 0.01MPa, medial temperature as 473 ℃, gas phase linear speed are as 0.5 meter per second take gauge pressure, and grid distributor percentage of open area is 60%.The stability that keeps catalyst flow control, reactor outlet product adopts online gas chromatographic analysis, and 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 1/2 fast bed reaction zone At The Height of fast bed reaction zone after degassed.First part's catalyzer is 8:1 with the ratio of second section mass flow of catalyst.The reaction conditions of fast bed reaction zone is: reaction pressure is counted 0.3MPa, medial temperature as 490 ℃, the average coke content of catalyzer are as 2.4% weight take gauge pressure; The reaction conditions of dense bed reaction zone is: reaction pressure is counted 0.3MPa, medial temperature as 524 ℃, gas phase linear speed are as 0.5 meter per second take gauge pressure, and grid distributor percentage of open area is 60%.The stability that keeps catalyst flow control, reactor outlet product adopts online gas chromatographic analysis, and 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 bottom, fast bed reaction zone by regenerator sloped tube, and 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 bottom, fast bed reaction zone by regenerator sloped tube, grid distributor and dense bed reaction zone are not set, and the gaseous stream of fast bed reaction zone outlet and catalyzer are after gas solid separation, and gaseous stream enters centrifugal station.The low-carbon alkene carbon base absorption rate of reactor outlet is 81.23% (weight).
Obviously, adopt method of the present invention, can reach the object that improves ethene, propylene carbon base absorption rate, there is larger technical superiority, can be used in the industrial production of ethene, propylene.
Claims (9)
1. a method that improves ethene, propene yield, comprises the following steps:
(1) raw material that is mainly methyl alcohol enters fast bed reaction zone, contact with the catalyzer that comprises silicoaluminophosphamolecular molecular sieve, the gaseous stream generating and catalyzer enter dense bed reaction zone through grid distributor, gaseous stream enters centrifugal station after gas solid separation, isolated catalyzer is at least divided into two portions, first part's catalyzer returns to bottom, described fast bed reaction zone after external warmer heat-obtaining, and second section catalyzer enters revivifier regeneration, forms regenerated catalyst;
(2) described regenerated catalyst enters 1/3～3/4 fast bed reaction zone At The Height of fast bed reaction zone after degassed;
Wherein, described first part catalyzer is 1～25:1 with the ratio of second section mass flow of catalyst.
2. improve according to claim 1 the method for ethene, propene yield, it is characterized in that described silicoaluminophosphamolecular molecular sieve is selected from least one in SAPO-18 or SAPO-34.
3. improve according to claim 2 the method for ethene, propene yield, it is characterized in that described silicoaluminophosphamolecular molecular sieve is selected from SAPO-34.
4. improve according to claim 1 the method for ethene, propene yield, it is characterized in that the reaction conditions of described fast bed reaction zone is: reaction pressure is counted 0.01～0.3MPa, medial temperature as 400～500 ℃, the average coke content of catalyzer are as 1.5～3.5% weight take gauge pressure.
5. improve according to claim 1 the method for ethene, propene yield, it is characterized in that the reaction conditions of described dense bed reaction zone is: reaction pressure is counted 0.01～0.3MPa, medial temperature as 420～550 ℃, gas phase linear speed are as 0.3～1.0 meter per second take gauge pressure.
6. improve according to claim 1 the method for ethene, propene yield, it is characterized in that described first part catalyzer and the ratio of second section mass flow of catalyst are 4～15.
7. improve according to claim 6 the method for ethene, propene yield, it is characterized in that described first part catalyzer and the ratio of second section mass flow of catalyst are 6～12.
8. improve according to claim 1 the method for ethene, propene yield, it is characterized in that described grid distributor percentage of open area is 20～70%.
9. improve according to claim 8 the method for ethene, propene yield, it is characterized in that described grid distributor percentage of open area is 30～60%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099947A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Method for preparing aromatic hydrocarbon by efficiently converting methanol |
| CN113385113A (en) * | 2020-03-13 | 2021-09-14 | 中国石油化工股份有限公司 | Method for improving yield of ethylene and propylene and fluidized bed reactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102464529A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for increasing yield of low-carbon olefins |
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| CN102464529A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for increasing yield of low-carbon olefins |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099947A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Method for preparing aromatic hydrocarbon by efficiently converting methanol |
| CN111099947B (en) * | 2018-10-25 | 2022-08-12 | 中国石油化工股份有限公司 | Method for preparing aromatic hydrocarbon by efficiently converting methanol |
| CN113385113A (en) * | 2020-03-13 | 2021-09-14 | 中国石油化工股份有限公司 | Method for improving yield of ethylene and propylene and fluidized bed reactor |
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